CN116903431B - Method for preparing propylene by purifying coked liquefied gas - Google Patents
Method for preparing propylene by purifying coked liquefied gas Download PDFInfo
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- CN116903431B CN116903431B CN202311146058.2A CN202311146058A CN116903431B CN 116903431 B CN116903431 B CN 116903431B CN 202311146058 A CN202311146058 A CN 202311146058A CN 116903431 B CN116903431 B CN 116903431B
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- Prior art keywords
- liquefied gas
- desulfurization
- ball milling
- propylene
- coked
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 97
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 73
- 230000023556 desulfurization Effects 0.000 claims abstract description 73
- 238000004939 coking Methods 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- 238000010521 absorption reaction Methods 0.000 claims abstract description 25
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 19
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 17
- -1 alcohol amine Chemical class 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940043276 diisopropanolamine Drugs 0.000 claims abstract description 11
- 239000001509 sodium citrate Substances 0.000 claims abstract description 11
- 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 claims abstract description 11
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 11
- 239000003549 soybean oil Substances 0.000 claims abstract description 11
- 239000004698 Polyethylene Substances 0.000 claims abstract description 10
- 229920000573 polyethylene Polymers 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 230000018044 dehydration Effects 0.000 claims abstract 3
- 238000006297 dehydration reaction Methods 0.000 claims abstract 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 61
- 238000000498 ball milling Methods 0.000 claims description 53
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 25
- 230000003009 desulfurizing effect Effects 0.000 claims description 25
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 10
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- 229920002674 hyaluronan Polymers 0.000 claims description 10
- 229960003160 hyaluronic acid Drugs 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000012188 paraffin wax Substances 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 235000010413 sodium alginate Nutrition 0.000 claims description 10
- 239000000661 sodium alginate Substances 0.000 claims description 10
- 229940005550 sodium alginate Drugs 0.000 claims description 10
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 10
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 10
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000001993 wax Substances 0.000 claims description 9
- 235000010489 acacia gum Nutrition 0.000 claims description 8
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 6
- 239000001273 butane Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- 239000001294 propane Substances 0.000 claims description 6
- 229920000084 Gum arabic Polymers 0.000 claims description 5
- 239000000205 acacia gum Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 241000220479 Acacia Species 0.000 claims description 2
- 235000010643 Leucaena leucocephala Nutrition 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 abstract description 13
- 239000011593 sulfur Substances 0.000 abstract description 13
- 238000000746 purification Methods 0.000 abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 150000001348 alkyl chlorides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/75—Multi-step processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/11—Purification; Separation; Use of additives by absorption, i.e. purification or separation of gaseous hydrocarbons with the aid of liquids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/163—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound by hydrogenation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention provides a method for preparing propylene by purifying coked liquefied gas, belonging to the field of coked liquefied gas purification; the method for preparing propylene by purifying the coked liquefied gas comprises the steps of primary desulfurization, secondary desulfurization, complete desulfurization, rectification and dehydration; the secondary desulfurization step is that the coking liquefied gas after primary desulfurization is put into an alcohol amine absorption tower, and the absorption liquid is utilized to remove hydrogen sulfide; the absorption liquid comprises deionized water, diisopropanolamine, polyethylene wax, sodium hydroxide and an auxiliary agent; the preparation method of the auxiliary agent comprises the steps of mixing sodium citrate, epoxidized soybean oil and aluminum oxide, performing heat treatment at 66-70 ℃ for 23-27min, and cooling to obtain the auxiliary agent. The purity of propylene prepared by the purification method is 99.96-99.99%, the yield is 96.3-96.8%, and the content of hydrogen sulfide is 0.01-0.04 mug/m 3 The total sulfur content is 0.25-0.32 mug/m 3 。
Description
Technical Field
The invention belongs to the field of coking liquefied gas purification, and particularly relates to a method for preparing propylene by purifying coking liquefied gas.
Background
Propylene is used as one of petrochemical basic raw materials, and can be used for producing a plurality of important organic chemical raw materials, such as acrylonitrile, glycerol, acetone, epoxy chloroalkane, glycerol, polypropylene and the like; the method is a raw material for preparing the laminated gasoline in the oil refining industry, can also be used for producing synthetic resin, synthetic fiber, synthetic rubber and the like, and is widely applied to the fields of environmental protection, medical science, basic research and the like.
In recent years, the contradiction between petroleum supply and demand in the world is increasingly activated, the quality of crude oil processed in China is increasingly heavier and inferior, and coking is an important method for processing inferior oil, so that the coking is quite commonly applied to refineries in more cities;
the propylene content in the coked liquefied gas produced after coking is about 18%, and if the coked liquefied gas can be purified, the propylene in the coked liquefied gas can be recycled, so that the application value of the coked liquefied gas can be greatly improved.
However, the sulfur content in the coked liquefied gas is about 10 times that of the liquefied gas discharged from a conventional catalytic cracking device, the prior art is not thorough in sulfur removal, and the total sulfur content is still higher, so that the purity and the yield of propylene are affected; moreover, the waste gas and waste residue generated by the desulfurization device are difficult to treat, and pollute the environment;
therefore, the method for preparing propylene by purifying the coking liquefied gas is provided, the purity and the yield of the propylene are improved, and the pollution to the environment is reduced, so that the technical problem to be solved in the prior art is urgent.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a method for preparing propylene by purifying coked liquefied gas, which improves the purity and yield of propylene and reduces the pollution to the environment.
In order to solve the technical problems, the invention adopts the following technical scheme:
1. preliminary desulfurization
Reacting the coking liquefied gas with hydrogen at the lower part of a reactor, wherein the pressure in the reactor is 0.9-1.2 MPa, the reaction temperature is 255-265 ℃, a desulfurizing agent enters from the upper part of the reactor for preliminary desulfurization treatment, the treatment temperature is 105-115 ℃, and after the treatment, the coking liquefied gas after the preliminary desulfurization treatment is discharged from the top of the reactor to obtain the coking liquefied gas after the preliminary desulfurization;
the mass ratio of the coking liquefied gas to the hydrogen is 1:48-52;
the mass ratio of the coking liquefied gas to the desulfurizing agent is 3:15-17;
the preparation method of the desulfurizing agent comprises the steps of modifying montmorillonite and mixing;
the modified montmorillonite is calcined for 3.1-3.3 hours at 310-330 ℃, and after the calcination is completed, the natural temperature is restored to room temperature, sulfuric acid solution is added, and stirring is carried out for 1.2-1.8 hours at 65-75 ℃, and the preliminary modified montmorillonite is obtained after centrifugation, filtration and drying;
the grain diameter of the montmorillonite is 90-110nm;
the mass concentration of the sulfuric acid solution is 38-42%;
the mass ratio of the montmorillonite to the sulfuric acid solution is 1:3-5;
placing the preliminary modified montmorillonite into a closed container for closed treatment, wherein the pressure in the closed container is 0.15-0.25MPa, the temperature is 160-180 ℃, the treatment time is 25-35min, the temperature is reduced to room temperature at the speed of 0.4-0.6 ℃/min after the closed treatment is finished, then deionized water, sodium dodecyl benzene sulfonate, hyaluronic acid and sodium alginate are added, the preliminary modified montmorillonite is placed into a ball mill for primary ball milling treatment, the ball material ratio is controlled to be 8-12:1, the ball milling rotating speed is 240-260rpm, the ball milling time is 30-50min, the ball milling temperature is 2-4 ℃, aluminum oxide, acacia and polyethylene glycol are added after the primary ball milling is finished, the secondary ball milling treatment is performed, the ball milling rotating speed is controlled to be 10-14:1, the ball milling rotating speed is 200-220rpm, the ball milling time is 22-28min, the ball milling temperature is 1.7-2.4 ℃, and the final modified montmorillonite is obtained after the ball milling is finished;
the mass ratio of the preliminary modified montmorillonite to the deionized water to the sodium dodecyl benzene sulfonate to the hyaluronic acid to the sodium alginate to the aluminum oxide to the acacia gum to the polyethylene glycol is 26-32:110-130:3-5:1-3:2-4:18.3-22.8:3.7-8.1:7.3-9.8;
mixing the modified montmorillonite, zinc oxide and deionized water, uniformly stirring, adding sodium pyrophosphate and paraffin, uniformly stirring, and drying to obtain a desulfurizing agent;
the mass ratio of the deionized water to the modified montmorillonite to the zinc oxide to the sodium pyrophosphate to the paraffin is 85-93:8-11:12-16:2-4:3-5.
2. Secondary desulfurization
Putting the coking liquefied gas subjected to primary desulfurization into an alcohol amine absorption tower, and removing hydrogen sulfide by utilizing an absorption liquid to obtain coking liquefied gas subjected to secondary desulfurization;
the mass ratio of the coking liquefied gas after preliminary desulfurization to the absorption liquid is 1:3.6-3.9;
the absorption liquid comprises deionized water, diisopropanolamine, polyethylene wax, sodium hydroxide and an auxiliary agent;
the mass ratio of the deionized water to the diisopropanolamine to the polyethylene wax to the sodium hydroxide to the auxiliary agent is 65-75:88-92:8-11:6-8:8-10;
the preparation method of the auxiliary agent comprises the steps of mixing sodium citrate, epoxidized soybean oil and aluminum oxide, performing heat treatment at 66-70 ℃ for 23-27min, and cooling to obtain the auxiliary agent;
the mass ratio of the sodium citrate to the epoxidized soybean oil to the alumina is 2-4:3-5:18-22.
3. Complete desulfurization
Putting the coked liquefied gas subjected to secondary desulfurization into an air tower, wherein the pressure of the air tower is 1.1-1.3MPa, the temperature is 450-470 ℃, and the coked liquefied gas subjected to complete desulfurization is obtained after reaction for 18-25 min;
the mass ratio of the coking liquefied gas after the secondary desulfurization to the air is 1:33-37.
4. Rectifying
And (3) rectifying the completely desulfurized coking liquefied gas sequentially through a depropanizer, a deethanizer and a propylene tower, and separating ethane, propane and butane to obtain crude propylene.
5. Dewatering
The crude propylene is dehydrated until the water content in the crude propylene is as low as less than 6ppm, and the propylene is obtained after drying.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention purifies the coking liquefied gas, firstly, mercaptans, carbonyl sulfide and the like in the coking liquefied gas are converted into hydrogen sulfide, and then, a desulfurizing agent is adopted to remove the hydrogen sulfide in the coking liquefied gas and hydrogen sulfide generated by hydrodesulfurization;
the desulfurizing agent is prepared by adopting a specific method, so that the contact area of the desulfurizing agent and the coking liquefied gas is increased, the reaction rate is accelerated, the removal effect is enhanced, and the desulfurizing agent is combined with specific absorption liquid components, so that the total sulfur content in propylene is reduced, and the purity and the yield of propylene are improved;
2. the propylene obtained by purifying the coking liquefied gas by adopting the method has the purity of 99.96-99.99 percent, the yield of 96.3-96.8 percent and the content of hydrogen sulfide of 0.01-0.04 mu g/m 3 The total sulfur content is 0.25-0.32 mug/m 3 。
Detailed Description
For a clearer understanding of the technical features, objects and effects of the present invention, specific embodiments of the present invention will be described.
The raw material components of the coking liquefied gas comprise 16.42wt% of propylene, 36.1wt% of propane, 22.6wt% of butane and 0.41wt% of ethane; mercaptan sulfur content of 3620mg/m 3 Total sulfur content of 5940 mg/m 3 。
Example 1 Process for preparing propylene by purifying coked liquefied gas
1. Preliminary desulfurization
The coking liquefied gas and hydrogen are reacted at the lower part of a reactor, the pressure in the reactor is 1.0MPa, the reaction temperature is 260 ℃, a desulfurizing agent enters from the upper part of the reactor for preliminary desulfurization treatment, the treatment temperature is 110 ℃, and after the completion of the preliminary desulfurization treatment, the coking liquefied gas after the preliminary desulfurization treatment is discharged from the top of the reactor to obtain the coking liquefied gas after the preliminary desulfurization;
the mass ratio of the coking liquefied gas to the hydrogen is 1:50;
the mass ratio of the coking liquefied gas to the desulfurizing agent is 3:16;
the preparation method of the desulfurizing agent comprises the steps of modifying montmorillonite and mixing;
the modified montmorillonite is calcined at 320 ℃ for 3.2 hours, the calcined montmorillonite is naturally restored to room temperature, sulfuric acid solution is added, stirring is carried out for 1.5 hours at 70 ℃, and preliminary modified montmorillonite is obtained after centrifugation, filtration and drying;
the grain diameter of the montmorillonite is 100nm;
the mass concentration of the sulfuric acid solution is 40%;
the mass ratio of the montmorillonite to the sulfuric acid solution is 1:4;
placing the preliminary modified montmorillonite into a closed container for closed treatment, wherein the pressure in the closed container is 0.2MPa, the temperature is 170 ℃, the treatment time is 30min, the temperature is reduced to room temperature at the speed of 0.5 ℃/min after the closed treatment is finished, then deionized water, sodium dodecyl benzene sulfonate, hyaluronic acid and sodium alginate are added, the preliminary modified montmorillonite is placed into a ball mill for primary ball milling treatment, the ball material ratio is controlled to be 10:1, the ball milling rotation speed is 250rpm, the ball milling time is 40min, the ball milling temperature is 3 ℃, aluminum oxide, arabic gum and polyethylene glycol are added after the primary ball milling is finished, the secondary ball milling treatment is performed, the ball material ratio is controlled to be 12:1, the ball milling rotation speed is 210rpm, the ball milling time is 25min, the ball milling temperature is 2.1 ℃, and the modified montmorillonite is prepared after the ball milling is finished;
the mass ratio of the preliminary modified montmorillonite to deionized water to sodium dodecyl benzene sulfonate to hyaluronic acid to sodium alginate to alumina to acacia gum to polyethylene glycol is 30:120:4:2:3:20.6:5.1:8.6;
mixing the modified montmorillonite, zinc oxide and deionized water, uniformly stirring, adding sodium pyrophosphate and paraffin, uniformly stirring, and drying to obtain a desulfurizing agent;
the mass ratio of the deionized water to the modified montmorillonite to the zinc oxide to the sodium pyrophosphate to the paraffin is 90:10:15:3:4.
2. Secondary desulfurization
Putting the coking liquefied gas subjected to primary desulfurization into an alcohol amine absorption tower, and removing hydrogen sulfide by utilizing an absorption liquid to obtain coking liquefied gas subjected to secondary desulfurization;
the mass ratio of the coking liquefied gas after preliminary desulfurization to the absorption liquid is 1:3.7;
the absorption liquid comprises deionized water, diisopropanolamine, polyethylene wax, sodium hydroxide and an auxiliary agent;
the mass ratio of the deionized water to the diisopropanolamine to the polyethylene wax to the sodium hydroxide to the auxiliary agent is 70:90:10:7:9;
the preparation method of the auxiliary agent comprises the steps of mixing sodium citrate, epoxidized soybean oil and aluminum oxide, performing heat treatment at 68 ℃ for 25min, and cooling to obtain the auxiliary agent;
the mass ratio of the sodium citrate to the epoxidized soybean oil to the alumina is 3:4:20.
3. Complete desulfurization
Putting the coked liquefied gas subjected to secondary desulfurization into an air tower, wherein the pressure of the air tower is 1.2MPa, the temperature is 460 ℃, and the coked liquefied gas is reacted for 20 minutes to obtain the coked liquefied gas subjected to complete desulfurization;
the mass ratio of the coking liquefied gas after the secondary desulfurization to the air is 1:35.
4. rectifying
And (3) rectifying the completely desulfurized coking liquefied gas sequentially through a depropanizer, a deethanizer and a propylene tower, and separating ethane, propane and butane to obtain crude propylene.
5. Dewatering
The crude propylene is dehydrated until the water content in the crude propylene is as low as less than 6ppm, and the propylene is obtained after drying.
Propylene obtained by purifying the coked liquefied gas by the method of example 1 has the purity of 99.99%, the yield of 96.8% and the hydrogen sulfide content of 0.01 mug/m 3 Total sulfur content of 0.25. Mu.g/m 3 。
Example 2 Process for preparing propylene by purifying coked liquefied gas
1. Preliminary desulfurization
The coking liquefied gas and hydrogen are reacted at the lower part of a reactor, the pressure in the reactor is 1.2MPa, the reaction temperature is 265 ℃, a desulfurizing agent enters from the upper part of the reactor for preliminary desulfurization treatment, the treatment temperature is 115 ℃, and after the treatment is finished, the coking liquefied gas after the preliminary desulfurization treatment is discharged from the top of the reactor to obtain the coking liquefied gas after the preliminary desulfurization;
the mass ratio of the coking liquefied gas to the hydrogen is 1:52;
the mass ratio of the coking liquefied gas to the desulfurizing agent is 3:17;
the preparation method of the desulfurizing agent comprises the steps of modifying montmorillonite and mixing;
the modified montmorillonite is calcined at 330 ℃ for 3.1 hours, the calcined montmorillonite is naturally restored to room temperature, sulfuric acid solution is added, stirring is carried out for 1.2 hours at 75 ℃, and the preliminary modified montmorillonite is obtained after centrifugation, filtration and drying;
the grain diameter of the montmorillonite is 110nm;
the mass concentration of the sulfuric acid solution is 42%;
the mass ratio of the montmorillonite to the sulfuric acid solution is 1:5;
placing the preliminary modified montmorillonite into a closed container for closed treatment, wherein the pressure in the closed container is 0.25MPa, the temperature is 180 ℃, the treatment time is 25min, the temperature is reduced to room temperature at the speed of 0.6 ℃/min after the closed treatment is finished, then deionized water, sodium dodecyl benzene sulfonate, hyaluronic acid and sodium alginate are added, the preliminary modified montmorillonite is placed into a ball mill for primary ball milling treatment, the ball material ratio is controlled to be 12:1, the ball milling rotation speed is 260rpm, the ball milling time is 30min, the ball milling temperature is 4 ℃, aluminum oxide, arabic gum and polyethylene glycol are added after the primary ball milling is finished, the secondary ball milling treatment is carried out, the ball material ratio is controlled to be 10:1, the ball milling rotation speed is 220rpm, the ball milling time is 28min, the ball milling temperature is 2.4 ℃, and the modified montmorillonite is obtained after the ball milling is finished;
the mass ratio of the preliminary modified montmorillonite to deionized water to sodium dodecyl benzene sulfonate to hyaluronic acid to sodium alginate to alumina to acacia gum to polyethylene glycol is 32:130:5:3:4:22.8:8.1:9.8;
mixing the modified montmorillonite, zinc oxide and deionized water, uniformly stirring, adding sodium pyrophosphate and paraffin, uniformly stirring, and drying to obtain a desulfurizing agent;
the mass ratio of the deionized water to the modified montmorillonite to the zinc oxide to the sodium pyrophosphate to the paraffin is 85:8:12:2:3.
2. Secondary desulfurization
Putting the coking liquefied gas subjected to primary desulfurization into an alcohol amine absorption tower, and removing hydrogen sulfide by utilizing an absorption liquid to obtain coking liquefied gas subjected to secondary desulfurization;
the mass ratio of the coking liquefied gas after preliminary desulfurization to the absorption liquid is 1:3.6;
the absorption liquid comprises deionized water, diisopropanolamine, polyethylene wax, sodium hydroxide and an auxiliary agent;
the mass ratio of the deionized water to the diisopropanolamine to the polyethylene wax to the sodium hydroxide to the auxiliary agent is 75:92:11:8:10;
the preparation method of the auxiliary agent comprises the steps of mixing sodium citrate, epoxidized soybean oil and aluminum oxide, performing heat treatment at 70 ℃ for 27min, and cooling to obtain the auxiliary agent;
the mass ratio of the sodium citrate to the epoxidized soybean oil to the alumina is 4:5:22.
3. Complete desulfurization
Putting the coked liquefied gas subjected to secondary desulfurization into an air tower, wherein the pressure of the air tower is 1.3MPa, the temperature is 470 ℃, and the coked liquefied gas is reacted for 25 minutes to obtain the coked liquefied gas subjected to complete desulfurization;
the mass ratio of the coking liquefied gas after the secondary desulfurization to the air is 1:37.
4. rectifying
And (3) rectifying the completely desulfurized coking liquefied gas sequentially through a depropanizer, a deethanizer and a propylene tower, and separating ethane, propane and butane to obtain crude propylene.
5. Dewatering
The crude propylene is dehydrated until the water content in the crude propylene is as low as less than 6ppm, and the propylene is obtained after drying.
Propylene obtained by purifying the coked liquefied gas by the method of example 2 has the purity of 99.97%, the yield of 96.5% and the hydrogen sulfide content of 0.03 mug/m 3 Total sulfur content of 0.29. Mu.g/m 3 。
Example 3 Process for preparing propylene by purifying coked liquefied gas
1. Preliminary desulfurization
The coking liquefied gas and hydrogen are reacted at the lower part of a reactor, the pressure in the reactor is 0.9 MPa, the reaction temperature is 255 ℃, a desulfurizing agent enters from the upper part of the reactor for preliminary desulfurization treatment, the treatment temperature is 105 ℃, and after the treatment is finished, the coking liquefied gas after the preliminary desulfurization treatment is discharged from the top of the reactor to obtain the coking liquefied gas after the preliminary desulfurization;
the mass ratio of the coking liquefied gas to the hydrogen is 1:48;
the mass ratio of the coking liquefied gas to the desulfurizing agent is 3:15;
the preparation method of the desulfurizing agent comprises the steps of modifying montmorillonite and mixing;
the modified montmorillonite is calcined at 310 ℃ for 3.3 hours, the calcined montmorillonite is naturally restored to room temperature, sulfuric acid solution is added, stirring is carried out for 1.8 hours at 65 ℃, and preliminary modified montmorillonite is obtained after centrifugation, filtration and drying;
the grain diameter of the montmorillonite is 90nm;
the mass concentration of the sulfuric acid solution is 38%;
the mass ratio of the montmorillonite to the sulfuric acid solution is 1:3;
placing the preliminary modified montmorillonite into a closed container for closed treatment, wherein the pressure in the closed container is 0.15MPa, the temperature is 160 ℃, the treatment time is 35min, the temperature is reduced to room temperature at the speed of 0.4 ℃/min after the closed treatment is finished, then deionized water, sodium dodecyl benzene sulfonate, hyaluronic acid and sodium alginate are added, the preliminary modified montmorillonite is placed into a ball mill for primary ball milling treatment, the ball-milling speed is 240rpm, the ball milling time is 50min, the ball milling temperature is 2 ℃, aluminum oxide, arabic gum and polyethylene glycol are added after the primary ball milling is finished, the secondary ball milling treatment is carried out, the ball milling speed is 14:1, the ball milling speed is 200rpm, the ball milling time is 22min, the ball milling temperature is 1.7 ℃, and the drying is carried out after the ball milling is finished, thus obtaining the modified montmorillonite;
the mass ratio of the preliminary modified montmorillonite to deionized water to sodium dodecyl benzene sulfonate to hyaluronic acid to sodium alginate to alumina to acacia gum to polyethylene glycol is 26:110:3:1:2:18.3:3.7:7.3;
mixing the modified montmorillonite, zinc oxide and deionized water, uniformly stirring, adding sodium pyrophosphate and paraffin, uniformly stirring, and drying to obtain a desulfurizing agent;
the mass ratio of the deionized water to the modified montmorillonite to the zinc oxide to the sodium pyrophosphate to the paraffin is 93:11:16:4:5.
2. Secondary desulfurization
Putting the coking liquefied gas subjected to primary desulfurization into an alcohol amine absorption tower, and removing hydrogen sulfide by utilizing an absorption liquid to obtain coking liquefied gas subjected to secondary desulfurization;
the mass ratio of the coking liquefied gas after preliminary desulfurization to the absorption liquid is 1:3.9;
the absorption liquid comprises deionized water, diisopropanolamine, polyethylene wax, sodium hydroxide and an auxiliary agent;
the mass ratio of the deionized water to the diisopropanolamine to the polyethylene wax to the sodium hydroxide to the auxiliary agent is 65:88:8:6:8;
the preparation method of the auxiliary agent comprises the steps of mixing sodium citrate, epoxidized soybean oil and aluminum oxide, performing heat treatment at 66 ℃ for 23min, and cooling to obtain the auxiliary agent;
the mass ratio of the sodium citrate to the epoxidized soybean oil to the alumina is 2:3:18.
3. Complete desulfurization
Putting the coked liquefied gas subjected to secondary desulfurization into an air tower, wherein the pressure of the air tower is 1.1MPa, the temperature is 450 ℃, and the coked liquefied gas subjected to complete desulfurization is obtained after reaction for 18 min;
the mass ratio of the coking liquefied gas after the secondary desulfurization to the air is 1:33.
4. rectifying
And (3) rectifying the completely desulfurized coking liquefied gas sequentially through a depropanizer, a deethanizer and a propylene tower, and separating ethane, propane and butane to obtain crude propylene.
5. Dewatering
The crude propylene is dehydrated until the water content in the crude propylene is as low as less than 6ppm, and the propylene is obtained after drying.
Propylene obtained by purifying the coked liquefied gas by the method of example 1 has the purity of 99.96%, the yield of 96.3% and the hydrogen sulfide content of 0.04 mug/m 3 Total sulfur content of 0.32. Mu.g/m 3 。
Comparative example 1
The modification was performed on the basis of example 1, except that the modified montmorillonite was replaced with alumina powder in the preparation method of the desulfurizing agent, and the rest of the operations were the same.
Propylene obtained by purifying the coking liquefied gas by adopting the method of comparative example 1 has the purity reaching 90.03 percent, the yield reaching 84.0 percent and the content of hydrogen sulfide reaching 0.31 mu g/m 3 Total sulfur content of 1.89. Mu.g/m 3 。
Comparative example 2
The modification of example 1 is that in the secondary desulfurization step, only diisopropanolamine is used as the absorption liquid, other components are omitted, and the rest of the operations are the same.
Propylene obtained by purifying the coking liquefied gas by adopting the method of comparative example 2 has the purity reaching 92.01 percent, the yield reaching 87.4 percent and the content of hydrogen sulfide reaching 0.26 mu g/m 3 Total sulfur content of 1.67. Mu.g/m 3 。
The percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing propylene by purifying coked liquefied gas, which is characterized by comprising the steps of primary desulfurization, secondary desulfurization, complete desulfurization, rectification and dehydration;
the primary desulfurization step comprises the steps of reacting coking liquefied gas with hydrogen at the lower part of a reactor, wherein the pressure in the reactor is 0.9-1.2 MPa, the reaction temperature is 255-265 ℃, introducing a desulfurizing agent from the upper part of the reactor to perform primary desulfurization treatment, and after the treatment is finished, discharging the coking liquefied gas subjected to the primary desulfurization treatment from the top of the reactor to obtain the coking liquefied gas subjected to the primary desulfurization;
the preparation method of the desulfurizing agent comprises the steps of modifying montmorillonite and mixing;
the modified montmorillonite is calcined for 3.1-3.3 hours at 310-330 ℃, and after the calcination is completed, the natural temperature is restored to room temperature, sulfuric acid solution is added, and stirring is carried out for 1.2-1.8 hours at 65-75 ℃, and the preliminary modified montmorillonite is obtained after centrifugation, filtration and drying;
placing the preliminary modified montmorillonite into a closed container for closed treatment, wherein the pressure in the closed container is 0.15-0.25MPa, the temperature is 160-180 ℃, the treatment time is 25-35min, the temperature is reduced to room temperature at the speed of 0.4-0.6 ℃/min after the closed treatment is finished, then deionized water, sodium dodecyl benzene sulfonate, hyaluronic acid and sodium alginate are added, the preliminary modified montmorillonite is placed into a ball mill for primary ball milling treatment, the ball material ratio is controlled to be 8-12:1, the ball milling rotating speed is 240-260rpm, the ball milling time is 30-50min, the ball milling temperature is 2-4 ℃, aluminum oxide, acacia and polyethylene glycol are added after the primary ball milling is finished, the secondary ball milling treatment is performed, the ball milling rotating speed is controlled to be 10-14:1, the ball milling rotating speed is 200-220rpm, the ball milling time is 22-28min, the ball milling temperature is 1.7-2.4 ℃, and the final modified montmorillonite is obtained after the ball milling is finished;
mixing the modified montmorillonite, zinc oxide and deionized water, uniformly stirring, adding sodium pyrophosphate and paraffin, uniformly stirring, and drying to obtain a desulfurizing agent;
the secondary desulfurization step is that the coking liquefied gas after primary desulfurization is put into an alcohol amine absorption tower, and hydrogen sulfide is removed by utilizing absorption liquid, so that the coking liquefied gas after secondary desulfurization is obtained;
the absorption liquid comprises deionized water, diisopropanolamine, polyethylene wax, sodium hydroxide and an auxiliary agent in a mass ratio of 65-75:88-92:8-11:6-8:8-10;
the preparation method of the auxiliary agent comprises the steps of mixing sodium citrate, epoxidized soybean oil and aluminum oxide, performing heat treatment at 66-70 ℃ for 23-27min, and cooling to obtain the auxiliary agent; the mass ratio of the sodium citrate to the epoxidized soybean oil to the alumina is 2-4:3-5:18-22;
the step of complete desulfurization is that the coking liquefied gas after secondary desulfurization is put into an air tower, the pressure of the air tower is 1.1-1.3MPa, the temperature is 450-470 ℃, and the coking liquefied gas after complete desulfurization is obtained after reaction for 18-25 min;
the mass ratio of the coking liquefied gas after the secondary desulfurization to the air is 1:33-37;
the rectification step is that the completely desulfurized coking liquefied gas is subjected to rectification treatment through a depropanizer, a deethanizer and a propylene tower in sequence, and ethane, propane and butane are separated out to obtain crude propylene;
the dehydration step is to dehydrate the crude propylene until the water content in the crude propylene is lower than 6ppm, and then to prepare propylene after drying.
2. A process for purifying a coked liquefied gas to produce propylene as claimed in claim 1,
in the preliminary desulfurization step, the mass ratio of the coking liquefied gas to the hydrogen is 1:48-52;
the mass ratio of the coking liquefied gas to the desulfurizing agent is 3:15-17.
3. A process for purifying a coked liquefied gas to produce propylene as claimed in claim 1,
in the step of modifying montmorillonite, the grain diameter of the montmorillonite is 90-110nm;
the mass concentration of the sulfuric acid solution is 38-42%;
the mass ratio of the montmorillonite to the sulfuric acid solution is 1:3-5.
4. A process for purifying a coked liquefied gas to produce propylene as claimed in claim 1,
in the step of modifying montmorillonite, the mass ratio of the preliminary modified montmorillonite, deionized water, sodium dodecyl benzene sulfonate, hyaluronic acid, sodium alginate, alumina, acacia gum and polyethylene glycol is 26-32:110-130:3-5:1-3:2-4:18.3-22.8:3.7-8.1:7.3-9.8.
5. A process for purifying a coked liquefied gas to produce propylene as claimed in claim 1,
in the mixing step, the mass ratio of the deionized water to the modified montmorillonite to the zinc oxide to the sodium pyrophosphate to the paraffin is 85-93:8-11:12-16:2-4:3-5.
6. A process for purifying a coked liquefied gas to produce propylene as claimed in claim 1,
in the secondary desulfurization step, the mass ratio of the coking liquefied gas after primary desulfurization to the absorption liquid is 1:3.6-3.9.
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| CN104194833A (en) * | 2014-07-15 | 2014-12-10 | 中国石油大学(华东) | Technological method for deep desulfurization of liquefied gas |
| CN106365944A (en) * | 2016-08-30 | 2017-02-01 | 宁波中金石化有限公司 | Method for preparing polymerization-grade propylene through liquefied petroleum gas separation |
| CN115216352A (en) * | 2021-04-15 | 2022-10-21 | 中国石油化工股份有限公司 | Method for producing polypropylene raw material by liquefied petroleum gas desulfurization |
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| JP2006316154A (en) * | 2005-05-12 | 2006-11-24 | Idemitsu Kosan Co Ltd | Liquefied petroleum gas for lp gas fuel cell, its desulfurization method and fuel cell system |
| CN104194833A (en) * | 2014-07-15 | 2014-12-10 | 中国石油大学(华东) | Technological method for deep desulfurization of liquefied gas |
| CN106365944A (en) * | 2016-08-30 | 2017-02-01 | 宁波中金石化有限公司 | Method for preparing polymerization-grade propylene through liquefied petroleum gas separation |
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