CN118702541A - Method for purifying CFC-113 mixture - Google Patents
Method for purifying CFC-113 mixture Download PDFInfo
- Publication number
- CN118702541A CN118702541A CN202411170228.5A CN202411170228A CN118702541A CN 118702541 A CN118702541 A CN 118702541A CN 202411170228 A CN202411170228 A CN 202411170228A CN 118702541 A CN118702541 A CN 118702541A
- Authority
- CN
- China
- Prior art keywords
- tower
- hcl
- cfc
- azeotropic
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000203 mixture Substances 0.000 title claims abstract description 32
- AJDIZQLSFPQPEY-UHFFFAOYSA-N 1,1,2-Trichlorotrifluoroethane Chemical compound FC(F)(Cl)C(F)(Cl)Cl AJDIZQLSFPQPEY-UHFFFAOYSA-N 0.000 title claims abstract 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000003507 refrigerant Substances 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 4
- 239000002699 waste material Substances 0.000 abstract description 26
- 239000003513 alkali Substances 0.000 abstract description 23
- 239000002253 acid Substances 0.000 abstract description 14
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 56
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 51
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 51
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 33
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 29
- 238000005406 washing Methods 0.000 description 17
- 239000007789 gas Substances 0.000 description 15
- 239000007795 chemical reaction product Substances 0.000 description 8
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000012043 crude product Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- BOSAWIQFTJIYIS-UHFFFAOYSA-N 1,1,1-trichloro-2,2,2-trifluoroethane Chemical compound FC(F)(F)C(Cl)(Cl)Cl BOSAWIQFTJIYIS-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- 241000736911 Turritella communis Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for purifying a CFC-113 mixture, which specifically comprises the following steps: step S1, directly delivering the CFC-113 mixture produced by the reactor to the middle part of an HCL rectifying tower, and utilizing the heat energy of the CFC-113 mixture to enable HCL gas to be produced from the top of the HCL rectifying tower, wherein materials containing CL 2 and HF at the bottom of the HCL rectifying tower are directly delivered to an azeotropic tower; and S2, feeding materials at the bottom of the HCL rectifying tower from the middle part of an azeotropic tower through a pump A, wherein in the azeotropic tower, CL 2 and HF in organic matters form an azeotrope to be produced from the top of the azeotropic tower, and obtaining a purified CFC-113 product at the bottom of the azeotropic tower. The beneficial effects of the invention are as follows: 1. the flow is simple, and the operation cost is low; the three wastes are less; the HF utilization rate is high; the CL 2 has high utilization rate; HCL yield is high; by adopting the process, water and alkali liquor do not need to be added, waste acid and waste alkali are not generated in the process, and corrosion of the device is reduced.
Description
Technical Field
The invention relates to the technical field of mixture purification, in particular to a method for purifying a CFC-113 mixture.
Background
1, 2-Trichloro-1, 2-trifluoroethane (CFC-113) is a widely used chemical product, and can be used as a raw material for cleaning agents and other chemical products. The industrial production of CFC-113 mainly uses tetrachloroethylene, chlorine gas and hydrogen fluoride as raw materials, and synthesizes CFC-113 under the action of catalyst. The main reaction equation is as follows:
CCL2CCL2+CL2 CCL3CCL3
CCL3CCL3+3HFCCL2FCCLF2+3HCL
The crude reactor product mixture is produced in the gas phase, which contains HF, HCL, CL 2 and other byproduct organics in addition to CFC-113. The prior purification process is shown in figure 1, and comprises the following specific steps:
S1, the crude reaction mixture is firstly subjected to three-stage condensation by a primary cooler 1, an intercooler 2 and a tail cooler 3, then is sent to a cryogenic condenser 4, most of uncondensed HCL gas, trace hydrogen fluoride and trifluorotrichloroethane enter a gas phase water washing system for treatment, most of hydrogen fluoride, trifluorotrichloroethane and part of hydrogen chloride are output from the bottom of a circulating tower 5 and then are sent to a layering device 7, and the bottom of the circulating tower 5 is communicated with a reboiler 6.
S2, the mixture is separated into an HF phase and an organic phase in a delaminator 7, the HF phase (containing a small amount of HCL, CL 2 and organic matters) at the top of the delaminator 7 is circulated back to the reactor to continue the reaction, and the organic phase (containing a small amount of HCL, CL 2 and HF) at the bottom of the delaminator 7 is sent to a deacidification tower 10 through an acid receiving tank 8 and a pump 9.
S3, conveying HCL, CL 2 and HF which are produced at the top of the deacidification tower 10 to a tail gas absorption system, sequentially conveying organic materials at the bottom of the deacidification tower 10 to a water washing tower 12, an alkaline washing tower 13 and a drying tower 14 through a pump 9 and a cooler 11, washing, alkaline washing and drying to obtain an organic crude product, and rectifying to obtain CFC-113.
The prior art has the following defects:
1. The flow is complex
The existing separation process flow of CFC-113 reaction products is complex, and comprises a plurality of process units of condensation, circulation, deacidification, water washing, alkali washing, drying, rectification and the like, and has the advantages of multiple equipment sets, wide occupied area of the device and large equipment investment.
2. High energy consumption
1) The crude product from the reaction kettle is gas phase, all organic matters and part of HCL are condensed into liquid in the condensation process, a large amount of refrigerant is consumed in the process, heat is released in the water alkali washing process, the part of heat is cooled by the refrigerant, the consumption of the refrigerant is increased, and an electric heater is also needed in the drying unit to provide heat energy.
In summary, the process requires a great deal of public engineering and electricity consumption, and the production and operation costs of the device are high.
3. HF utilization is low
The crude reaction product also contains a large amount of HF, a part of HF returns to the reactor from the upper part through the layering device to continue the reaction, but part of HF is dissolved in organic matters at the bottom of the layering device, and finally the part of HF is removed through water washing and alkali washing, waste acid and waste alkali are generated in the process, three wastes are generated, and the unit consumption of HF is increased.
4. CL 2 has high unit consumption
The CL 2 in the crude reaction product is finally extracted from the top of the deacidification tower and sent to a tail gas absorption system, and the part of CL 2 is finally changed into waste acid and waste alkali, so that three wastes are generated, and the unit consumption of CL 2 is increased.
5. HCL yield is low
In the process, a small amount of HCL part can be extracted from the top of the deacidification tower and sent to a tail gas absorption system, and the part of HCL can be finally changed into waste acid and waste alkali, so that three wastes are generated, and the yield of HCL is reduced.
6. Three wastes are more
The acid gas at the top of the deacidification tower and the acid organic matters at the bottom of the deacidification tower are all required to be washed by water and alkali to remove the acid matters, and a large amount of waste acid and waste alkali are generated in the water and alkali washing process; the drying unit can produce waste molecular sieve solids, so the three wastes are treated with high cost.
7. Severe corrosion of the device
During the water alkali washing process, hydrofluoric acid, hydrochloric acid, alkali liquor and inorganic salt are generated due to the addition of water and alkali liquor. These materials are prone to corrosion in equipment, devices and piping.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for purifying a CFC-113 mixture.
The aim of the invention is achieved by the following technical scheme. A process for purifying a mixture of CFC-113, comprising separating HF, HCL, CL 2 from a mixture of 1, 2-trichloro-1, 2-trifluoroethane (CFC-113) containing Hydrogen Fluoride (HF), hydrogen Chloride (HCL), chlorine (CL 2), to obtain CFC-113 of high purity, comprising the steps of:
Step S1, directly delivering the CFC-113 mixture produced by the reactor to the middle part of an HCL rectifying tower, and utilizing the heat energy of the CFC-113 mixture to enable HCL gas to be produced from the top of the HCL rectifying tower, wherein materials containing CL 2 and HF at the bottom of the HCL rectifying tower are directly delivered to an azeotropic tower;
And S2, feeding materials at the bottom of the HCL rectifying tower from the middle part of an azeotropic tower through a pump A, wherein in the azeotropic tower, CL 2 and HF in organic matters form an azeotrope to be produced from the top of the azeotropic tower, and obtaining a purified CFC-113 product at the bottom of the azeotropic tower.
Further, in step S1, the top of the HCL rectifying column is condensed by a refrigerant using a condenser a, and HCL gas having a purity of 99.9% is obtained from the top of the HCL rectifying column.
Further, in step S2, the top of the azeotropic column employs a condenser B and provides cold energy through chilled water.
Still further, in step S2, all of the CL 2 and HF produced are returned to the reactor for further reaction.
Still further, in step S2, a reboiler a is provided in communication with the bottom of the azeotropic column, the reboiler a providing heat to maintain boiling and evaporation of the liquid in the azeotropic column.
Further, in step S1, a reboiler B is provided in communication with the bottom of the HCL rectifying column, and the reboiler B provides heat to maintain boiling and evaporation of the liquid in the HCL rectifying column.
The beneficial effects of the invention are as follows:
1) The flow is simple
The object of the present invention is to provide a process for separating acidic materials and organic materials from the reaction product of CFC-113. In the process, acid separation and recovery in the reaction product of CFC-113 can be simplified into two process units of HCL rectification and azeotropic rectification, compared with the prior art, the process flow is simpler, the number of equipment sets is small, and the occupied area of the device is small, so that the occupied area and project investment can be saved.
2) Low running cost
A) The gas mixture for reacting the crude product is directly sent to the HCL rectifying tower instead of being directly condensed, so that the heat of the crude product of the reaction product can be recovered, the condensing energy consumption is saved, and the running cost is reduced.
B) HF and CL 2 in the reactor gas mixture are separated by azeotropic distillation. The steps of condensation, water washing, alkali washing, drying and the like are omitted, and public engineering and electricity consumption can be saved.
In conclusion, compared with the traditional process, the process can save a great deal of public engineering and electricity consumption, and has low production and operation costs.
3) Less three wastes
The process does not need alkali to absorb HF, HCL and CL 2 in the operation process, so waste acid and waste alkali are not generated; no water enters the system in the process, and a drying unit is not needed, so that no waste molecular sieve solid is generated. Can save the cost of three wastes treatment.
4) High HF utilization rate
By adopting the process, the unreacted HF in the crude reaction product can be completely returned to the reaction kettle to continue the reaction due to no loss caused by absorbing the HF by alkali, and the HF utilization rate is high.
5) CL 2 has high utilization rate
By adopting the process, the unreacted CL 2 in the crude reaction product can be completely returned to the reaction kettle to continue the reaction because no alkali is absorbed by the CL 2 to cause loss, and the CL 2 utilization rate is high.
6) High HCL yield
By adopting the process, all HCL is extracted from the top of the rectifying tower, and the HCL is not sent to a downstream water alkali washing process to generate waste acid and waste alkali, so that the HCL yield is high.
7) The corrosion of the device is small
By adopting the process, water and alkali liquor do not need to be added, waste acid and waste alkali are not generated in the process, and corrosion of production devices can be reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art or ordinary skill.
FIG. 1 is a schematic flow chart of a prior art process.
FIG. 2 is a flow chart of the present invention.
Reference numerals illustrate: the device comprises a primary cooler 1, an intercooler 2, a tail cooler 3, a cryogenic condenser 4, a circulating tower 5, a reboiler 6, a delaminator 7, an acid material receiving tank 8, a pump 9, a deacidification tower 10, a cooler 11, a water washing tower 12, an alkaline washing tower 13, a dryer 14, an HCL rectifying tower 21, a pump A22, a condenser A23, an azeotropic tower 24, a reboiler A25, a condenser B26 and a reboiler B27.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without any inventive effort, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
As shown in FIG. 2, the present invention provides a process for purifying a mixture of CFC-113 to obtain a high purity CFC-113 by separating HF, HCL, CL 2 from a mixture of 1, 2-trichloro-1, 2-trifluoroethane (CFC-113) containing Hydrogen Fluoride (HF), hydrogen Chloride (HCL) and chlorine (CL 2), which comprises the steps of:
Step S1, directly conveying the CFC-113 mixture produced by the reactor to the middle part of an HCL rectifying tower 21, wherein the operating condition of the HCL rectifying tower is 0.5-1.5MPa, the temperature of the top of the rectifying tower is-50 to-15 ℃, and the temperature of the bottom of the rectifying tower is 80-130 ℃. The reflux ratio of the rectifying tower is 1.2-5. Utilizing the heat energy of the CFC-113 mixture to enable HCL gas to be produced from the top of the HCL rectifying tower 21, wherein the top of the HCL rectifying tower 21 adopts a condenser A23 and is condensed by a refrigerant, and the HCL gas with the purity of 99.9% is obtained from the top of the HCL rectifying tower 21; the bottom of the HCL rectifying tower 21 is communicated with a reboiler B27, the reboiler B27 provides heat to maintain boiling and evaporation of liquid in the HCL rectifying tower 21, and materials containing CL2 and HF at the bottom of the HCL rectifying tower 21 are directly sent to an azeotropic tower;
And S2, feeding materials at the bottom of the HCL rectifying tower 21 from the middle part of an azeotropic tower 24 through a pump A22, wherein in the azeotropic tower 24, CL2 and HF in organic matters form an azeotrope and are produced from the top of the azeotropic tower 24, the operation condition of the azeotropic tower is 0.2-1.2MPa, the temperature of the top of the azeotropic tower is-10-40 ℃, and the temperature of the bottom of the azeotropic tower is 80-160 ℃. The reflux ratio of the rectifying tower is 0.5-2.1. The top of the azeotropic tower 24 adopts a condenser B26 and provides cold energy through chilled water, and the produced CL2 and HF are all sent back to the reactor for continuous reaction; the bottom of the azeotropic column 24 is provided with a reboiler A25 in a communicating manner, and the reboiler A25 provides heat to maintain boiling and evaporation of the liquid in the azeotropic column 24, and the bottom of the azeotropic column 24 is provided with a purified CFC-113 product.
The HCL rectifying tower and the azeotropic tower in the steps S1 and S2 can adopt a packed tower or a plate tower, the packing of the packed tower is preferably metal pall rings, and the packing can also be metal structured packing. The material of the packing tower shell is preferably stainless steel, and carbon steel can also be adopted.
Examples:
The reactor output CFC-113 mixture (weight fraction: HCL/32%, CFC-113/55%, CL2/10%, HF/3%) was fed at a feed rate of 1t/h to the middle of HCL rectification column 21. The HCL rectifier operating conditions are preferably: the tower top is 1.2MPa, the operating temperature of the tower top/tower kettle is-25 ℃/115 ℃, the reflux ratio is 2.5, the top of the HCL rectifying tower 21 is condensed by R22 liquid, and the purity of the HCL gas obtained from the top of the HCL rectifying tower 21 is 99.9%; the mixture at the bottom of the HCL rectifying column 21 contains less than 100ppm HCL.
The mixture at the bottom of the HCL rectifying tower 21 is pumped and then is fed into the middle part of the azeotropic tower, the operation condition of the azeotropic tower is controlled to be 0.7Pa at the top of the tower, the operation temperature of the tower top/tower kettle is 10 ℃ per 130 ℃, the reflux ratio is 1.0, the bottom of the azeotropic tower is provided with heat by steam, and the top of the azeotropic tower is provided with cold by chilled water. A mixture of AHF and CL2 was obtained at the top of the azeotropic column, containing 1000ppm of organics, and CFC-113 product was obtained at the bottom of the azeotropic column.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. A process for purifying a CFC-113 mixture, characterized by: the method comprises the following steps:
Step S1, directly sending the CFC-113 mixture produced by the reactor to the middle part of an HCL rectifying tower (21), and directly sending a material containing CL 2 and HF at the bottom of the HCL rectifying tower (21) to an azeotropic tower (24) by utilizing the heat energy of the CFC-113 mixture to enable HCL gas to be produced from the top of the HCL rectifying tower (21);
And S2, feeding materials at the bottom of the HCL rectifying tower (21) from the middle part of an azeotropic tower (24) through a pump A (22), wherein in the azeotropic tower (24), CL 2 and HF in organic matters form an azeotrope to be produced from the top of the azeotropic tower (24), and obtaining a purified CFC-113 product at the bottom of the azeotropic tower (24).
2. The process for purifying CFC-113 mixtures of claim 1, wherein: in step S1, the top of the HCL rectifying column (21) is condensed by a refrigerant using a condenser a (23), and HCL gas having a purity of 99.9% is obtained from the top of the HCL rectifying column (21).
3. The process for purifying CFC-113 mixtures of claim 1, wherein: in step S2, a condenser B (26) is adopted at the top of the azeotropic column (24) and provides cold energy through chilled water.
4. A process for purifying CFC-113 mixtures according to claim 1 or 3, characterized in that: in step S2, all of the CL 2 and HF produced are returned to the reactor for further reaction.
5. A process for purifying CFC-113 mixtures according to claim 1 or 3, characterized in that: in step S2, a reboiler a (25) is disposed in communication with the bottom of the azeotropic column (24), and the reboiler a (25) provides heat to maintain boiling and evaporation of the liquid in the azeotropic column (24).
6. A process for purifying CFC-113 mixtures according to claim 1 or 3, characterized in that: in step S1, a reboiler B (27) is disposed in communication with the bottom of the HCL rectifying column (21), and the reboiler B (27) provides heat to maintain boiling and evaporation of the liquid in the HCL rectifying column (21).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202411170228.5A CN118702541A (en) | 2024-08-26 | 2024-08-26 | Method for purifying CFC-113 mixture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202411170228.5A CN118702541A (en) | 2024-08-26 | 2024-08-26 | Method for purifying CFC-113 mixture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118702541A true CN118702541A (en) | 2024-09-27 |
Family
ID=92811672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202411170228.5A Pending CN118702541A (en) | 2024-08-26 | 2024-08-26 | Method for purifying CFC-113 mixture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118702541A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4944846A (en) * | 1988-08-01 | 1990-07-31 | E. I. Dupont De Nemours And Company | Process for the separation of HF via Azeotropic distillation |
| CN1064859A (en) * | 1991-03-14 | 1992-09-30 | 帝国化学工业公司 | A kind of separation method |
| CN1106373A (en) * | 1993-10-13 | 1995-08-09 | 埃勒夫阿托化学有限公司 | Process for the purification of 1,1,1,2-tetrafluoroethane |
| WO1997007052A1 (en) * | 1995-08-11 | 1997-02-27 | E.I. Du Pont De Nemours And Company | Azeotropes of chlorofluoroethanes with hydrogen fluoride |
| CN104151131A (en) * | 2014-08-08 | 2014-11-19 | 浙江衢化氟化学有限公司 | Preparation method of HFO (hydrofluoroolefin)-1234yf |
| CN104402665A (en) * | 2014-09-30 | 2015-03-11 | 陈岳芹 | Preparation method of trichlorotrifluoroethane |
-
2024
- 2024-08-26 CN CN202411170228.5A patent/CN118702541A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4944846A (en) * | 1988-08-01 | 1990-07-31 | E. I. Dupont De Nemours And Company | Process for the separation of HF via Azeotropic distillation |
| CN1064859A (en) * | 1991-03-14 | 1992-09-30 | 帝国化学工业公司 | A kind of separation method |
| CN1106373A (en) * | 1993-10-13 | 1995-08-09 | 埃勒夫阿托化学有限公司 | Process for the purification of 1,1,1,2-tetrafluoroethane |
| WO1997007052A1 (en) * | 1995-08-11 | 1997-02-27 | E.I. Du Pont De Nemours And Company | Azeotropes of chlorofluoroethanes with hydrogen fluoride |
| CN104151131A (en) * | 2014-08-08 | 2014-11-19 | 浙江衢化氟化学有限公司 | Preparation method of HFO (hydrofluoroolefin)-1234yf |
| CN104402665A (en) * | 2014-09-30 | 2015-03-11 | 陈岳芹 | Preparation method of trichlorotrifluoroethane |
Non-Patent Citations (1)
| Title |
|---|
| 韩国庆: "氟代烷烃的萃取精制", 《浙江化工》, vol. 35, no. 09, 31 December 2004 (2004-12-31), pages 20 - 21 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104311383B (en) | A kind of method of the hydrogen chloride production monochloro methane that utilizes by-product in tetrachloro-ethylene production process | |
| US3635664A (en) | REGENERATION OF HYDROCHLORIC ACID PICKLING WASTE BY H{11 SO{11 {0 ADDITION, DISTILLATION AND FeSO{11 {0 Precipitation | |
| US3983180A (en) | Process for preparing methyl chloride | |
| CN108358176B (en) | Dilute sulfuric acid vacuum concentrating device and method | |
| CN111302899A (en) | Device and method for recovering ammonia and tert-butyl alcohol in cyclohexanone ammoximation production process | |
| CN105481640B (en) | A kind of VCM rectification technique of the low loss of low energy consumption | |
| CN214399818U (en) | Device for purifying hydrogen chloride by calcium chloride method containing impurity dilute hydrochloric acid | |
| CN111606776A (en) | Clean production process for synthesizing methane chloride by liquid-phase catalyst-free synthesis | |
| CN113398719A (en) | Device and method for recovering chlorine in tail chlorine | |
| CN112320758A (en) | Method for purifying trichloroethylene by-product hydrochloric acid | |
| CN106831315A (en) | A kind of continuous production method of chloroethanes | |
| CN101891583A (en) | Method for co-production of trichloroethylene and tetrachloroethylene by gas phase catalysis method | |
| CN210065174U (en) | Concentrated recovery system of dilute sulfuric acid | |
| CN110922292A (en) | Preparation method of chloromethane | |
| CN104803357B (en) | A kind of method that high-purity hydrogen chloride is purified in tetrachloro-ethylene device | |
| CN113955723A (en) | Rectification separation purification method and system for gas containing hydrogen chloride sulfur dioxide | |
| CN103497085A (en) | Processes for bi-coproduction and tri-coproduction of methyl chloride, methane chloride, and tetrachloroethylene | |
| CN111185070B (en) | NF removal using low temperature HF3System and method for removing impurities from electrolysis gas | |
| CN109180417A (en) | A kind of method and system using low-purity chlorine production dichloroethanes EDC | |
| CN219744427U (en) | Device for separating and recovering sulfur dioxide and hydrogen chloride mixed tail gas | |
| CN108083984A (en) | For glyphosate solvent and the method for by-product recovery | |
| CN105480948B (en) | Method and system for recycling byproduct hydrogen chloride in fatty acid or fatty acyl chloride chlorination production process | |
| CN118702541A (en) | Method for purifying CFC-113 mixture | |
| US4554392A (en) | Method of preparing 1,2-dichloroethane from ethylene and chlorine gas | |
| CN111606304A (en) | Dilute hydrochloric acid dechlorination concentration system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |