CN118440738A - Processing method for coking and hydrocracking combined productive chemical raw material - Google Patents
Processing method for coking and hydrocracking combined productive chemical raw material Download PDFInfo
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- CN118440738A CN118440738A CN202310055032.0A CN202310055032A CN118440738A CN 118440738 A CN118440738 A CN 118440738A CN 202310055032 A CN202310055032 A CN 202310055032A CN 118440738 A CN118440738 A CN 118440738A
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- 238000004517 catalytic hydrocracking Methods 0.000 title claims abstract description 135
- 238000004939 coking Methods 0.000 title claims abstract description 51
- 239000013064 chemical raw material Substances 0.000 title claims abstract description 5
- 238000003672 processing method Methods 0.000 title abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 89
- 239000003921 oil Substances 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 45
- 239000002994 raw material Substances 0.000 claims abstract description 39
- 239000007789 gas Substances 0.000 claims abstract description 21
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- 230000003111 delayed effect Effects 0.000 claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 15
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 8
- 239000000295 fuel oil Substances 0.000 claims abstract description 6
- 239000002006 petroleum coke Substances 0.000 claims abstract description 6
- 239000003209 petroleum derivative Substances 0.000 claims abstract description 4
- 238000004227 thermal cracking Methods 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims description 69
- 229910052751 metal Inorganic materials 0.000 claims description 33
- 239000002184 metal Substances 0.000 claims description 33
- 239000002808 molecular sieve Substances 0.000 claims description 27
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 27
- 238000005336 cracking Methods 0.000 claims description 22
- 238000005984 hydrogenation reaction Methods 0.000 claims description 19
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000011593 sulfur Substances 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000010779 crude oil Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 229910052976 metal sulfide Inorganic materials 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 239000003079 shale oil Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 11
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 229930195733 hydrocarbon Natural products 0.000 description 22
- 150000002430 hydrocarbons Chemical class 0.000 description 22
- 239000000047 product Substances 0.000 description 20
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 14
- 239000005977 Ethylene Substances 0.000 description 14
- 238000001035 drying Methods 0.000 description 14
- 238000005470 impregnation Methods 0.000 description 14
- 239000004215 Carbon black (E152) Substances 0.000 description 13
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000012071 phase Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 8
- 238000002407 reforming Methods 0.000 description 7
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 6
- 239000001273 butane Substances 0.000 description 6
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 6
- 239000001294 propane Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000001833 catalytic reforming Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 5
- -1 olefin compounds Chemical class 0.000 description 5
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 238000004523 catalytic cracking Methods 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000007142 ring opening reaction Methods 0.000 description 4
- 239000001993 wax Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 239000003502 gasoline Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000003915 liquefied petroleum gas Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 125000002950 monocyclic group Chemical group 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000004230 steam cracking Methods 0.000 description 2
- 230000000153 supplemental effect Effects 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000012668 chain scission Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010763 heavy fuel oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G69/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one other conversion process
- C10G69/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one other conversion process plural serial stages only
- C10G69/06—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one other conversion process plural serial stages only including at least one step of thermal cracking in the absence of hydrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a processing method of coking and hydrocracking combined productive chemical raw materials. The method comprises the following steps: the coking raw material enters a delayed coking reaction zone to carry out thermal cracking reaction to obtain petroleum coke and gas phase effluent; fractionating the gas phase effluent to obtain coking dry gas and coking full distillate; the initial distillation point of the coking full distillate oil is 50-80 ℃ and the final distillation point is 460-520 ℃; in the presence of hydrogen, coking full distillate enters a first hydrocracking reaction zone to obtain a first hydrocracking product; the mass content of C 7 + normal alkane in the first hydrocracking product is controlled to be 0.1-5.0%; the first hydrocracking product enters a second hydrocracking reaction zone, and the obtained second hydrocracking product is separated and fractionated to obtain gas fractions, light naphtha, heavy naphtha and tail oil. The method uses heavy oil such as vacuum residue oil as raw material, and can improve quality and yield of chemical raw material.
Description
Technical Field
The invention belongs to the field of heavy oil processing, in particular to a processing method combining delayed coking and hydrocracking, and particularly relates to a processing method for producing high-quality chemical raw materials by taking vacuum residuum as a raw material.
Background
Reducing heavy fuel oil production is a developing trend in the oil refining industry in the world today. The capability of single and blending resid in catalytic cracking at present accounts for more than 25% of the total catalytic cracking capability, but not all resid can be processed by catalytic cracking. When the carbon residue content of the residual oil exceeds 10 percent and the metal content exceeds 100-150 ppm, the residual oil hydrotreating/catalytic cracking combined device is difficult to bear higher and higher catalyst cost and longer downtime, and the light oil product demand is increased, the price difference of the light crude oil and the heavy high sulfur crude oil is enlarged, the proportion of the heavy sulfur/high sulfur crude oil supply is enlarged, particularly, the delayed coking can process cheap heavy high sulfur high metal residual oil, the coked gasoline can be used as a raw material for cracking to produce ethylene after hydrogenation, thus the delayed coking becomes the most popular technology for residual oil processing, and a plurality of residual oil processing schemes preferred by refineries are formed.
CN201580070326.4 discloses a process for preparing LPG and BTX comprising: a) Subjecting the mixed hydrocarbon stream to first hydrocracking in the presence of a first hydrocracking catalyst to produce a first hydrocracking product stream; b) Separating the first hydrocracking product stream to provide at least one light hydrocarbon stream comprising at least C2 and C3 hydrocarbons, an intermediate hydrocarbon stream consisting of C4 and/or C5 hydrocarbons, and a heavy hydrocarbon stream comprising at least c6+ hydrocarbons, and C) subjecting the heavy hydrocarbon stream to a second hydrocracking in the presence of a second hydrocracking catalyst to produce a second hydrocracking product stream comprising BTX, wherein the second hydrocracking is more severe than the first hydrocracking, d) wherein at least part of the intermediate hydrocarbon stream is subjected to C4 hydrocracking in the presence of the C4 hydrocracking catalyst to produce a C4 hydrocracking product stream, the C4 hydrocracking being optimized for converting C4 hydrocarbons to C3 hydrocarbons.
CN201480037272.7 discloses a process for producing light olefin compounds from a hydrocarbon feedstock comprising the steps of: (a) feeding a hydrocarbon feedstock to a reaction zone for ring opening; (b) Separating the reaction product produced from the reaction zone into an overhead stream and a side stream; (c) Feeding the side stream from (b) to a Gasoline Hydrocracker (GHC) unit; (d) Separating the reaction product of the GHC of step (c) into a top stream comprising hydrogen, methane, ethane and liquefied petroleum gas and a stream comprising aromatic hydrocarbon compounds and minor amounts of hydrogen and non-aromatic hydrocarbon compounds; (e) The top stream from a Gasoline Hydrocracker (GHC) unit is fed to a steam cracker unit.
In summary, petroleum hydrocarbons are complex in composition and mainly comprise paraffins, naphthenes and aromatics, where paraffins, especially small molecular paraffins, are good ethylene feeds and naphthenes and aromatics are good reforming feeds. The delayed coking causes the heavy raw materials to thermally crack, and follows the free radical reaction mechanism, the normal hydrocarbon and the cyclic hydrocarbon in the product are high in content, and the conversion effect of 'Yikene, yifang' can not be efficiently realized aiming at the coking distillate oil in the prior art. Therefore, the development of a processing method which is suitable for producing high-quality chemical raw materials by using heavy oil such as vacuum residue oil as a raw material through delayed coking and hydrocracking has great significance.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a processing method of coking and hydrocracking combined multi-product chemical raw materials. The method takes heavy oil such as vacuum residue oil as raw material, and can greatly improve the quality and yield of chemical raw materials.
The invention provides a processing method of coking and hydrocracking combined multi-product chemical raw materials, which comprises the following steps:
(1) The coking raw material enters a delayed coking reaction zone to carry out thermal cracking reaction to obtain petroleum coke and gas phase effluent; fractionating the gas phase effluent to obtain coking dry gas and coking full distillate; wherein the initial distillation point of the coking full distillate oil is 50-80 ℃ and the final distillation point is 460-520 ℃;
(2) In the presence of hydrogen, the coked full distillate oil obtained in the step (1) enters a first hydrocracking reaction zone, and n-alkane in a first hydrocracking product is selectively cracked to obtain the first hydrocracking product; wherein, in the first hydrocracking product, the mass content of C 7 + normal alkane is controlled to be 0.1-5.0%;
(3) Feeding the first hydrocracking product into a second hydrocracking reaction zone in the presence of hydrogen to obtain a second hydrocracking product containing monocyclic cyclic hydrocarbons;
(4) And (3) separating and fractionating the second hydrocracking product obtained in the step (3) to obtain a gas fraction, light naphtha, heavy naphtha and tail oil.
According to the present invention, the coking feedstock oil in step (1) is typically a heavy oil having an initial boiling point of greater than 350 ℃ and may be selected from one or more of atmospheric residuum, vacuum residuum, visbreaking residuum, heavy deasphalted oil, catalytically cracked slurry oil, thickened oil, topped crude oil, shale oil and coal liquefaction oil, preferably vacuum residuum. The initial distillation point of the vacuum residuum is 420 ℃ to 620 ℃, preferably 450 ℃ to 550 ℃; the mass content of sulfur is 2-10%, preferably 4-8%; the nitrogen mass content is 0.2-1.0%, preferably 0.3-0.5%; the metal content is 100mg/kg to 500mg/kg, preferably 200mg/kg to 300mg/kg.
According to the invention, the temperature of the delayed coking reaction zone in step (1) is from 480 to 520 ℃, preferably from 490 to 505 ℃; the operation pressure is 0.1 MPa-2 MPa, preferably 0.2 MPa-0.5 MPa, and can be constant-pressure operation or variable-pressure operation; the circulation ratio is 0.1-0.5, preferably 0.2-0.4, and the circulation ratio is the mass ratio of the coked full distillate oil to the raw oil.
According to the invention, the initial distillation point of the coking full distillate in the step (1) is 60-70 ℃ and the final distillation point is 480-500 ℃.
According to the invention, the mass content of aromatic hydrocarbon greater than three rings in the coked full distillate in the step (1) is not higher than 1.0%, preferably 0.2% -0.6%.
According to the present invention, the coker whole distillate may contain impurities such as sulfur, nitrogen, and the like. According to actual needs, a hydrofining catalyst may be disposed upstream of the first hydrocracking catalyst to remove sulfur, nitrogen and other impurities. Wherein the nitrogen content in the reactant stream contacted with the first hydrocracking catalyst is preferably 100mg/kg or less, more preferably 50mg/kg or less.
According to the present invention, preferably, the mass content of C 7 + n-alkane in the step (2) is controlled to be 1.0% to 3.0%.
According to the invention, the chemical raw materials mainly comprise ethane, propane, butane and light naphtha and can also comprise heavy naphtha, wherein the heavy naphtha is used as a reforming raw material to produce BTX, the ethane, propane, butane and light naphtha are used as raw materials for producing low-carbon olefin, such as ethylene by being used as a steam cracking raw material, and the propane and butane can also be directly dehydrogenated to produce propylene and butene. Wherein, the low-carbon olefin refers to olefin with four or less carbon atoms, in particular ethylene, propylene and butadiene.
According to the invention, the first hydrocracking reaction zone in step (2) is charged with a first hydrocracking catalyst, which may be one or more catalysts. In step (2), the first hydrocracking catalyst comprises an active metal component and a support; the support comprises a molecular sieve having a selectively cracked normal alkane, preferably one or more selected from the group consisting of ZSM-5 molecular sieve, ZSM-11, ZSM-12, ZSM-22, ZSM-23, ZSM-35 and ZSM-38 molecular sieves, preferably ZSM-5 molecular sieve. The molar ratio of SiO 2/Al2O3 of the ZSM-5 molecular sieve is 20-60. The carrier may also include a binder. Preferably, the binder is alumina. The active metal component comprises at least one of a group VIB metal, preferably molybdenum and/or tungsten, and a group VIII metal, preferably cobalt and/or nickel.
According to the present invention, in the step (2), preferably, the first hydrocracking catalyst has a content of group VIB metal (in terms of oxide) of 5.0% to 15.0%, a content of group VIII metal (in terms of oxide) of 2.0% to 5.0% and a content of carrier of 80.0% to 93.0% based on the weight of the catalyst.
According to the present invention, in the step (2), preferably, the content of the binder in the carrier of the first hydrocracking catalyst is 8% to 60% and the content of the molecular sieve is 40% to 92% based on the weight of the carrier.
According to the invention, in the step (2), the specific surface area of the first hydrocracking catalyst is 200-400 m 2/g, and the pore volume is 0.25-0.45 cm 3/g. The particle size of the second hydrocracking catalyst is 1.0-3.0 mu m.
According to the present invention, the preparation method of the first hydrocracking catalyst in the step (2) may be prepared according to a conventional method in the art. The preparation method comprises the steps of preparing a carrier and loading active metal components, wherein the preparation process of the carrier is as follows: mechanically mixing the shape selective cracking molecular sieve and the binder, molding, drying and roasting to prepare the catalyst carrier. Conventional conditions may be used for drying and calcining the support. The drying conditions are as follows: drying at 100-150 deg.c for 1-12 hr. The roasting conditions are as follows: roasting at 450-550 deg.c for 2.5-6.0 hr.
According to the present invention, in the preparation method of the first hydrocracking catalyst in the step (2), the method of supporting the active metal component is a conventional method such as a kneading method, an impregnation method or the like, and the impregnation method is preferable. The impregnation method may be a saturated impregnation method, an excessive impregnation method or a complex impregnation method, i.e., impregnating the catalyst support with a solution containing the desired active component, followed by drying and calcination to obtain the second hydrocracking catalyst. The drying conditions are as follows: drying at 100-150 deg.c for 1-12 hr. The roasting conditions are as follows: roasting for 2.5-6.0 hours at 450-550 ℃.
According to the invention, the reaction conditions of the first hydrocracking reaction zone in step (2) are as follows: the reaction pressure is 14 to 17MPa, preferably 15 to 16MPa.
According to the invention, the reaction conditions of the first hydrocracking reaction in step (2) are as follows: the average reaction temperature is 250-450 ℃, preferably 300-400 ℃; the liquid hourly space velocity is 0.1-15.0 h -1, preferably 1.0-5.0 h -1; the hydrogen oil volume ratio is 100:1 to 2500:1, preferably 400:1 to 2000:1.
According to the invention, the ratio of the mass of C 6～C8 monocyclic cyclic hydrocarbons in the second hydrocracking product of step (3) to the mass of total cyclic hydrocarbons in the coked whole distillate feedstock is from 0.20 to 0.40, preferably from 0.30 to 0.36.
According to the present invention, the second hydrocracking catalyst in step (3) has the ring-opening cracking of polycyclic cyclic hydrocarbons, selectively cracking side chains of heterogeneous hydrocarbons or cyclic hydrocarbons and retaining the function of monocyclic cyclic hydrocarbons. The second hydrocracking catalyst includes a cracking component, a hydrogenation component, and a binder. The second hydrocracking catalyst may be commercially available or prepared according to the prior art. The hydrogenation component is at least one of metal, metal oxide and metal sulfide of the active metal component; the active metal component comprises VIB and/or VIII group metals; the active metal component is more preferably at least one of iron, chromium, molybdenum, tungsten, cobalt, and nickel. In the second hydrocracking catalyst, the binder is alumina and/or silica; the cracking component comprises at least one of an acidic molecular sieve, preferably a Beta molecular sieve, a Y molecular sieve.
According to the present invention, preferably, the second hydrocracking reaction zone in step (3) is sequentially filled with a catalyst using a Y molecular sieve as a cracking component and a catalyst using a Beta molecular sieve as a cracking component along the material flow direction; preferably, the volume ratio of the catalyst with the Y molecular sieve as the cracking component to the catalyst with the Beta molecular sieve as the cracking component is 5:1-1:2, preferably 3:1-1:1.
According to the invention, the second hydrocracking catalyst in step (3) has a hydrogenation component content of from 5% to 40% by weight, preferably from 10% to 30% by weight, calculated as oxide, based on the weight of the second hydrocracking catalyst; the content of the cracking component is 10wt percent to 80wt percent, preferably 20wt percent to 60wt percent; the content of the binder is 5wt% to 85wt%, preferably 10wt% to 50wt%.
According to the present invention, the preparation method of the second hydrocracking catalyst in the step (3) may be prepared according to a conventional method in the art. The preparation method comprises the steps of preparing a carrier and loading a hydrogenation component, wherein the preparation process of the carrier is as follows: mechanically mixing the cracking component and the binder, molding, drying and roasting to prepare the catalyst carrier. Conventional conditions may be used for drying and calcining the support. The drying conditions are as follows: drying at 100-150 deg.c for 1-12 hr. The roasting conditions are as follows: roasting at 450-550 deg.c for 2.5-6.0 hr.
According to the present invention, in the preparation method of the second hydrocracking catalyst in the step (3), the method of supporting the hydrogenation component is a conventional method such as a kneading method, an impregnation method or the like, and the impregnation method is preferable. The impregnation method may be a saturated impregnation method, an excessive impregnation method or a complex impregnation method, i.e., impregnating the catalyst support with a solution containing the desired hydrogenation component, followed by drying and calcination to obtain the second hydrocracking catalyst. The drying conditions are as follows: drying at 100-150 deg.c for 1-12 hr. The roasting conditions are as follows: roasting for 2.5-6.0 hours at 450-550 ℃.
According to the invention, the reaction conditions of the second hydrocracking reaction zone in step (3) are as follows: the reaction pressure is 14 to 17MPa, preferably 15 to 16MPa.
According to the invention, the reaction conditions of the second hydrocracking reaction zone in step (3) are as follows: the average reaction temperature is 250-450 ℃, preferably 300-400 ℃; the liquid hourly space velocity is 0.1-15.0 h -1, preferably 1.0-5.0 h -1; the hydrogen oil volume ratio is 100:1 to 2500:1, preferably 400:1 to 2000:1.
According to the present invention, preferably, the first hydrocracking reaction zone and the second hydrocracking reaction zone employ the same pressure.
According to the present invention, the second hydrocracking reaction effluent in step (3) is preferably subjected to supplemental hydrofinishing. The supplemental hydrofining can be carried out by filling hydrofining catalyst at the bottom of the second hydrocracking reaction zone or can be carried out by entering a separate hydrofining reaction zone.
According to the present invention, the second hydrocracking reaction effluent from step (3) may also be fed directly to the fractionation system to make up the heavy naphtha fraction separated.
According to the invention, the tail oil obtained in step (3) is recycled to the second hydrocracking reaction zone.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) In the prior art, when the coking wax oil is used as a raw material for hydrocracking to produce chemical raw materials, the final distillation point of the coking wax oil obtained by separation of a fractionating tower is generally 520-560 ℃, so that the content of aromatic hydrocarbon larger than tricyclic in the wax oil fraction is higher, the hydrocracking of the tricyclic aromatic hydrocarbon can be realized only by higher reaction pressure, and part of monocyclic aromatic hydrocarbon can be cracked by ring opening in the hydrocracking process by higher reaction pressure, thereby causing the loss of aromatic hydrocarbon. In the processing method for joint production of chemical raw materials, the content of aromatic hydrocarbon larger than three rings in coked full-fraction wax oil is controlled to be not higher than 1%, and proper reaction pressure is selected, so that mixed processing of aromatic hydrocarbon with three rings or less is realized, the loss of aromatic hydrocarbon in the hydrogenation process of the raw materials is reduced, and the content of aromatic hydrocarbon in a hydrogenation product is improved. Specifically, the coked full-distillate oil and hydrogen enter a first hydrocracking reaction zone, mainly n-alkanes and long straight-chain cracking containing long straight-chain isoparaffins and naphthenes in the raw materials are selectively cracked to generate small-molecular n-alkanes, the content of C 7 + n-alkanes in the first hydrocracking reaction effluent is 0.1-5.0%, the first hydrocracking reaction effluent enters a second hydrocracking reaction zone, mainly ring-opening cracking of polycyclic cyclic hydrocarbons is carried out, single-ring cyclic hydrocarbons are reserved, and further chain scission is carried out on side chains in each hydrocarbon to generate small-molecular hydrocarbons, so that a large amount of chain alkanes in the raw materials can be converted into gas and light naphtha components, namely enriched in ethylene raw materials, while single-ring cyclic hydrocarbons are reserved in heavy naphtha fractions, namely enriched in reforming raw materials, high-efficiency separation of paraffins and cyclic hydrocarbons can be realized through simple fractionation, and the quality of high-quality ethylene cracking feeding is improved, and the quality of heavy naphtha as catalytic reforming feeding is improved.
Petroleum hydrocarbons have complex compositions and mainly comprise alkane, naphthene and arene, while high-quality ethylene raw materials are small-molecular normal alkane, and reforming raw materials are monocyclic naphthene and arene. The inventor finds that the technical scheme of the invention can keep monocyclic cyclic hydrocarbon as much as possible, and can generate small molecular normal paraffins with high selectivity, thereby realizing high-efficiency enrichment of the small molecular normal paraffins in the low-carbon olefin raw material, and simultaneously keeping monocyclic cyclic hydrocarbon in heavy naphtha as much as possible, thereby realizing high-efficiency enrichment of high-quality reforming raw material, thus being capable of realizing the aim of greatly improving the yield of chemical raw materials (namely ethylene raw material and reforming raw material) and the quality of the ethylene raw material and the reforming raw material, and completing the invention.
(2) The heavy naphtha obtained by the method has high content of monocyclic annular hydrocarbon, is used as a feed for a catalytic reforming device, can cancel paraffin cyclization and dehydrogenation units in the catalytic reforming device, and can greatly reduce investment and energy consumption of the catalytic reforming device; meanwhile, the hydrocracking reaction follows a positive carbon ion reaction mechanism, so that the side chain breaking reaction of the cyclic hydrocarbon with more than C 9 can be realized selectively, the C 6～C8 cyclic hydrocarbon in the product has higher enrichment degree, and the BTX yield can be greatly improved after catalytic reforming and aromatic hydrocarbon extraction.
(3) The invention selectively converts the paraffin in the coked full distillate oil into small molecular paraffin, the process consumes a certain amount of hydrogen, but the light hydrocarbon is used as the raw material of the ethylene device, the hydrogen yield is high, the lower the carbon number is, the higher the hydrogen yield is, so that most of hydrogen consumed in the hydrogenation process can be recovered after the light hydrocarbon passes through the ethylene device, and meanwhile, the yield of ethylene, propylene and butadiene can be greatly improved, the gel cleaning period of the ethylene device is prolonged, and the economic benefit of the device is obviously improved.
Drawings
FIG. 1 is a schematic illustration of the process flow of examples 1-4 of the present invention;
the main reference numerals illustrate:
1-vacuum residuum, 2-delayed coking reaction zone, 3-petroleum coke, 4-delayed coking gas phase effluent, 5-fractionating tower, 6-coking gas fraction, 7-coking full distillate, 8-hydrogen, 9-first hydrocracking reaction zone, 10-first hydrocracking reaction effluent, 11-second hydrocracking reaction zone, 12-second hydrocracking reaction effluent, 13-separator, 14-gas phase stream hydrogen-rich gas, 15-liquid phase stream, 16-fractionating tower, 17-gas fraction, 18-light naphtha, 19-heavy naphtha, 20-tail oil.
Detailed Description
The operation and effect of the present invention will be further illustrated by the following examples, which are not to be construed as limiting the process of the present invention.
In the invention, the mass fraction is the percentage unless otherwise specified.
The total volume space velocity in both the examples and comparative examples is the ratio of fresh feed volume to total catalyst volume.
The method of the invention, as shown in FIG. 1, comprises the following steps: the vacuum residuum 1 enters a delayed coking reaction zone 2 to obtain petroleum coke 3 and delayed coking gas-phase effluent 4, the delayed coking gas-phase effluent 4 enters a fractionating tower 5 to be separated to obtain coking gas fraction 6 and coking full-fraction oil 7, the coking full-fraction oil 7 is mixed with hydrogen 8 and enters a first hydrocracking reaction zone 9 to carry out first hydrocracking reaction, the first hydrocracking reaction effluent 10 enters a second hydrocracking reaction zone 11 to carry out second hydrocracking reaction, the second hydrocracking reaction effluent 12 enters a separator 13, the separated gas-phase material flow hydrogen-rich gas 14 is recycled, a liquid-phase material flow 15 enters the fractionating tower 16 to be fractionated to obtain gas fraction 17, light naphtha 18, heavy naphtha 19 and tail oil 20, and the tail oil 20 is recycled to the second hydrocracking reaction zone 11.
In the present invention, the first hydrocracking catalyst in each case is denoted by Cat-A plus a number, such as Cat-A1, cat-A2, cat-A3. The first hydrocracking catalyst was prepared by conventional active metal saturation impregnation, and the physicochemical properties of the obtained catalyst are shown in table 1.
In the present invention, the second hydrocracking catalyst in each case is represented by Cat-B plus a number, such as Cat-B1, cat-B2. The physical and chemical properties of the catalyst are shown in Table 2. The second hydrocracking catalyst in each case was prepared using a conventional active metal saturation impregnation process in which the Beta molecular sieve used in Cat-B2 had the following properties: siO 2/Al2O3 molar ratio is 30, specific surface area is 350m 2/g, pore volume is 0.32cm 3/g, and the properties of the Y molecular sieve used in Cat-B1 are as follows: siO 2/Al2O3 in a molar ratio of 15, a specific surface area of 400m 2/g and a pore volume of 0.30cm 3/g.
In the present invention, the raw oil in each example was vacuum residue, and the main properties thereof are shown in Table 3.
In the present invention, the nitrogen content of the reactant stream contacted with the first hydrocracking catalyst in each case is 50mg/kg or less
In the present invention, the ethylene raw material in each case refers to ethane, propane, butane and light naphtha obtained in the step (3), and the ethane, propane, butane and light naphtha can be directly used as raw materials for preparing ethylene by steam cracking.
In the invention, the light naphtha is a liquid component with the distillation range of less than 60 ℃, the heavy naphtha is a component with the distillation range of 60-175 ℃ and the tail oil is a component with the distillation range of >175 ℃.
In the present invention, the yield of ethylene feedstock refers to the mass ratio of ethane, propane, butane and light naphtha in the hydrocracked product to the hydrocracked fresh feedstock (coked full distillate), and the yield of heavy naphtha refers to the mass ratio of heavy naphtha in the hydrocracked product to the hydrocracked fresh feedstock (coked full distillate).
Examples 1 to 4
The processing method of the coking and hydrocracking combined productive chemical raw material adopts the flow as shown in figure 1, and comprises the following steps:
(1) The vacuum residuum enters a delayed coking reaction zone to carry out thermal cracking reaction to obtain petroleum coke and gas phase effluent; the gaseous effluent enters a fractionating tower to obtain coking dry gas and coking full distillate;
(2) The coked full distillate oil and hydrogen are mixed and sequentially enter a first hydrocracking reaction zone and a second hydrocracking reaction zone; the first hydrocracking reaction zone is filled with a first hydrocracking catalyst; the second hydrocracking reaction zone is filled with a second hydrocracking catalyst; controlling the content of C 7 + normal paraffins in the first hydrocracking reaction effluent of the step (2) and the content of polycyclic paraffins in the second hydrocracking product.
(3) The reaction effluent of the second hydrocracking reaction zone is subjected to gas-liquid separation to obtain a gas-phase material flow and a liquid-phase material flow; the gas phase material flow is recycled, and the liquid phase material flow enters a fractionating tower to be fractionated to obtain gas fractions, light naphtha, heavy naphtha and tail oil.
The process conditions and hydrogenation effects in each case are shown in Table 5.
Comparative example 1
The difference from example 1 is that: the coked full distillate oil directly enters a second hydrocracking reaction zone after being hydrofined.
The process conditions and hydrogenation effects in this example are shown in Table 5.
Comparative example 2
The difference from example 1 is that: in the step (2), the mass content of C 7 + normal alkane in the second hydrocracking reaction effluent is controlled to be 6 percent.
The process conditions and hydrogenation effects in this example are shown in Table 5.
Comparative example 3
The difference from example 1 is that: the second hydrocracking reaction zone was packed with catalysts in a different order than example 1, which exchanged the order of catalysts Cat-B1 and Cat-B2. Specifically, the hydrocracking reaction zone of this example is filled with catalyst Cat-B2 and catalyst Cat-B1 in sequence along the material flow direction.
The process conditions and hydrogenation effects in this example are shown in Table 5.
Comparative example 4
The difference from example 1 is that: the mass content of the aromatic hydrocarbon with more than three rings in the coking full distillate oil is 3.5 percent.
The process conditions and hydrogenation effects in this example are shown in Table 5.
TABLE 1 physicochemical Properties of the first hydrocracking catalyst
| Catalyst | Cat-A1 | Cat-A2 | Cat-A3 |
| Pore volume, cm 3/g | 0.35 | 0.45 | 0.25 |
| Specific surface area, m 2/g | 300 | 200 | 400 |
| Content by weight percent based on the weight of the carrier | |||
| ZSM-5 | 58 | 42 | 85 |
| Alumina oxide | 42 | 58 | 15 |
| Active metal content in the catalyst, wt% | |||
| MoO3 | 10.0 | 15.0 | 5.0 |
| NiO | 3.5 | 2.0 | 5.0 |
| Carrier content in catalyst, wt% | 86.5 | 83.0 | 90.0 |
| SiO 2/Al2O3 molar ratio of ZSM-5 | 40 | 60 | 20 |
TABLE 2 physicochemical Properties of the second hydrocracking catalyst
TABLE 3 Main Properties of raw oil
| Raw oil name | Vacuum residuum |
| Density (20 ℃ C.)/kg.m -3 | 1.032 |
| Distillation range/. Degree.C | |
| IBP/10％ | 464/558 |
| 30％/50％ | 606/646 |
| 70％/90％ | 749/973 |
| 95％/EBP | 1025/1055 |
| Sulfur content, wt% | 5.61 |
| Nitrogen content, wt% | 0.38 |
| Ni+V，mg/kg | 200 |
TABLE 4 delayed coking Process conditions and coking full distillate Main Properties
Continuous table 4
TABLE 5 hydrogenation effect
Continuous table 4
The above describes in detail the specific embodiments of the present invention, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (13)
1. A method for processing a coking and hydrocracking combined multi-product chemical raw material, which is characterized by comprising the following steps:
(1) The coking raw material enters a delayed coking reaction zone to carry out thermal cracking reaction to obtain petroleum coke and gas phase effluent; fractionating the gas phase effluent to obtain coking dry gas and coking full distillate; wherein the initial distillation point of the coking full distillate oil is 50-80 ℃ and the final distillation point is 460-520 ℃;
(2) In the presence of hydrogen, the coked full distillate oil obtained in the step (1) enters a first hydrocracking reaction zone, and n-alkane in a first hydrocracking product is selectively cracked to obtain the first hydrocracking product; wherein, in the first hydrocracking product, the mass content of C 7 + normal alkane is controlled to be 0.1-5.0%;
(3) Feeding the first hydrocracking product into a second hydrocracking reaction zone in the presence of hydrogen to obtain a second hydrocracking product containing monocyclic cyclic hydrocarbons;
(4) And (3) separating and fractionating the second hydrocracking product obtained in the step (3) to obtain a gas fraction, light naphtha, heavy naphtha and tail oil.
2. The method according to claim 1, wherein the coker feedstock of step (1) is a heavy oil having an initial boiling point of greater than 350 ℃, and is selected from one or more of atmospheric residuum, vacuum residuum, visbroken residuum, heavy deasphalted oil, catalytically cracked slurry oil, thickened oil, topped crude oil, shale oil, and coal liquefaction oil, preferably vacuum residuum; further preferably, the initial distillation point of the vacuum residuum is 420 ℃ to 620 ℃, preferably 450 ℃ to 550 ℃; the mass content of sulfur is 2-10%, preferably 4-8%; the nitrogen mass content is 0.2-1.0%, preferably 0.3-0.5%; the metal content is 100mg/kg to 500mg/kg, preferably 200mg/kg to 300mg/kg.
3. The process of claim 1 wherein the coker whole distillate in step (1) has an initial boiling point of from 60 ℃ to 70 ℃ and a final boiling point of from 480 ℃ to 500 ℃;
and/or the mass content of aromatic hydrocarbon larger than tricyclic in the coked full distillate is not higher than 1.0%, preferably 0.2% -0.6%.
4. The process according to claim 1, wherein the temperature of the delayed coking reaction zone in step (1) is from 480 to 520 ℃, preferably from 490 to 505 ℃; the operating pressure is 0.1MPa to 2MPa, preferably 0.2MPa to 0.5MPa; the circulation ratio is 0.1 to 0.5, preferably 0.2 to 0.4.
5. The process of claim 1 wherein in step (2) the first hydrocracking reaction zone is charged with a first hydrocracking catalyst; the first hydrocracking catalyst comprises an active metal component and a carrier;
And/or the carrier comprises a molecular sieve having selectively cracked normal paraffins, preferably one or more selected from the group consisting of ZSM-5 molecular sieve, ZSM-11, ZSM-12, ZSM-22, ZSM-23, ZSM-35 and ZSM-38 molecular sieves, further preferably ZSM-5 molecular sieve;
and/or the active metal component comprises at least one of a group VIB metal and a group VIII metal, the group VIB metal preferably being molybdenum and/or tungsten, the group VIII metal preferably being cobalt and/or nickel;
And/or, the first hydrocracking catalyst comprises 5.0-15.0% of VIB group metal calculated by oxide, 2.0-5.0% of VIII group metal calculated by oxide and 80.0-93.0% of carrier based on the weight of the catalyst.
6. The process according to claim 1, wherein in step (2) the reaction pressure in the first hydrocracking reaction zone is from 14 to 17MPa, preferably from 15 to 16MPa.
7. The process of claim 1 or 5 wherein the reaction conditions in the first hydrocracking reaction zone in step (2) are as follows: the average reaction temperature is 250-450 ℃, preferably 300-400 ℃; the liquid hourly space velocity is 0.1-15.0 h -1, preferably 1.0-5.0 h -1; the hydrogen oil volume ratio is 100:1 to 2500:1, preferably 400:1 to 2000:1.
8. The method according to claim 1, wherein the mass content of the C 7 + n-alkane in the step (2) is controlled to be 1.0-3.0%.
9. The process of claim 1 wherein in step (3) the second hydrocracking reaction zone is charged with a second hydrocracking catalyst; the second hydrocracking catalyst comprises a cracking component, a hydrogenation component and a binder;
Preferably, the content of the hydrogenation component in terms of oxide is from 5wt% to 40wt%, preferably from 10wt% to 30wt%, based on the weight of the second hydrocracking catalyst; the content of the cracking component is 10wt percent to 80wt percent, preferably 20wt percent to 60wt percent; the content of the adhesive is 5 to 85 weight percent, preferably 10 to 50 weight percent;
And/or, in the second hydrocracking catalyst, the hydrogenation component is at least one of metal, metal oxide and metal sulfide of the active metal component; the active metal component comprises VIB and/or VIII group metals; the active metal component is more preferably at least one of iron, chromium, molybdenum, tungsten, cobalt and nickel;
and/or, in the second hydrocracking catalyst, the binder is alumina and/or silica;
And/or, in the second hydrocracking catalyst, the cracking component comprises at least one of an acidic molecular sieve, preferably a Beta molecular sieve and a Y molecular sieve;
And/or, sequentially filling a catalyst taking a Y molecular sieve as a cracking component and a catalyst taking a Beta molecular sieve as a cracking component in the second hydrocracking reaction zone in the step (3) along the material flow direction; preferably, the volume ratio of the catalyst with the Y molecular sieve as the cracking component to the catalyst with the Beta molecular sieve as the cracking component is 5:1-1:2, preferably 3:1-1:1.
10. The process according to claim 1, wherein the reaction pressure in the second hydrocracking reaction zone in step (3) is from 14 to 17MPa, preferably from 15 to 16MPa.
11. The process according to claim 1 or 9, wherein the reaction conditions of the second hydrocracking reaction zone in step (3) are as follows: the average reaction temperature is 250-450 ℃, preferably 300-400 ℃; the liquid hourly space velocity is 0.1-15.0 h -1, preferably 1.0-5.0 h -1; the hydrogen oil volume ratio is 100:1 to 2500:1, preferably 400:1 to 2000:1.
12. The process according to claim 1, characterized in that in the second hydrocracking product of step (3) the mass ratio of C 6～C8 monocyclic cyclic hydrocarbons to the total cyclic hydrocarbons in the coker whole distillate feedstock is from 0.20 to 0.40, preferably from 0.30 to 0.36.
13. The process of claim 1 wherein the first hydrocracking reaction zone and the second hydrocracking reaction zone employ the same pressure.
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