CN110040691B - Device and method for preparing and producing high-purity sulfur dioxide by using acid gas - Google Patents
Device and method for preparing and producing high-purity sulfur dioxide by using acid gas Download PDFInfo
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- CN110040691B CN110040691B CN201910224997.1A CN201910224997A CN110040691B CN 110040691 B CN110040691 B CN 110040691B CN 201910224997 A CN201910224997 A CN 201910224997A CN 110040691 B CN110040691 B CN 110040691B
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- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 239000002253 acid Substances 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 394
- 239000007788 liquid Substances 0.000 claims abstract description 213
- 239000012071 phase Substances 0.000 claims abstract description 163
- 239000007791 liquid phase Substances 0.000 claims abstract description 130
- 239000002994 raw material Substances 0.000 claims abstract description 100
- 238000002485 combustion reaction Methods 0.000 claims abstract description 76
- 239000002918 waste heat Substances 0.000 claims abstract description 45
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000001301 oxygen Substances 0.000 claims abstract description 44
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 44
- 238000003860 storage Methods 0.000 claims abstract description 41
- 238000001035 drying Methods 0.000 claims abstract description 34
- 238000010521 absorption reaction Methods 0.000 claims abstract description 24
- 239000002699 waste material Substances 0.000 claims abstract description 20
- 239000002808 molecular sieve Substances 0.000 claims abstract description 14
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000001105 regulatory effect Effects 0.000 claims description 110
- 238000000746 purification Methods 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 230000003009 desulfurizing effect Effects 0.000 claims description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 18
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 12
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 238000002309 gasification Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000001509 sodium citrate Substances 0.000 description 6
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- XFKVHUONJVDEIW-UHFFFAOYSA-N [Cl].S(O)(O)(=O)=O Chemical compound [Cl].S(O)(O)(=O)=O XFKVHUONJVDEIW-UHFFFAOYSA-N 0.000 description 1
- HIPVJRPEJALNIE-UHFFFAOYSA-L [Na+].[K+].OS([O-])=O.OS([O-])=O Chemical compound [Na+].[K+].OS([O-])=O.OS([O-])=O HIPVJRPEJALNIE-UHFFFAOYSA-L 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 239000002316 fumigant Substances 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004076 pulp bleaching Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention belongs to a device and a method for preparing and producing high-purity sulfur dioxide by using acid gas; the device comprises an acid gas buffer tank, an oxygen storage tank, a product tank and a waste liquid absorption tower, wherein the acid gas buffer tank is connected with a first inlet of a combustion furnace, the oxygen storage tank is connected with a second inlet of the combustion furnace, an outlet of the combustion furnace is connected with a first gas-liquid separator through a tube pass of a waste heat boiler, and a gas phase outlet of the first gas-liquid separator is connected with a first raw material gas inlet of a first rectifying tower through a drying and purifying tower with a molecular sieve; the liquid phase outlet of the first rectifying tower is connected with the first raw material liquid inlet of the second rectifying tower through a pipeline, the top gas phase outlet of the second rectifying tower is connected with the second raw material gas inlet of the top condenser, and the second raw material liquid outlet of the top condenser is connected with the product storage tank through a second tee joint and a product pump; has the characteristics of stable operation, simple and convenient operation and capability of improving the purity of the product to 99.99 percent high purity level.
Description
Technical Field
The invention belongs to the technical field of high-purity sulfur dioxide production, and particularly relates to a device and a method for producing high-purity sulfur dioxide by using acid gas, wherein the purity of sulfur dioxide produced by using a mode of synthesizing acid gas and rectifying acid gas is not less than 99.99%.
Background
Sulfur dioxide, also known as thionic anhydride, is a colorless, strongly irritating odor gas at ordinary temperatures, and is a major cause of "acid rain" worldwide. In the chemical industry, sulfur dioxide is mainly used for preparing sulfuric acid, sulfite, sodium (potassium) bisulfite, sulfuric acid chlorine and the like; as a catalyst in the manufacture of various resins and plastics. In the pulp, paper and textile industries, sulphite cooking liquor of the pulping process can be prepared; a pulp bleaching process; purging chlorine gas; as a chlorine removing agent, an acidic substance, etc. The method is environment-friendly and is used for dechlorination of urban or industrial sewage. Petroleum processing and metal refining, as solvents; refined kerosene and light lubricating oil; is used for the smelting process of nonferrous metals. It is widely used in the food industry as a preservative, bleaching agent and fumigant. Pure sulfur dioxide can also be used for preparing environment-friendly standard gas.
The traditional production method of the high-purity sulfur dioxide comprises the following steps:
1. normal pressure water absorption method: water (natural cold sea water with the temperature of 10 ℃) is used as an absorbent, sulfur dioxide is absorbed and then is resolved by steam, and the resolved gas is condensed, dried and liquefied to obtain a sulfur dioxide product. The purity of sulfur dioxide obtained by the method is generally less than or equal to 99.9 percent.
2. Pressurized water absorption process: the gas sulfur dioxide is absorbed by water under the condition of pressurization, SO that the solubility of SO2 can be increased, the absorptivity can be improved, and the purity of the sulfur dioxide prepared by the method is less than 99.99%.
3. Ammonia-acid process: is commonly used for recovering SO2 from low-concentration SO2 gas, and takes gas ammonia, liquid ammonia or ammonia water as an ammonia source to absorb sulfur dioxide.
Absorption reaction formula: (1) 2NH3+2H2O+SO2→ (NH 4) 2SO3+H2O
(2)(NH4)2SO3+H2O+SO2→2NH4HSO3
The total salt content of the absorption liquid is controlled to be about 400-450 g/L, wherein the mass ratio of the ammonium sulfite to the ammonium bisulfate is 1:3, and the absorption liquid of the salt can be decomposed when meeting concentrated sulfuric acid to release high-concentration sulfur dioxide.
The solution equation: (NH 4) 2SO3+H2SO4→ (NH 4) 2SO4+H2O+SO2 ≡
2NH4HSO3+H2SO4→(NH4)2SO4+2H2O+2SO2↑
The liquid SO2 produced by the method has simple flow and equipment and less investment, but the method needs to consume ammonia and sulfuric acid, is rich in liquid ammonium sulfate, needs to build equipment for evaporating, concentrating, crystallizing, separating and the like, and needs to consume steam. The process is generally only suitable for use in plants where there is an inexpensive supply of ammonia, steam, and liquid ammonium sulfate is a commodity.
4. Sodium citrate process
In the process of producing liquid sulfur dioxide by sodium citrate, gas sulfur dioxide is absorbed by sodium citrate solution, the absorption liquid is directly heated to about 115 ℃ to resolve high-concentration sulfur dioxide, and then the high-concentration sulfur dioxide is dried and liquefied. Because of the higher price of sodium citrate and the increased amount of waste liquid discharged per unit of product, which increases the consumption of citric acid, the method is generally applicable to factories for producing sodium citrate or places where the price of sodium citrate is low.
Fuming sulfuric acid process: the method is a method for producing the liquid sulfur dioxide by combining the existing fuming sulfuric acid or concentrated sulfuric acid production device, and the purity of the liquid sulfur dioxide product prepared by the method can reach 99.98 percent at most.
By introducing and comparing the method, the traditional production process of the high-purity sulfur dioxide is influenced by different processes, so that the purity of the product can not reach the high-purity level, and the requirements of the standard gas industry and the semiconductor industry on the high-purity sulfur dioxide can not be met.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a device and a production method for producing high-purity sulfur dioxide by utilizing acid gas, wherein the device utilizes the acid gas to synthesize low-concentration sulfur dioxide firstly, then utilizes a drying purification tower to adsorb impurities and then utilizes a rectification purification mode to prepare sulfur dioxide.
The object of the invention is achieved in that: the device comprises an acid gas buffer tank, an oxygen storage tank, a product tank and a waste liquid absorption tower, wherein the acid gas buffer tank is connected with a first inlet of a combustion furnace, the oxygen storage tank is connected with a second inlet of the combustion furnace, an outlet of the combustion furnace is connected with a first gas-liquid separator through a tube side of a waste heat boiler, and a gas phase outlet of the first gas-liquid separator is connected with a first raw material gas inlet of a first rectifying tower through a drying and purifying tower with a molecular sieve; the liquid phase outlet of the first rectifying tower is connected with the first raw material liquid inlet of the second rectifying tower through a pipeline, the top gas phase outlet of the second rectifying tower is connected with the top condenser second raw material gas inlet, and the top condenser second raw material liquid outlet is connected with the product storage tank through a second tee joint and a product pump.
Preferably, a shell side inlet of the waste heat boiler is connected with a circulating water supply pipeline through a tenth regulating valve, and a shell side outlet of the waste heat boiler is connected with a steam pipe network; the liquid phase outlet of the first gas-liquid separator is connected with the waste liquid absorption tower through a pipeline which is inclined downwards.
Preferably, the gas phase outlet at the top of the first rectifying tower is connected with the first raw material gas inlet of the top condenser, the first raw material gas outlet of the top condenser is connected with the inlet of the second gas-liquid separator, the liquid phase outlet of the second gas-liquid separator is connected with the second inlet of the first rectifying tower through the second regulating valve, and the gas phase outlet of the second gas-liquid separator is connected with the inlet of the desulfurizing tower through the fourth regulating valve and the first tee joint in sequence.
Preferably, the third end of the second tee is connected with the raw material liquid second inlet of the second rectifying tower through a fifth regulating valve.
Preferably, the bottom liquid phase outlet of the second rectifying tower is connected with the desulfurizing tower through the third end of the first tee joint.
Preferably, the circulating gas outlet of the heat pump is connected with the inlets of the first reboiler at the bottom of the first rectifying tower and the second reboiler at the bottom of the second rectifying tower through a third tee joint respectively, the outlets of the first reboiler and the second reboiler are connected with the shell-side circulating liquid inlet of the top condenser through a fourth tee joint respectively, and the shell-side circulating gas outlet is connected with the circulating gas inlet of the heat pump.
Preferably, a first regulating valve and a first cut-off valve are sequentially arranged between the acid gas buffer tank and a first inlet of the combustion furnace, an eighth regulating valve and a second cut-off valve are arranged between the oxygen storage tank and a second inlet of the combustion furnace, a third regulating valve and a third cut-off valve are arranged between a liquid phase outlet of the first rectifying tower and a first raw material liquid inlet of the second rectifying tower, and a sixth regulating valve is arranged between the product pump and the product storage tank.
Preferably, a seventh regulating valve is arranged between the third tee joint and the first reboiler inlet, an eleventh regulating valve is arranged between the third tee joint and the second reboiler inlet, and a ninth regulating valve is arranged between the shell side circulating gas outlet and the circulating gas inlet of the heat pump.
A production method of a device for producing high-purity sulfur dioxide by using acid gas comprises the following steps:
step 1: the acid gas in the acid gas buffer tank enters the combustion furnace through the first regulating valve, the first cut-off valve and the first inlet of the combustion furnace, and the oxygen in the oxygen storage tank enters the combustion furnace through the eighth regulating valve, the second cut-off valve and the second inlet of the combustion furnace; the main components of the acid gas are as follows: methanol, hydrogen sulfide, carbon dioxide, nitrogen, carbon monoxide, hydrogen, carbonyl sulfide, sulfur dioxide, and propane; the temperature of the acid gas is as follows: the temperature is 20-30 ℃ and the pressure is as follows: the flow rate of 0.2Mpa is: 28Nm 3 And (3) the gas phase fraction is: 0. the mole fraction of hydrogen sulfide is: 25-43%;
step 2: enabling the acid gas and the oxygen in the step 1 to enter a combustion furnace for combustion, exchanging heat through a tube side of a waste heat boiler, enabling the gas after heat exchange to enter a first gas-liquid separator for separating free water, enabling the separated free water to enter a waste liquid absorption tower through a liquid phase outlet of the first gas-liquid separator, and enabling the separated gas to enter a drying and purifying tower through a gas phase outlet of the first gas-liquid separator; gas phase outlet temperature of the first gas-liquid separator: 30-40 ℃ SO 2 Mole fraction: 30-40%;
step 3: drying, impurity removing and purifying the gas entering the drying and purifying tower in the step 2 through a molecular sieve, and entering the purified raw material gas into a first rectifying tower; gas temperature after passing through the drying purification tower: 30-40 ℃ SO 2 55-65% of mole fraction;
step 4: the raw material gas entering the first rectifying tower in the step 3 is subjected to primary rectifying purification, the liquid phase at the bottom of the first rectifying tower after primary rectifying purification enters the second rectifying tower through a third regulating valve and a third cut-off valve, and the liquid phase temperature of a liquid phase outlet at the bottom of the first rectifying tower is as follows: 16-25 ℃, flow rate: 11-15.4 Nm 3 /h、SO 2 Mole fraction: 97.6 to 99.9 percent;
step 5: carrying out secondary rectification purification on the liquid phase entering the second rectifying tower in the step 4, wherein a gas phase after the secondary rectification purification enters a second tee joint through a top gas phase outlet of the second rectifying tower, a second raw material gas inlet of a top condenser and a second raw material liquid outlet of the top condenser, and a part of the liquid phase in the second tee joint enters a product tank through a product pump; the other part of liquid phase in the second tee joint flows back into the second rectifying tower through a fifth regulating valve and a second raw material liquid inlet of the second rectifying tower; top gas phase outlet temperature of the second rectification column: 13-19 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second raw material liquid outlet of the top condenser entering the second rectifying tower: 11-17 ℃, gas phase fraction: 0; the top condenser enters the liquid phase temperature of the inlet of the product pump through the third end of the second tee joint: 11-17 ℃ SO 2 The purity of the product is not lower than 99.99%;
step 6: the gas phase after primary rectification and purification in the step 4 enters a second gas-liquid separator through a gas phase outlet at the top of the first rectifying tower, a first raw material gas inlet of a top condenser and a first raw material liquid outlet of the top condenser for gas-liquid separation, and a liquid phase after gas-liquid separation enters the first rectifying tower through a liquid phase outlet of the second gas-liquid separator and a second regulating valve; gas phase temperature of the first rectifying column top gas phase outlet: 16-25 ℃ SO 2 Mole fraction: 63-72%, gas phase fraction: 1, a step of; the liquid phase temperature of the liquid phase outlet of the second gas-liquid separator entering the first rectifying tower is 15-22 ℃, SO 2 Mole fraction: 90-96%, gas phase fraction: 0;
step 7: in the step 6, the gas phase after gas-liquid separation in the second gas-liquid separator sequentially passes through a gas phase outlet of the second gas-liquid separator, a fourth regulating valve and a first tee joint to enter the desulfurizing tower, wherein the temperature of the gas phase outlet of the second gas-liquid separator is as follows: 15-22 ℃, flow rate: 4.4 to 7.2Nm 3 Gas phase fraction/h: 1, a step of;
step 8: the liquid phase purified by the rectification of the second rectifying tower in the step 5 enters the desulfurizing tower through a bottom liquid phase outlet and a third end of a first tee joint, and the bottom liquid phase outlet temperature of the second rectifying tower: 14-20 ℃, flow: 5.5 to 9.6Nm 3 Gas phase fraction/h: 0;
step 9: circulating gas in the heat pump respectively enters the first reboiler and the second reboiler through the third tee joint, circulating liquid in the outlet of the first reboiler and the outlet of the second reboiler respectively enters the shell side of the top condenser through the fourth tee joint and the shell side circulating liquid inlet of the top condenser for gasification, and gasified gas phase enters the heat pump through the shell side circulating gas outlet of the top condenser and the circulating gas inlet of the heat pump; the outlet temperature of the first reboiler is: 20-26 ℃, gas phase fraction: 0; the outlet temperature of the second reboiler was: 16-22 ℃, gas phase fraction: 0; gas ammonia mole fraction of the shell side recycle gas outlet of the top condenser: 100%, temperature: 9-13 ℃, gas phase fraction: 100%;
Step 10: desalted water in the circulating water supply pipeline enters the shell side of the waste heat boiler through a tenth regulating valve and a shell side inlet of the waste heat boiler, and heat exchanged steam enters a steam pipe network through a shell side outlet of the waste heat boiler.
The invention adopts the device and the production method for producing the high-purity sulfur dioxide by rectifying and purifying the acid gas to generate the sulfur dioxide which is used as the raw material of the whole system, the purity of the liquid-phase sulfur dioxide of the product is not lower than 99.99 percent, fills the blank of the domestic high-purity sulfur dioxide production, lays the foundation for the development of the electronic industry and the semiconductor industry, and has important significance. Compared with the traditional process technology, the invention has the following advantages: 1. the acid gas inlet and the oxygen inlet are respectively provided with one regulating valve and one cutting valve, so that the function of rapidly cutting off the raw gas when the temperature of the combustion furnace is unstable is realized; 2. the acid gas is used as the raw material gas, so that the economic benefit of the product is improved, and the problem of atmospheric environment protection is solved; 3. the defects of complex process flow and low product purity of the traditional process are overcome, the reacted acid gas is dried and purified in a drying and purifying tower by adopting a molecular sieve, and the product purity is effectively improved by purifying in a rectifying tower; 4. the product purity can reach more than 99.99%, fills the production blank of domestic high-purity sulfur dioxide, and solves the difficult problem that the purity of sulfur dioxide produced by the traditional process is not high (the highest purity is 99.98%). The device and the production method not only greatly improve the purity of the product, but also solve the problem that the traditional method for preparing sulfur by using hydrogen sulfide generally has low economic benefit; the method has the characteristics of stable operation, simple and convenient operation and capability of improving the purity of the product to 99.99 percent high purity level; provides guarantee for the research of special gas in the electronic industry and the development of the semiconductor field, and has good economic and social benefits.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
For a clearer understanding of the technical features, objects and effects of the present invention, embodiments of the present invention will now be described with reference to the drawings, in which like reference numerals refer to like parts throughout the various views. For simplicity of the drawing, only the parts relevant to the present invention are schematically shown in each drawing, and they do not represent the actual structure thereof as a product.
As shown in fig. 1, the invention is an apparatus for producing high-purity sulfur dioxide by using acid gas and a production method thereof, the apparatus comprises an acid gas buffer tank 12, an oxygen storage tank 47, a product tank 24 and a waste liquid absorption tower 40, wherein the acid gas buffer tank 12 is connected with a first inlet 39 of a combustion furnace 15, the oxygen storage tank 47 is connected with a second inlet 38 of the combustion furnace 15, an outlet of the combustion furnace 15 is connected with a first gas-liquid separator 25 through a tube pass of a waste heat boiler 16, and a gas phase outlet of the first gas-liquid separator 25 is connected with a first raw material gas inlet 27 of a first rectifying tower 17 through a drying and purifying tower 26 with molecular sieve; the liquid phase outlet 49 of the first rectifying tower 17 is connected with the first raw material liquid inlet 31 of the second rectifying tower 21 through a pipeline, the top gas phase outlet of the second rectifying tower 21 is connected with the second raw material gas inlet 32 of the top condenser 20, and the second raw material liquid outlet 33 of the top condenser 20 is connected with the product storage tank 24 through the second tee joint 11 and the product pump 23. The shell side inlet of the waste heat boiler 16 is connected with the circulating water supply pipeline 44 through a tenth regulating valve 50, and the shell side outlet of the waste heat boiler 16 is connected with the steam pipe network 43; the liquid phase outlet of the first gas-liquid separator 25 is connected to the waste liquid absorption column 40 through a pipe inclined downward. The gas phase outlet at the top of the first rectifying tower 17 is connected with the first raw material gas inlet 28 of the top condenser 20, the first raw material gas outlet 29 of the top condenser 20 is connected with the inlet of the second gas-liquid separator 19, the liquid phase outlet of the second gas-liquid separator 19 is connected with the second inlet 30 of the first rectifying tower 17 through the second regulating valve 2, and the gas phase outlet of the second gas-liquid separator 19 is connected with the inlet of the desulfurizing tower 46 sequentially through the fourth regulating valve 4 and the first tee joint 10. The third end of the second tee 11 is connected with a raw material liquid second inlet 34 of the second rectifying tower 21 through a fifth regulating valve 5. The bottom liquid phase outlet 37 of the second rectifying tower 21 is connected with the desulfurizing tower 46 through the third end of the first tee 10. The circulating gas outlet of the heat pump 45 is respectively connected with the inlets of the first reboiler 18 at the bottom of the first rectifying tower 17 and the second reboiler 22 at the bottom of the second rectifying tower 21 through the third tee joint 13, the outlets of the first reboiler 18 and the second reboiler 22 are respectively connected with the shell-side circulating liquid inlet 41 of the top condenser 20 through the fourth tee joint 14, and the shell-side circulating gas outlet 42 is connected with the circulating gas inlet of the heat pump 45. A first regulating valve 1 and a first cut-off valve 48 are sequentially arranged between the acid gas buffer tank 12 and the first inlet 39 of the combustion furnace 15, an eighth regulating valve 8 and a second cut-off valve 51 are arranged between the oxygen storage tank 47 and the second inlet 38 of the combustion furnace 15, a third regulating valve 3 and a third cut-off valve 36 are arranged between the liquid phase outlet 49 of the first rectifying tower 17 and the first raw material liquid inlet 31 of the second rectifying tower 21, and a sixth regulating valve 6 is arranged between the product pump 23 and the product storage tank 24. A seventh regulating valve 7 is arranged between the third tee 13 and the inlet of the first reboiler 18, an eleventh regulating valve 35 is arranged between the third tee 13 and the inlet of the second reboiler 22, and a ninth regulating valve 9 is arranged between the shell side circulating gas outlet 42 and the circulating gas inlet of the heat pump 45.
A production method of a device for producing high-purity sulfur dioxide by using acid gas comprises the following steps:
step 1: the acid gas in the acid gas buffer tank 12 enters the combustion furnace 15 through the first regulating valve 1, the first cut-off valve 48 and the first inlet 39 of the combustion furnace 15, and the oxygen in the oxygen storage tank 47 enters the combustion furnace 15 through the eighth regulating valve 8, the second cut-off valve 51 and the second inlet 38 of the combustion furnace 15; the main components of the acid gas are as follows: methanol, hydrogen sulfide, carbon dioxide, nitrogenCarbon monoxide, hydrogen, carbonyl sulfide, sulfur dioxide and propane; the temperature of the acid gas is as follows: the temperature is 20-30 ℃ and the pressure is as follows: the flow rate of 0.2Mpa is: 28Nm 3 And (3) the gas phase fraction is: 0. the mole fraction of hydrogen sulfide is: 25-43%;
step 2: the acid gas and oxygen in the step 1 enter a combustion furnace 15 for combustion, heat exchange is carried out through a tube side of a waste heat boiler 16, the heat exchanged gas enters a first gas-liquid separator 25 for separating free water, the separated free water enters a waste liquid absorption tower 40 through a liquid phase outlet of the first gas-liquid separator 25, and the separated gas enters a drying and purifying tower 26 through a gas phase outlet of the first gas-liquid separator 25; gas phase outlet temperature of the first gas-liquid separator 25: 30-40 ℃ SO 2 Mole fraction: 30-40%;
step 3: drying, impurity removing and purifying the gas entering the drying and purifying tower 26 in the step 2 through a molecular sieve, and entering the purified raw material gas into a first rectifying tower 17; temperature of gas after passing through the drying and purifying column 26: 30-40 ℃ SO 2 55-65% of mole fraction;
step 4: the raw material gas entering the first rectifying tower 17 in the step 3 is subjected to primary rectifying purification, and liquid phase at the bottom of the first rectifying tower 17 after primary rectifying purification enters the second rectifying tower 21 through the third regulating valve 3 and the third cut-off valve 36, and the liquid phase temperature of the liquid phase outlet 49 at the bottom of the first rectifying tower 17: 16-25 ℃, flow rate: 11-15.4 Nm 3 /h、SO 2 Mole fraction: 97.6 to 99.9 percent;
step 5: subjecting the liquid phase entering the second rectifying tower 21 in the step 4 to secondary rectifying purification, wherein the gas phase after the secondary rectifying purification enters the second tee joint 11 through a top gas phase outlet of the second rectifying tower 21, a second raw material gas inlet 32 of the top condenser 20 and a second raw material liquid outlet 33 of the top condenser 20, and a part of the liquid phase in the second tee joint 11 enters the product tank 24 through the product pump 23; the other part of liquid phase in the second tee 11 flows back into the second rectifying tower 21 through the fifth regulating valve 5 and the second raw material liquid inlet 34 of the second rectifying tower 21; top gas phase outlet temperature of the second rectification column 21: 13-19 ℃, gas phase fraction: 1, a step of; top condenser 20 second feed solution Liquid phase temperature at outlet 33 into second rectification column 21: 11-17 ℃, gas phase fraction: 0; the top condenser 20 enters the liquid phase temperature at the inlet of the product pump 23 through the third end of the second tee 11: 11-17 ℃ SO 2 The purity of the product is not lower than 99.99%;
step 6: the gas phase after primary rectification and purification in the step 4 enters the second gas-liquid separator 19 through a gas phase outlet at the top of the first rectifying tower 17, a first raw material gas inlet 28 of the top condenser 20 and a first raw material liquid outlet 29 of the top condenser 20 for gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower 17 through a liquid phase outlet of the second gas-liquid separator 19 and a second regulating valve 2; gas phase temperature at the top gas phase outlet of the first rectifying column 17: 16-25 ℃ SO 2 Mole fraction: 63-72%, gas phase fraction: 1, a step of; the liquid phase temperature of the liquid phase outlet of the second gas-liquid separator 19 entering the first rectifying tower 17 is 15-22 ℃, SO 2 Mole fraction: 90-96%, gas phase fraction: 0;
step 7: the gas phase after gas-liquid separation in the second gas-liquid separator 19 in step 6 sequentially passes through the gas phase outlet of the second gas-liquid separator 19, the fourth regulating valve 4 and the first tee 10 to enter the desulfurizing tower 46, and the gas phase outlet temperature of the second gas-liquid separator 19 is: 15-22 ℃, flow rate: 4.4 to 7.2Nm 3 Gas phase fraction/h: 1, a step of;
step 8: the liquid phase after rectification and purification in the second rectifying tower 21 in the step 5 enters the desulfurizing tower 46 through the bottom liquid phase outlet 37 and the third end of the first tee 10, and the bottom liquid phase outlet 37 of the second rectifying tower 21 has the temperature: 14-20 ℃, flow: 5.5 to 9.6Nm 3 Gas phase fraction/h: 0;
step 9: circulating gas in the heat pump 45 respectively enters the first reboiler 18 and the second reboiler 22 through the third tee joint 13, circulating liquid in the outlet of the first reboiler 18 and the outlet of the second reboiler 22 respectively enters the shell side of the top condenser 20 through the fourth tee joint 14 and the shell side circulating liquid inlet 41 of the top condenser 20 for gasification, and gasified gas phase enters the heat pump 45 through the shell side circulating gas outlet 42 of the top condenser 20 and the circulating gas inlet of the heat pump 45; the outlet temperature of the first reboiler 18 is: 20-26 ℃, gas phase fraction: 0; the outlet temperature of the second reboiler 22 is: 16-22 ℃, gas phase fraction: 0; gas ammonia mole fraction of the shell side recycle gas outlet 42 of the top condenser 20: 100%, temperature: 9-13 ℃, gas phase fraction: 100%;
step 10: desalted water in the circulating water supply pipeline 44 enters the shell side of the waste heat boiler 16 through the tenth regulating valve 50 and the shell side inlet of the waste heat boiler 16, and the heat exchanged steam enters the steam pipe network 43 through the shell side outlet of the waste heat boiler 16.
The invention relates to a device and a production method for producing high-purity sulfur dioxide by adopting a mode of synthesizing acid gas and rectifying, wherein the quality of the high-purity sulfur dioxide product has no national standard, and the quality standard of high-purity sulfur dioxide in China is referred to the high-purity hydrogen sulfide enterprise standard of China industry gas institute and foreign gas company: 99.97% or more, and the highest purity of the quality technical index of foreign gas company: 99.98% (anhydrous grade), ref: the high-purity sulfur dioxide products in China are compared with similar products in foreign countries in the fourth volume of the general national institute of Industrial gases, 3711 th Page Table II.3.50-34 and Table II.3.50-35. The books are published by the university of the company, china industry gas industry Association. The process method has the advantages that on one hand, acid gas is utilized to carry out a synthesis reaction to generate low-concentration sulfur dioxide, then a drying and purifying tower is adopted to absorb some impurities in the reacted gas, so that the purity of the sulfur dioxide in the synthesis gas is improved, and after the synthesis gas enters a rectifying tower, a double-tower heat pump rectifying mode is adopted to realize high product purity and high energy utilization efficiency; on the other hand, the back of the acid gas buffer tank and the back of the oxygen storage tank are respectively provided with a self-regulating valve and a cut-off valve, when the temperature of the combustion furnace is unstable, the cut-off valve can be utilized to realize the function of rapidly cutting off raw gas; meanwhile, when the temperature of the combustion furnace is stable and the system is stably operated, the bypass pipeline regulating valve behind the oxygen storage tank can be utilized to finely regulate the oxygen content, so that the strict air distribution ratio is realized, and the stable regulation of the system is realized; when the system fluctuates or the purity of the product of the first rectifying tower is improper, the product of the second rectifying tower can be prevented from being influenced by utilizing a cut-off valve from the liquid phase outlet of the first rectifying tower to the first raw material liquid inlet of the second rectifying tower. The process method fully considers various conditions of the reaction of the acid gas and the oxygen in the combustion furnace, utilizes the micro-adjustment and observation of the flame condition in the combustion furnace, controls the oxygen content, ensures the complete reaction in the combustion furnace, and introduces a proper amount of nitrogen to take away heat during normal production so as to prevent the overtemperature of the combustion furnace. The water feeding amount of the circulating water automatically controls the temperature of the waste heat boiler, ensures the full utilization of the heat of the waste heat boiler, adopts double-tower rectification of the heat pump to produce high-purity sulfur dioxide, and has the characteristics of stable device, simple and convenient operation, low running cost, safety and controllability.
The invention will now be further illustrated with reference to examples for a more detailed explanation of the invention. Specific examples are as follows:
example 1
An apparatus for producing high-purity sulfur dioxide by using acid gas comprises an acid gas buffer tank 12, an oxygen storage tank 47, a product tank 24 and a waste liquid absorption tower 40, wherein the acid gas buffer tank 12 is connected with a first inlet 39 of a combustion furnace 15, the oxygen storage tank 47 is connected with a second inlet 38 of the combustion furnace 15, an outlet of the combustion furnace 15 is connected with a first gas-liquid separator 25 through a tube side of a waste heat boiler 16, and a gas phase outlet of the first gas-liquid separator 25 is connected with a first raw material gas inlet 27 of a first rectifying tower 17 through a drying and purifying tower 26 with molecular sieves; the liquid phase outlet 49 of the first rectifying tower 17 is connected with the first raw material liquid inlet 31 of the second rectifying tower 21 through a pipeline, the top gas phase outlet of the second rectifying tower 21 is connected with the second raw material gas inlet 32 of the top condenser 20, and the second raw material liquid outlet 33 of the top condenser 20 is connected with the product storage tank 24 through the second tee joint 11 and the product pump 23. The shell side inlet of the waste heat boiler 16 is connected with the circulating water supply pipeline 44 through a tenth regulating valve 50, and the shell side outlet of the waste heat boiler 16 is connected with the steam pipe network 43; the liquid phase outlet of the first gas-liquid separator 25 is connected to the waste liquid absorption column 40 through a pipe inclined downward. The gas phase outlet at the top of the first rectifying tower 17 is connected with the first raw material gas inlet 28 of the top condenser 20, the first raw material gas outlet 29 of the top condenser 20 is connected with the inlet of the second gas-liquid separator 19, the liquid phase outlet of the second gas-liquid separator 19 is connected with the second inlet 30 of the first rectifying tower 17 through the second regulating valve 2, and the gas phase outlet of the second gas-liquid separator 19 is connected with the inlet of the desulfurizing tower 46 sequentially through the fourth regulating valve 4 and the first tee joint 10. The third end of the second tee 11 is connected with a raw material liquid second inlet 34 of the second rectifying tower 21 through a fifth regulating valve 5. The bottom liquid phase outlet 37 of the second rectifying tower 21 is connected with the desulfurizing tower 46 through the third end of the first tee 10. The circulating gas outlet of the heat pump 45 is respectively connected with the inlets of the first reboiler 18 at the bottom of the first rectifying tower 17 and the second reboiler 22 at the bottom of the second rectifying tower 21 through the third tee joint 13, the outlets of the first reboiler 18 and the second reboiler 22 are respectively connected with the shell-side circulating liquid inlet 41 of the top condenser 20 through the fourth tee joint 14, and the shell-side circulating gas outlet 42 is connected with the circulating gas inlet of the heat pump 45. A first regulating valve 1 and a first cut-off valve 48 are sequentially arranged between the acid gas buffer tank 12 and the first inlet 39 of the combustion furnace 15, an eighth regulating valve 8 and a second cut-off valve 51 are arranged between the oxygen storage tank 47 and the second inlet 38 of the combustion furnace 15, a third regulating valve 3 and a third cut-off valve 36 are arranged between the liquid phase outlet 49 of the first rectifying tower 17 and the first raw material liquid inlet 31 of the second rectifying tower 21, and a sixth regulating valve 6 is arranged between the product pump 23 and the product storage tank 24. A seventh regulating valve 7 is arranged between the third tee 13 and the inlet of the first reboiler 18, an eleventh regulating valve 35 is arranged between the third tee 13 and the inlet of the second reboiler 22, and a ninth regulating valve 9 is arranged between the shell side circulating gas outlet 42 and the circulating gas inlet of the heat pump 45.
A production method of a device for producing high-purity sulfur dioxide by using acid gas comprises the following steps:
step 1: the acid gas in the acid gas buffer tank 12 enters the combustion furnace 15 through the first regulating valve 1, the first cut-off valve 48 and the first inlet 39 of the combustion furnace 15, and the oxygen in the oxygen storage tank 47 enters the combustion furnace 15 through the eighth regulating valve 8, the second cut-off valve 51 and the second inlet 38 of the combustion furnace 15; the main components of the acid gas are as follows: methanol, hydrogen sulfide, carbon dioxide, nitrogen, carbon monoxide, hydrogen, carbonyl sulfide, sulfur dioxide, and propane; the temperature of the acid gas is as follows: 20 ℃ and the pressure is as follows: the flow rate of 0.2Mpa is: 28Nm 3 /h, gas phaseThe dividing rate is as follows: 0. the mole fraction of hydrogen sulfide is: 25-43%;
step 2: the acid gas and oxygen in the step 1 enter a combustion furnace 15 for combustion, heat exchange is carried out through a tube side of a waste heat boiler 16, the heat exchanged gas enters a first gas-liquid separator 25 for separating free water, the separated free water enters a waste liquid absorption tower 40 through a liquid phase outlet of the first gas-liquid separator 25, and the separated gas enters a drying and purifying tower 26 through a gas phase outlet of the first gas-liquid separator 25; gas phase outlet temperature of the first gas-liquid separator 25: 30 ℃, SO 2 Mole fraction: 30-40%;
step 3: drying, impurity removing and purifying the gas entering the drying and purifying tower 26 in the step 2 through a molecular sieve, and entering the purified raw material gas into a first rectifying tower 17; temperature of gas after passing through the drying and purifying column 26: 30 ℃, SO 2 55-65% of mole fraction;
step 4: the raw material gas entering the first rectifying tower 17 in the step 3 is subjected to primary rectifying purification, and liquid phase at the bottom of the first rectifying tower 17 after primary rectifying purification enters the second rectifying tower 21 through the third regulating valve 3 and the third cut-off valve 36, and the liquid phase temperature of the liquid phase outlet 49 at the bottom of the first rectifying tower 17: 16 ℃, flow rate: 11-15.4 Nm 3 /h、SO 2 Mole fraction: 97.6 to 99.9 percent;
step 5: subjecting the liquid phase entering the second rectifying tower 21 in the step 4 to secondary rectifying purification, wherein the gas phase after the secondary rectifying purification enters the second tee joint 11 through a top gas phase outlet of the second rectifying tower 21, a second raw material gas inlet 32 of the top condenser 20 and a second raw material liquid outlet 33 of the top condenser 20, and a part of the liquid phase in the second tee joint 11 enters the product tank 24 through the product pump 23; the other part of liquid phase in the second tee 11 flows back into the second rectifying tower 21 through the fifth regulating valve 5 and the second raw material liquid inlet 34 of the second rectifying tower 21; top gas phase outlet temperature of the second rectification column 21: 13 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid outlet 33 of the top condenser 20 into the second rectifying column 21: 11 ℃, gas phase fraction: 0; the top condenser 20 enters the liquid phase temperature at the inlet of the product pump 23 through the third end of the second tee 11: 11 ℃, SO 2 The purity of the product is not lower than 99.99%;
step 6: the gas phase after primary rectification and purification in the step 4 enters the second gas-liquid separator 19 through a gas phase outlet at the top of the first rectifying tower 17, a first raw material gas inlet 28 of the top condenser 20 and a first raw material liquid outlet 29 of the top condenser 20 for gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower 17 through a liquid phase outlet of the second gas-liquid separator 19 and a second regulating valve 2; gas phase temperature at the top gas phase outlet of the first rectifying column 17: 16 ℃, SO 2 Mole fraction: 63-72%, gas phase fraction: 1, a step of; the liquid phase temperature of the liquid phase outlet of the second gas-liquid separator 19 entering the first rectifying tower 17 is 15 ℃, SO 2 Mole fraction: 90-96%, gas phase fraction: 0;
step 7: the gas phase after gas-liquid separation in the second gas-liquid separator 19 in step 6 sequentially passes through the gas phase outlet of the second gas-liquid separator 19, the fourth regulating valve 4 and the first tee 10 to enter the desulfurizing tower 46, and the gas phase outlet temperature of the second gas-liquid separator 19 is: 15 ℃, flow rate: 4.4Nm 3 Gas phase fraction/h: 1, a step of;
step 8: the liquid phase after rectification and purification in the second rectifying tower 21 in the step 5 enters the desulfurizing tower 46 through the bottom liquid phase outlet 37 and the third end of the first tee 10, and the bottom liquid phase outlet 37 of the second rectifying tower 21 has the temperature: 14 ℃, flow rate: 5.5Nm 3 Gas phase fraction/h: 0;
step 9: circulating gas in the heat pump 45 respectively enters the first reboiler 18 and the second reboiler 22 through the third tee joint 13, circulating liquid in the outlet of the first reboiler 18 and the outlet of the second reboiler 22 respectively enters the shell side of the top condenser 20 through the fourth tee joint 14 and the shell side circulating liquid inlet 41 of the top condenser 20 for gasification, and gasified gas phase enters the heat pump 45 through the shell side circulating gas outlet 42 of the top condenser 20 and the circulating gas inlet of the heat pump 45; the outlet temperature of the first reboiler 18 is: 20 ℃, gas phase fraction: 0; the outlet temperature of the second reboiler 22 is: 16 ℃, gas phase fraction: 0; gas ammonia mole fraction of the shell side recycle gas outlet 42 of the top condenser 20: 100%, temperature: 9 ℃, gas phase fraction: 100%;
step 10: desalted water in the circulating water supply pipeline 44 enters the shell side of the waste heat boiler 16 through the tenth regulating valve 50 and the shell side inlet of the waste heat boiler 16, and the heat exchanged steam enters the steam pipe network 43 through the shell side outlet of the waste heat boiler 16.
Example 2
An apparatus for producing high-purity sulfur dioxide by using acid gas comprises an acid gas buffer tank 12, an oxygen storage tank 47, a product tank 24 and a waste liquid absorption tower 40, wherein the acid gas buffer tank 12 is connected with a first inlet 39 of a combustion furnace 15, the oxygen storage tank 47 is connected with a second inlet 38 of the combustion furnace 15, an outlet of the combustion furnace 15 is connected with a first gas-liquid separator 25 through a tube side of a waste heat boiler 16, and a gas phase outlet of the first gas-liquid separator 25 is connected with a first raw material gas inlet 27 of a first rectifying tower 17 through a drying and purifying tower 26 with molecular sieves; the liquid phase outlet 49 of the first rectifying tower 17 is connected with the first raw material liquid inlet 31 of the second rectifying tower 21 through a pipeline, the top gas phase outlet of the second rectifying tower 21 is connected with the second raw material gas inlet 32 of the top condenser 20, and the second raw material liquid outlet 33 of the top condenser 20 is connected with the product storage tank 24 through the second tee joint 11 and the product pump 23. The shell side inlet of the waste heat boiler 16 is connected with the circulating water supply pipeline 44 through a tenth regulating valve 50, and the shell side outlet of the waste heat boiler 16 is connected with the steam pipe network 43; the liquid phase outlet of the first gas-liquid separator 25 is connected to the waste liquid absorption column 40 through a pipe inclined downward. The gas phase outlet at the top of the first rectifying tower 17 is connected with the first raw material gas inlet 28 of the top condenser 20, the first raw material gas outlet 29 of the top condenser 20 is connected with the inlet of the second gas-liquid separator 19, the liquid phase outlet of the second gas-liquid separator 19 is connected with the second inlet 30 of the first rectifying tower 17 through the second regulating valve 2, and the gas phase outlet of the second gas-liquid separator 19 is connected with the inlet of the desulfurizing tower 46 sequentially through the fourth regulating valve 4 and the first tee joint 10. The third end of the second tee 11 is connected with a raw material liquid second inlet 34 of the second rectifying tower 21 through a fifth regulating valve 5. The bottom liquid phase outlet 37 of the second rectifying tower 21 is connected with the desulfurizing tower 46 through the third end of the first tee 10. The circulating gas outlet of the heat pump 45 is respectively connected with the inlets of the first reboiler 18 at the bottom of the first rectifying tower 17 and the second reboiler 22 at the bottom of the second rectifying tower 21 through the third tee joint 13, the outlets of the first reboiler 18 and the second reboiler 22 are respectively connected with the shell-side circulating liquid inlet 41 of the top condenser 20 through the fourth tee joint 14, and the shell-side circulating gas outlet 42 is connected with the circulating gas inlet of the heat pump 45. A first regulating valve 1 and a first cut-off valve 48 are sequentially arranged between the acid gas buffer tank 12 and the first inlet 39 of the combustion furnace 15, an eighth regulating valve 8 and a second cut-off valve 51 are arranged between the oxygen storage tank 47 and the second inlet 38 of the combustion furnace 15, a third regulating valve 3 and a third cut-off valve 36 are arranged between the liquid phase outlet 49 of the first rectifying tower 17 and the first raw material liquid inlet 31 of the second rectifying tower 21, and a sixth regulating valve 6 is arranged between the product pump 23 and the product storage tank 24. A seventh regulating valve 7 is arranged between the third tee 13 and the inlet of the first reboiler 18, an eleventh regulating valve 35 is arranged between the third tee 13 and the inlet of the second reboiler 22, and a ninth regulating valve 9 is arranged between the shell side circulating gas outlet 42 and the circulating gas inlet of the heat pump 45.
A production method of a device for producing high-purity sulfur dioxide by using acid gas comprises the following steps:
step 1: the acid gas in the acid gas buffer tank 12 enters the combustion furnace 15 through the first regulating valve 1, the first cut-off valve 48 and the first inlet 39 of the combustion furnace 15, and the oxygen in the oxygen storage tank 47 enters the combustion furnace 15 through the eighth regulating valve 8, the second cut-off valve 51 and the second inlet 38 of the combustion furnace 15; the main components of the acid gas are as follows: methanol, hydrogen sulfide, carbon dioxide, nitrogen, carbon monoxide, hydrogen, carbonyl sulfide, sulfur dioxide, and propane; the temperature of the acid gas is as follows: the temperature and pressure are 30 DEG, the pressure is: the flow rate of 0.2Mpa is: 28Nm 3 And (3) the gas phase fraction is: 0. the mole fraction of hydrogen sulfide is: 25-43%;
step 2: the acid gas and oxygen in the step 1 enter a combustion furnace 15 for combustion, heat exchange is carried out through a tube side of a waste heat boiler 16, the heat exchanged gas enters a first gas-liquid separator 25 for separating free water, the separated free water enters a waste liquid absorption tower 40 through a liquid phase outlet of the first gas-liquid separator 25, and the separated gas enters a drying and purifying tower 26 through a gas phase outlet of the first gas-liquid separator 25; the first gasGas phase outlet temperature of the liquid separator 25: 40 ℃ SO 2 Mole fraction: 30-40%;
step 3: drying, impurity removing and purifying the gas entering the drying and purifying tower 26 in the step 2 through a molecular sieve, and entering the purified raw material gas into a first rectifying tower 17; temperature of gas after passing through the drying and purifying column 26: 40 ℃ SO 2 55-65% of mole fraction;
step 4: the raw material gas entering the first rectifying tower 17 in the step 3 is subjected to primary rectifying purification, and liquid phase at the bottom of the first rectifying tower 17 after primary rectifying purification enters the second rectifying tower 21 through the third regulating valve 3 and the third cut-off valve 36, and the liquid phase temperature of the liquid phase outlet 49 at the bottom of the first rectifying tower 17: 25 ℃, flow rate: 11-15.4 Nm 3 /h、SO 2 Mole fraction: 97.6 to 99.9 percent;
step 5: subjecting the liquid phase entering the second rectifying tower 21 in the step 4 to secondary rectifying purification, wherein the gas phase after the secondary rectifying purification enters the second tee joint 11 through a top gas phase outlet of the second rectifying tower 21, a second raw material gas inlet 32 of the top condenser 20 and a second raw material liquid outlet 33 of the top condenser 20, and a part of the liquid phase in the second tee joint 11 enters the product tank 24 through the product pump 23; the other part of liquid phase in the second tee 11 flows back into the second rectifying tower 21 through the fifth regulating valve 5 and the second raw material liquid inlet 34 of the second rectifying tower 21; top gas phase outlet temperature of the second rectification column 21: 19 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid outlet 33 of the top condenser 20 into the second rectifying column 21: 17 ℃, gas phase fraction: 0; the top condenser 20 enters the liquid phase temperature at the inlet of the product pump 23 through the third end of the second tee 11: 17 ℃, SO 2 The purity of the product is not lower than 99.99%;
step 6: the gas phase after primary rectification and purification in the step 4 enters the second gas-liquid separator 19 through a gas phase outlet at the top of the first rectifying tower 17, a first raw material gas inlet 28 of the top condenser 20 and a first raw material liquid outlet 29 of the top condenser 20 for gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower 17 through a liquid phase outlet of the second gas-liquid separator 19 and a second regulating valve 2; the top of the first rectifying tower 17Gas phase temperature at gas phase outlet: 25 ℃, SO 2 Mole fraction: 63-72%, gas phase fraction: 1, a step of; the liquid phase temperature of the liquid phase outlet of the second gas-liquid separator 19 entering the first rectifying tower 17 is 22 ℃, SO 2 Mole fraction: 90-96%, gas phase fraction: 0;
step 7: the gas phase after gas-liquid separation in the second gas-liquid separator 19 in step 6 sequentially passes through the gas phase outlet of the second gas-liquid separator 19, the fourth regulating valve 4 and the first tee 10 to enter the desulfurizing tower 46, and the gas phase outlet temperature of the second gas-liquid separator 19 is: 22 ℃, flow rate: 7.2Nm 3 Gas phase fraction/h: 1, a step of;
step 8: the liquid phase after rectification and purification in the second rectifying tower 21 in the step 5 enters the desulfurizing tower 46 through the bottom liquid phase outlet 37 and the third end of the first tee 10, and the bottom liquid phase outlet 37 of the second rectifying tower 21 has the temperature: 20 ℃, flow: 9.6Nm 3 Gas phase fraction/h: 0;
step 9: circulating gas in the heat pump 45 respectively enters the first reboiler 18 and the second reboiler 22 through the third tee joint 13, circulating liquid in the outlet of the first reboiler 18 and the outlet of the second reboiler 22 respectively enters the shell side of the top condenser 20 through the fourth tee joint 14 and the shell side circulating liquid inlet 41 of the top condenser 20 for gasification, and gasified gas phase enters the heat pump 45 through the shell side circulating gas outlet 42 of the top condenser 20 and the circulating gas inlet of the heat pump 45; the outlet temperature of the first reboiler 18 is: 20-26 ℃, gas phase fraction: 0; the outlet temperature of the second reboiler 22 is: 22 ℃, gas phase fraction: 0; gas ammonia mole fraction of the shell side recycle gas outlet 42 of the top condenser 20: 100%, temperature: 13 ℃, gas phase fraction: 100%;
step 10: desalted water in the circulating water supply pipeline 44 enters the shell side of the waste heat boiler 16 through the tenth regulating valve 50 and the shell side inlet of the waste heat boiler 16, and the heat exchanged steam enters the steam pipe network 43 through the shell side outlet of the waste heat boiler 16.
Example 3
An apparatus for producing high-purity sulfur dioxide by using acid gas comprises an acid gas buffer tank 12, an oxygen storage tank 47, a product tank 24 and a waste liquid absorption tower 40, wherein the acid gas buffer tank 12 is connected with a first inlet 39 of a combustion furnace 15, the oxygen storage tank 47 is connected with a second inlet 38 of the combustion furnace 15, an outlet of the combustion furnace 15 is connected with a first gas-liquid separator 25 through a tube side of a waste heat boiler 16, and a gas phase outlet of the first gas-liquid separator 25 is connected with a first raw material gas inlet 27 of a first rectifying tower 17 through a drying and purifying tower 26 with molecular sieves; the liquid phase outlet 49 of the first rectifying tower 17 is connected with the first raw material liquid inlet 31 of the second rectifying tower 21 through a pipeline, the top gas phase outlet of the second rectifying tower 21 is connected with the second raw material gas inlet 32 of the top condenser 20, and the second raw material liquid outlet 33 of the top condenser 20 is connected with the product storage tank 24 through the second tee joint 11 and the product pump 23. The shell side inlet of the waste heat boiler 16 is connected with the circulating water supply pipeline 44 through a tenth regulating valve 50, and the shell side outlet of the waste heat boiler 16 is connected with the steam pipe network 43; the liquid phase outlet of the first gas-liquid separator 25 is connected to the waste liquid absorption column 40 through a pipe inclined downward. The gas phase outlet at the top of the first rectifying tower 17 is connected with the first raw material gas inlet 28 of the top condenser 20, the first raw material gas outlet 29 of the top condenser 20 is connected with the inlet of the second gas-liquid separator 19, the liquid phase outlet of the second gas-liquid separator 19 is connected with the second inlet 30 of the first rectifying tower 17 through the second regulating valve 2, and the gas phase outlet of the second gas-liquid separator 19 is connected with the inlet of the desulfurizing tower 46 sequentially through the fourth regulating valve 4 and the first tee joint 10. The third end of the second tee 11 is connected with a raw material liquid second inlet 34 of the second rectifying tower 21 through a fifth regulating valve 5. The bottom liquid phase outlet 37 of the second rectifying tower 21 is connected with the desulfurizing tower 46 through the third end of the first tee 10. The circulating gas outlet of the heat pump 45 is respectively connected with the inlets of the first reboiler 18 at the bottom of the first rectifying tower 17 and the second reboiler 22 at the bottom of the second rectifying tower 21 through the third tee joint 13, the outlets of the first reboiler 18 and the second reboiler 22 are respectively connected with the shell-side circulating liquid inlet 41 of the top condenser 20 through the fourth tee joint 14, and the shell-side circulating gas outlet 42 is connected with the circulating gas inlet of the heat pump 45. A first regulating valve 1 and a first cut-off valve 48 are sequentially arranged between the acid gas buffer tank 12 and the first inlet 39 of the combustion furnace 15, an eighth regulating valve 8 and a second cut-off valve 51 are arranged between the oxygen storage tank 47 and the second inlet 38 of the combustion furnace 15, a third regulating valve 3 and a third cut-off valve 36 are arranged between the liquid phase outlet 49 of the first rectifying tower 17 and the first raw material liquid inlet 31 of the second rectifying tower 21, and a sixth regulating valve 6 is arranged between the product pump 23 and the product storage tank 24. A seventh regulating valve 7 is arranged between the third tee 13 and the inlet of the first reboiler 18, an eleventh regulating valve 35 is arranged between the third tee 13 and the inlet of the second reboiler 22, and a ninth regulating valve 9 is arranged between the shell side circulating gas outlet 42 and the circulating gas inlet of the heat pump 45.
A production method of a device for producing high-purity sulfur dioxide by using acid gas comprises the following steps:
step 1: the acid gas in the acid gas buffer tank 12 enters the combustion furnace 15 through the first regulating valve 1, the first cut-off valve 48 and the first inlet 39 of the combustion furnace 15, and the oxygen in the oxygen storage tank 47 enters the combustion furnace 15 through the eighth regulating valve 8, the second cut-off valve 51 and the second inlet 38 of the combustion furnace 15; the main components of the acid gas are as follows: methanol, hydrogen sulfide, carbon dioxide, nitrogen, carbon monoxide, hydrogen, carbonyl sulfide, sulfur dioxide, and propane; the temperature of the acid gas is as follows: 25 ℃ and the pressure is: the flow rate of 0.2Mpa is: 28Nm 3 And (3) the gas phase fraction is: 0. the mole fraction of hydrogen sulfide is: 25-43%;
step 2: the acid gas and oxygen in the step 1 enter a combustion furnace 15 for combustion, heat exchange is carried out through a tube side of a waste heat boiler 16, the heat exchanged gas enters a first gas-liquid separator 25 for separating free water, the separated free water enters a waste liquid absorption tower 40 through a liquid phase outlet of the first gas-liquid separator 25, and the separated gas enters a drying and purifying tower 26 through a gas phase outlet of the first gas-liquid separator 25; gas phase outlet temperature of the first gas-liquid separator 25: 35 ℃, SO 2 Mole fraction: 30-40%;
step 3: drying, impurity removing and purifying the gas entering the drying and purifying tower 26 in the step 2 through a molecular sieve, and entering the purified raw material gas into a first rectifying tower 17; temperature of gas after passing through the drying and purifying column 26: 35 ℃, SO 2 55-65% of mole fraction;
step 4: the raw material fed into the first rectifying tower 17 in the step 3The material gas is subjected to primary rectification purification, liquid phase at the bottom of the first rectification tower 17 after primary rectification purification enters the second rectification tower 21 through the third regulating valve 3 and the third cut-off valve 36, and the liquid phase temperature of a liquid phase outlet 49 at the bottom of the first rectification tower 17: 20.5 ℃, flow: 11-15.4 Nm 3 /h、SO 2 Mole fraction: 97.6 to 99.9 percent;
step 5: subjecting the liquid phase entering the second rectifying tower 21 in the step 4 to secondary rectifying purification, wherein the gas phase after the secondary rectifying purification enters the second tee joint 11 through a top gas phase outlet of the second rectifying tower 21, a second raw material gas inlet 32 of the top condenser 20 and a second raw material liquid outlet 33 of the top condenser 20, and a part of the liquid phase in the second tee joint 11 enters the product tank 24 through the product pump 23; the other part of liquid phase in the second tee 11 flows back into the second rectifying tower 21 through the fifth regulating valve 5 and the second raw material liquid inlet 34 of the second rectifying tower 21; top gas phase outlet temperature of the second rectification column 21: 16 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second feed liquid outlet 33 of the top condenser 20 into the second rectifying column 21: 14 ℃, gas phase fraction: 0; the top condenser 20 enters the liquid phase temperature at the inlet of the product pump 23 through the third end of the second tee 11: 14 ℃, SO 2 The purity of the product is not lower than 99.99%;
step 6: the gas phase after primary rectification and purification in the step 4 enters the second gas-liquid separator 19 through a gas phase outlet at the top of the first rectifying tower 17, a first raw material gas inlet 28 of the top condenser 20 and a first raw material liquid outlet 29 of the top condenser 20 for gas-liquid separation, and the liquid phase after gas-liquid separation enters the first rectifying tower 17 through a liquid phase outlet of the second gas-liquid separator 19 and a second regulating valve 2; gas phase temperature at the top gas phase outlet of the first rectifying column 17: 20.5 ℃ SO 2 Mole fraction: 63-72%, gas phase fraction: 1, a step of; the liquid phase temperature of the liquid phase outlet of the second gas-liquid separator 19 entering the first rectifying tower 17 is 18.5 ℃, SO 2 Mole fraction: 90-96%, gas phase fraction: 0;
step 7: the gas phase after the gas-liquid separation in the second gas-liquid separator 19 in the step 6 passes through the gas phase outlet of the second gas-liquid separator 19, the fourth regulating valve 4 and the first valve in sequenceThe tee 10 enters the desulfurizing tower 46, and the gas phase outlet temperature of the second gas-liquid separator 19 is as follows: 18.5 ℃, flow rate: 5.8Nm 3 Gas phase fraction/h: 1, a step of;
step 8: the liquid phase after rectification and purification in the second rectifying tower 21 in the step 5 enters the desulfurizing tower 46 through the bottom liquid phase outlet 37 and the third end of the first tee 10, and the bottom liquid phase outlet 37 of the second rectifying tower 21 has the temperature: 17 ℃, flow rate: 7.5Nm 3 Gas phase fraction/h: 0;
step 9: circulating gas in the heat pump 45 respectively enters the first reboiler 18 and the second reboiler 22 through the third tee joint 13, circulating liquid in the outlet of the first reboiler 18 and the outlet of the second reboiler 22 respectively enters the shell side of the top condenser 20 through the fourth tee joint 14 and the shell side circulating liquid inlet 41 of the top condenser 20 for gasification, and gasified gas phase enters the heat pump 45 through the shell side circulating gas outlet 42 of the top condenser 20 and the circulating gas inlet of the heat pump 45; the outlet temperature of the first reboiler 18 is: 23 ℃, gas phase fraction: 0; the outlet temperature of the second reboiler 22 is: 19 ℃, gas phase fraction: 0; gas ammonia mole fraction of the shell side recycle gas outlet 42 of the top condenser 20: 100%, temperature: 11 ℃, gas phase fraction: 100%;
step 10: desalted water in the circulating water supply pipeline 44 enters the shell side of the waste heat boiler 16 through the tenth regulating valve 50 and the shell side inlet of the waste heat boiler 16, and the heat exchanged steam enters the steam pipe network 43 through the shell side outlet of the waste heat boiler 16.
In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the terms "end," "inner wall," "front end," etc. are based on the orientation or positional relationship shown in the drawings, and are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element in question must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. In the description of the present invention, it should be noted that, unless explicitly stated and limited otherwise, the terms "provided with," "mounted to," "connected to," and the like are to be construed broadly, and may be, for example, fixedly connected, integrally connected, or detachably connected; or the communication between the two components is also possible; may be directly connected or indirectly connected through an intermediate medium, and the specific meaning of the above terms in the present invention will be understood by those skilled in the art according to the specific circumstances. Finally, it is noted that the above-mentioned preferred embodiments are only intended to illustrate rather than limit the invention, and that, although the invention has been described in detail by means of the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. An apparatus for producing high purity sulfur dioxide by using acid gas, the apparatus comprising an acid gas buffer tank (12), an oxygen storage tank (47), a product tank (24) and a waste liquid absorption tower (40), characterized in that: the acid gas buffer tank (12) is connected with a first inlet (39) of the combustion furnace (15), the oxygen storage tank (47) is connected with a second inlet (38) of the combustion furnace (15), an outlet of the combustion furnace (15) is connected with the first gas-liquid separator (25) through a tube side of the waste heat boiler (16), and a gas phase outlet of the first gas-liquid separator (25) is connected with a first raw material gas inlet (27) of the first rectifying tower (17) through a drying and purifying tower (26) with molecular sieve;
the liquid phase outlet (49) of the first rectifying tower (17) is connected with the first raw material liquid inlet (31) of the second rectifying tower (21) through a pipeline, the top gas phase outlet of the second rectifying tower (21) is connected with the second raw material gas inlet (32) of the top condenser (20), and the second raw material liquid outlet (33) of the top condenser (20) is connected with the product storage tank (24) through a second tee joint (11) and a product pump (23);
the liquid phase outlet of the first gas-liquid separator (25) is connected with the waste liquid absorption tower (40) through a pipeline which is inclined downwards.
2. An apparatus for producing high purity sulfur dioxide from sour gas according to claim 1, wherein: the shell side inlet of the waste heat boiler (16) is connected with a circulating water supply pipeline (44) through a tenth regulating valve (50), and the shell side outlet of the waste heat boiler (16) is connected with a steam pipe network (43).
3. An apparatus for producing high purity sulfur dioxide from sour gas according to claim 1, wherein: the gas phase outlet at the top of the first rectifying tower (17) is connected with a first raw material gas inlet (28) of a top condenser (20), a first raw material gas outlet (29) of the top condenser (20) is connected with an inlet of a second gas-liquid separator (19), a liquid phase outlet of the second gas-liquid separator (19) is connected with a second inlet (30) of the first rectifying tower (17) through a second regulating valve (2), and a gas phase outlet of the second gas-liquid separator (19) is sequentially connected with an inlet of a desulfurizing tower (46) through a fourth regulating valve (4) and a first tee joint (10).
4. An apparatus for producing high purity sulfur dioxide from sour gas according to claim 1, wherein: the third end of the second tee joint (11) is connected with a raw material liquid second inlet (34) of the second rectifying tower (21) through a fifth regulating valve (5).
5. An apparatus for producing high purity sulfur dioxide from sour gas according to claim 1, wherein: the bottom liquid phase outlet (37) of the second rectifying tower (21) is connected with the desulfurizing tower (46) through the third end of the first tee joint (10).
6. An apparatus for producing high purity sulfur dioxide from sour gas according to claim 1, wherein: the circulating gas outlet of the heat pump (45) is connected with the inlets of a first reboiler (18) at the bottom of the first rectifying tower (17) and a second reboiler (22) at the bottom of the second rectifying tower (21) through a third tee joint (13), the outlets of the first reboiler (18) and the second reboiler (22) are connected with a shell side circulating liquid inlet (41) of the top condenser (20) through a fourth tee joint (14), and a shell side circulating gas outlet (42) is connected with a circulating gas inlet of the heat pump (45).
7. An apparatus for producing high purity sulfur dioxide from sour gas according to claim 1, wherein: the acid gas buffer tank is characterized in that a first regulating valve (1) and a first cut-off valve (48) are sequentially arranged between the acid gas buffer tank (12) and a first inlet (39) of the combustion furnace (15), an eighth regulating valve (8) and a second cut-off valve (51) are arranged between an oxygen storage tank (47) and a second inlet (38) of the combustion furnace (15), a third regulating valve (3) and a third cut-off valve (36) are arranged between a liquid phase outlet (49) of the first rectifying tower (17) and a first raw material liquid inlet (31) of the second rectifying tower (21), and a sixth regulating valve (6) is arranged between a product pump (23) and a product storage tank (24).
8. An apparatus for producing high purity sulfur dioxide utilizing sour gas as defined in claim 6 wherein: a seventh regulating valve (7) is arranged between the third tee joint (13) and the inlet of the first reboiler (18), an eleventh regulating valve (35) is arranged between the third tee joint (13) and the inlet of the second reboiler (22), and a ninth regulating valve (9) is arranged between the shell side circulating gas outlet (42) and the circulating gas inlet of the heat pump (45).
9. A method for producing an apparatus for producing high purity sulfur dioxide using acid gas as claimed in any one of claims 1 to 8, wherein: the method comprises the following steps:
Step 1: the acid gas in the acid gas buffer tank (12) enters the combustion furnace (15) through a first regulating valve (1), a first cut-off valve (48) and a first inlet (39) of the combustion furnace (15), and the oxygen in the oxygen storage tank (47) enters the combustion furnace (15) through an eighth regulating valve (8), a second cut-off valve (51) and a second inlet (38) of the combustion furnace (15); the main components of the acid gas are as follows: methanol, hydrogen sulfide, carbon dioxide, nitrogen, carbon monoxide, hydrogen, carbonyl sulfide, sulfur dioxide, and propane; the temperature of the acid gas is as follows: the temperature is 20-30 ℃ and the pressure is as follows: the flow rate of 0.2Mpa is: 28Nm 3 And (3) the gas phase fraction is: 0. the mole fraction of hydrogen sulfide is: 25-43%;
step 2: the acid gas and oxygen in the step 1 enter a combustion furnace (15) for combustion, heat exchange is carried out through a tube side of a waste heat boiler (16), the heat exchanged gas enters a first gas-liquid separator (25) for separating free water, and the separated free water enters a waste liquid suction device through a liquid phase outlet of the first gas-liquid separator (25)A receiving tower (40), wherein the separated gas enters a drying and purifying tower (26) through a gas phase outlet of a first gas-liquid separator (25); gas phase outlet temperature of the first gas-liquid separator (25): 30-40 ℃ SO 2 Mole fraction: 30-40%;
Step 3: drying, impurity removing and purifying the gas entering the drying and purifying tower (26) in the step 2 through a molecular sieve, and entering the purified raw material gas into a first rectifying tower (17); temperature of gas after passing through the drying and purifying column (26): 30-40 ℃ SO 2 55-65% of mole fraction;
step 4: the raw material gas entering the first rectifying tower (17) in the step 3 is subjected to primary rectifying purification, liquid phase at the bottom of the first rectifying tower (17) after primary rectifying purification enters the second rectifying tower (21) through a third regulating valve (3) and a third cut-off valve (36), and liquid phase temperature of a liquid phase outlet (49) at the bottom of the first rectifying tower (17) is higher than that of the liquid phase: 16-25 ℃, flow rate: 11-15.4 Nm 3 /h、SO 2 Mole fraction: 97.6 to 99.9 percent;
step 5: the liquid phase entering the second rectifying tower (21) in the step 4 is subjected to secondary rectifying purification, and gas phase after the secondary rectifying purification enters a second tee joint (11) through a top gas phase outlet of the second rectifying tower (21), a second raw material gas inlet (32) of a top condenser (20) and a second raw material liquid outlet (33) of the top condenser (20), and a part of liquid phase in the second tee joint (11) enters a product tank (24) through a product pump (23); the other part of liquid phase in the second tee joint (11) flows back into the second rectifying tower (21) through the fifth regulating valve (5) and the second raw material liquid inlet (34) of the second rectifying tower (21); top gas phase outlet temperature of the second rectifying column (21): 13-19 ℃, gas phase fraction: 1, a step of; liquid phase temperature of the second raw material liquid outlet (33) of the top condenser (20) entering the second rectifying tower (21): 11-17 ℃, gas phase fraction: 0; the top condenser (20) enters the liquid phase temperature of the inlet of the product pump (23) through the third end of the second tee joint (11): 11-17 ℃ SO 2 The purity of the product is not lower than 99.99%;
step 6: the gas phase after primary rectification purification in the step 4 passes through a gas phase outlet at the top of a first rectifying tower (17), a first raw material gas inlet (28) of a top condenser (20) and a first raw material gas inlet of the top condenser (20)The raw material liquid outlet (29) enters the second gas-liquid separator (19) to carry out gas-liquid separation, and the liquid phase after the gas-liquid separation enters the first rectifying tower (17) through the liquid phase outlet of the second gas-liquid separator (19) and the second regulating valve (2); gas phase temperature at the top gas phase outlet of the first rectifying tower (17): 16-25 ℃ SO 2 Mole fraction: 63-72%, gas phase fraction: 1, a step of; the liquid phase temperature of the liquid phase outlet of the second gas-liquid separator (19) entering the first rectifying tower (17) is 15-22 ℃, SO 2 Mole fraction: 90-96%, gas phase fraction: 0;
step 7: the gas phase after gas-liquid separation in the second gas-liquid separator (19) in the step 6 sequentially passes through a gas phase outlet of the second gas-liquid separator (19), a fourth regulating valve (4) and a first tee joint (10) to enter a desulfurizing tower (46), and the gas phase outlet temperature of the second gas-liquid separator (19) is as follows: 15-22 ℃, flow rate: 4.4 to 7.2Nm 3 Gas phase fraction/h: 1, a step of;
step 8: the liquid phase purified by rectification in the second rectifying tower (21) in the step 5 enters the desulfurizing tower (46) through a bottom liquid phase outlet (37) and a third end of the first tee joint (10), and the temperature of the bottom liquid phase outlet (37) of the second rectifying tower (21) is as follows: 14-20 ℃, flow: 5.5 to 9.6Nm 3 Gas phase fraction/h: 0;
step 9: circulating gas in the heat pump (45) respectively enters the first reboiler (18) and the second reboiler (22) through the third tee joint (13), circulating liquid in the outlet of the first reboiler (18) and the outlet of the second reboiler (22) respectively enters the shell side of the top condenser (20) through the fourth tee joint (14) and the shell side circulating liquid inlet (41) of the top condenser (20) for gasification, and gasified gas phase enters the heat pump (45) through the shell side circulating gas outlet (42) of the top condenser (20) and the circulating gas inlet of the heat pump (45); the outlet temperature of the first reboiler (18) is: 20-26 ℃, gas phase fraction: 0; the outlet temperature of the second reboiler (22) is: 16-22 ℃, gas phase fraction: 0; gas ammonia mole fraction of the shell side recycle gas outlet (42) of the top condenser (20): 100%, temperature: 9-13 ℃, gas phase fraction: 100%;
step 10: desalted water in the circulating water supply pipeline (44) enters the shell side of the waste heat boiler (16) through a tenth regulating valve (50) and a shell side inlet of the waste heat boiler (16), and heat exchanged steam enters a steam pipe network (43) through a shell side outlet of the waste heat boiler (16).
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| CN111141108B (en) * | 2020-03-06 | 2024-02-13 | 河南心连心深冷能源股份有限公司 | Rectification purification device and purification process for liquid sulfur dioxide |
| JPWO2021182045A1 (en) * | 2020-03-09 | 2021-09-16 | ||
| CN113654034B (en) * | 2021-07-20 | 2023-08-29 | 山东联盟化工股份有限公司 | Comprehensive recycling method for low-grade steam containing acidic noncondensable gas |
| CN113562702B (en) * | 2021-08-25 | 2022-11-01 | 福建福豆新材料有限公司 | Method for purifying high-purity electronic-grade sulfur dioxide |
| CN114291795B (en) * | 2022-01-18 | 2023-04-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing high-purity sulfur dioxide |
| CN115340072B (en) * | 2022-09-14 | 2024-01-26 | 江西洪安化工有限公司 | Sulfur dioxide gas preparation system and method |
| CN115854653B (en) * | 2023-02-27 | 2023-05-12 | 河南心连心深冷能源股份有限公司 | Device and production process for producing lean krypton-xenon and ultra-pure oxygen by adopting same heat pump |
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