CN115386395A - Method for reducing cloud point of Fischer-Tropsch synthetic oil and application of complexing agent and complexing agent - Google Patents
Method for reducing cloud point of Fischer-Tropsch synthetic oil and application of complexing agent and complexing agent Download PDFInfo
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- CN115386395A CN115386395A CN202110552287.9A CN202110552287A CN115386395A CN 115386395 A CN115386395 A CN 115386395A CN 202110552287 A CN202110552287 A CN 202110552287A CN 115386395 A CN115386395 A CN 115386395A
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- 239000008139 complexing agent Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 65
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 29
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940080818 propionamide Drugs 0.000 claims abstract description 8
- 239000001913 cellulose Substances 0.000 claims abstract description 7
- 229920002678 cellulose Polymers 0.000 claims abstract description 7
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 5
- 239000008103 glucose Substances 0.000 claims abstract description 5
- -1 argil Chemical compound 0.000 claims abstract 2
- 238000001914 filtration Methods 0.000 claims description 41
- 238000000926 separation method Methods 0.000 claims description 37
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000007795 chemical reaction product Substances 0.000 claims description 28
- 230000015572 biosynthetic process Effects 0.000 claims description 25
- 238000009835 boiling Methods 0.000 claims description 25
- 238000003786 synthesis reaction Methods 0.000 claims description 25
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004064 recycling Methods 0.000 claims description 13
- 238000006317 isomerization reaction Methods 0.000 claims description 7
- 238000010668 complexation reaction Methods 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims 2
- 239000002904 solvent Substances 0.000 abstract description 20
- 230000003213 activating effect Effects 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 239000003921 oil Substances 0.000 description 116
- 238000003756 stirring Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 17
- 230000000536 complexating effect Effects 0.000 description 14
- 239000012188 paraffin wax Substances 0.000 description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 239000000843 powder Substances 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000010687 lubricating oil Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000004927 clay Substances 0.000 description 5
- 238000004898 kneading Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000001993 wax Substances 0.000 description 4
- 239000002199 base oil Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000002283 diesel fuel Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000003113 dilution method Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- CUXBWTQHRPHWCK-UHFFFAOYSA-N propan-2-ol;urea Chemical compound CC(C)O.NC(N)=O CUXBWTQHRPHWCK-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000219793 Trifolium Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 239000010742 number 1 fuel oil Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 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
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/02—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils
-
- 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
- C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/30—Physical properties of feedstocks or products
- C10G2300/304—Pour point, cloud point, cold flow properties
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (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 relates to the technical field of Fischer-Tropsch synthetic oil dewaxing processes, and discloses a method for reducing cloud point of Fischer-Tropsch synthetic oil and application of a complexing agent and a complexing agent. The complexing agent comprises a component A and a component B, wherein the component A is at least one of cellulose, glucose, urea, thiourea, acetamide and propionamide, and the component B is at least one of kieselguhr, argil, kaolin, titanium dioxide and pseudo-boehmite; wherein the component A: the mass ratio of the component B is (1-50): 1. the dewaxing method has the advantages of high dewaxing efficiency, no need of an activating agent and a solvent, simple process and easiness in realization, and can obviously reduce the cloud point of the Fischer-Tropsch synthetic oil and improve the low-temperature fluidity.
Description
Technical Field
The invention relates to the technical field of Fischer-Tropsch synthetic oil dewaxing processes, in particular to a method for reducing cloud point of Fischer-Tropsch synthetic oil and application of a complexing agent and a complexing agent.
Background
For the oil product prepared by the Fischer-Tropsch synthesis process, the content of straight-chain hydrocarbon is usually more than 90 percent, so the product can be used as the raw material of high-quality diesel oil and lubricating oil base oil. Because the oil product has the defects of higher condensation point and poorer low-temperature flow performance, the property of the oil product needs to be improved by adopting an isomerization technology. However, after the oil product prepared by the Fischer-Tropsch synthesis process is subjected to isomerization treatment, normal paraffin residues still exist in the product, so that the cloud point reduction amplitude of the product oil is low, and the low-temperature flow performance of the product oil is still not ideal. It is therefore dewaxed to lower the cloud point.
CN104560195B discloses a dewaxing method of an isopropanol urea aqueous solution, which comprises the following steps: mixing raw oil and an isopropanol urea aqueous solution, then feeding the mixture into a reactor for complex reaction, wherein the reactor is operated under a reduced pressure condition, a gas phase effluent at the top of the reactor is cooled and then circulated back to the reactor, one part of a reaction product obtained at the bottom of the reactor is returned to the reactor, and the rest part of the reaction product is removed from a complex settling washing tower for subsequent separation treatment, wherein the feeding temperature of the reactor is 60-80 ℃, the final reaction temperature is 20-32 ℃, and the operating pressure of the reactor is 22-50kPa. The method adopts isopropanol as a cooling medium, utilizes vaporization heat absorption when the isopropanol and water form an azeotrope, meets the requirement of multiple temperatures of a complex reaction, but needs to perform pressure reduction operation on a reactor.
CN102453548B discloses a solvent dewaxing process using a dewaxing aid, the process comprising: mixing a molten dewaxing raw material and a dewaxing assistant, adding a dewaxing solvent, cooling to a dewaxing temperature, filtering and separating at the dewaxing temperature by adopting a multi-point dilution method or a one-time full dilution method by adopting the solvent adding mode to obtain dewaxed oil and dewaxed cerate, wherein the dewaxing assistant is any fraction of Fischer-Tropsch synthetic wax at a temperature of more than 530 ℃. The solvent may be a C3-C6 aliphatic ketone or a mixture thereof, or a mixture of a ketone and a C6-C8 aromatic hydrocarbon. This method can increase the filtration rate but involves the use of adjuvants and solvents of the ketone and aromatic type.
CN101191083B discloses a method for reducing cloud point of solvent dewaxing oil, which comprises the following steps: a. mixing the wax-containing lubricating oil material with a dewaxing solvent, cooling to a filtering temperature, and feeding the mixture into a rotary drum filter for filtering; b. cooling the filtrate obtained in the step a to a temperature 1-5 ℃ lower than the filtering temperature of the rotary drum filter, and feeding the filtrate into a tubular filter for secondary filtration; sending the filtrate into a separation system to separate the dewaxing solvent from the dewaxing lubricating oil stock; c. and (b) stopping filtering after the difference force between the inlet and the outlet of the tubular filter is reduced to a set value, washing the wax crystals dissolved on the tubular filter by using a dewaxing solvent, and mixing the washing liquid with the wax-containing lubricating oil material in the step a. This process requires the use of dewaxing solvents, is a lengthy process flow and has specific requirements for filters.
In summary, in the prior art, an activating agent and an organic dewaxing solvent are generally required to be introduced in the dewaxing process, strict condition requirements are imposed on the reaction or filtration process, the solvent needs to be removed and recovered by multiple times of distillation in the subsequent process, the process flow is long, and the treatment period is long and the cost is high. Therefore, the method which has high dewaxing efficiency, simple and easy process and short treatment period has important practical significance.
Disclosure of Invention
The invention aims to solve the problems of high cloud point and poor low-temperature fluidity of product oil caused by residual normal paraffin which still exists after isomerization treatment of oil products prepared by a Fischer-Tropsch synthesis process and the problems of complex solvent recovery process and high energy consumption in the existing solvent dewaxing technology, and provides a method for reducing the cloud point of Fischer-Tropsch synthesis oil and application of a complexing agent and a complexing agent.
In order to achieve the above object, the first aspect of the present invention provides a complexing agent for reducing cloud point of fischer-tropsch synthesis oil, the complexing agent comprising a component a and a component B, the component a is at least one of cellulose, glucose, urea, thiourea, acetamide and propionamide, and the component B is at least one of diatomite, clay, kaolin, titanium dioxide and pseudo-boehmite; wherein,
the component A: the mass ratio of the component B is (1-50): 1.
in a second aspect, the invention provides a method of reducing the cloud point of a fischer-tropsch synthesis oil, the method comprising:
(A) Carrying out a complex reaction on Fischer-Tropsch synthetic oil and a complexing agent to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product to obtain dewaxed oil and cerate;
wherein, in the step (a), the complexing agent is the complexing agent provided in the first aspect of the present invention.
In a third aspect, the invention provides the use of a complexing agent as described in the first aspect above for reducing the cloud point of a fischer-tropsch synthesis oil.
Through the technical scheme, the method provided by the invention has the following beneficial effects:
(1) An activating agent and a solvent are not needed in the dewaxing process, so that the process of solvent recovery for multiple times is avoided, the process flow is simplified, and the energy consumption is reduced;
(2) The high-efficiency separation of normal paraffin and isoparaffin in the isomerized Fischer-Tropsch synthetic oil is realized, and the content of isoparaffin in the obtained dewaxed oil is higher than 98wt%;
(3) The cloud point of the Fischer-Tropsch synthetic oil can be remarkably reduced, after the Fischer-Tropsch synthetic oil is treated by the method, the cloud point of the obtained dewaxed oil can be reduced to-30 ℃, and the low-temperature flowing property is greatly improved;
(4) The method is not only suitable for removing residual normal paraffin in the base oil of the lubricating oil prepared by the isomerization of the Fischer-Tropsch synthetic oil, but also can effectively reduce the cloud point of diesel oil and white oil products prepared by the Fischer-Tropsch synthetic oil.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides a complexing agent for reducing cloud point of Fischer-Tropsch synthetic oil, which comprises a component A and a component B, wherein the component A is at least one of cellulose, glucose, urea, thiourea, acetamide and propionamide, and the component B is at least one of kieselguhr, white clay, kaolin, titanium dioxide and pseudo-boehmite; wherein,
the component A: the mass ratio of the component B is (1-50): 1.
in the invention, the inventor finds that a solid complexing agent containing a component A and a component B is adopted, the solid complexing agent can perform high-selectivity complexing reaction with residual normal paraffin in isomerized Fischer-Tropsch synthetic oil, the generated dewaxed oil can be used for subsequent finishing, and the generated complexing product is heated and decomposed to obtain the normal paraffin and the solid complexing agent, wherein the normal paraffin can be recovered, and the solid complexing agent can be added into raw oil to be treated again for recycling. The solid complexing agent is applied to the complexing dewaxing of the isomerized Fischer-Tropsch synthetic oil, an activating agent and a solvent in a conventional dewaxing method are not needed, a tedious solvent recovery process is avoided, the high-efficiency separation of normal paraffin and isoparaffin in the isomerized Fischer-Tropsch synthetic oil can be realized through the research on the specific component A and component B in the complexing agent and the dewaxing process conditions, the content of the isoparaffin in the obtained dewaxed oil is higher than 98wt%, the cloud point of the Fischer-Tropsch synthetic oil is greatly reduced, and the low-temperature flow performance is further improved.
In some embodiments of the invention, the complexing agent comprises component a and component B, the component a preferably being at least one of cellulose, glucose, urea, thiourea, acetamide, propionamide; the component B is preferably at least one of diatomite, clay, kaolin, titanium dioxide and pseudo-boehmite; the component A: the mass ratio of (1-50): 1.
in the present invention, the complexing agent is a solid, and the preparation process thereof may include: (1) Crushing the component A to obtain component A powder, wherein the particle size of the component A powder is preferably 100-200 meshes; (2) Crushing the component B to obtain component B powder, wherein the particle size of the component B powder is preferably 80-100 meshes; (3) Fully mixing the component A powder and the component B powder, and kneading and molding to obtain the complexing agent, wherein the mass ratio of the component A to the component B can be (1-50): 1, the shape of the complexing agent can be one of a sphere, a clover and a butterfly. The present invention is not particularly limited to the pulverization and kneading molding in the preparation of the complexing agent, and a method of pulverization and kneading molding which is conventional in the art may be employed.
In the invention, in order to enable the complexing agent to have better selective complexing effect on normal paraffin, and further obtain better dewaxing effect, more preferably, the component A is at least one of cellulose, urea, thiourea and propionamide; the component B is at least one of argil, kaolin and titanium dioxide; the component A: the mass ratio of the component B can be (2-40): 1;
further preferably, the component A is thiourea and at least one of urea and propionamide, wherein the thiourea accounts for 1/2-5/6 of the total mass of the component A; the component B is clay and kaolin, wherein the clay accounts for 1/2-7/8 of the total mass of the component B; the component A: the mass ratio of the component B is (15-30): 1.
in a second aspect, the invention provides a method of reducing the cloud point of a fischer-tropsch synthesis oil, the method comprising:
(A) Carrying out a complex reaction on Fischer-Tropsch synthetic oil and a complexing agent to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product to obtain dewaxed oil and cerate;
wherein, in the step (a), the complexing agent is the complexing agent provided by the first aspect of the present invention.
In some embodiments of the invention, the fischer-tropsch oil is an oil product obtained by isomerizing an oil produced by a fischer-tropsch synthesis process, preferably having a cloud point of from-30 ℃ to 60 ℃. The isomerization treatment can be performed by a method for performing isomerization treatment on an oil product prepared by a Fischer-Tropsch synthesis process, which is conventional in the field, for example, at least one of a full fraction comprising Fischer-Tropsch hydrofined tail oil, a narrow fraction comprising Fischer-Tropsch hydrofined tail oil and a full fraction comprising Fischer-Tropsch hydrocracked tail oil is performed in the presence of a catalyst. Wherein the catalyst comprises at least one of ZSM-12, ZSM-22, ZSM-23, ZSM-48, SAPO-11 and mordenite supported catalyst.
Preferably, the Fischer-Tropsch synthesis oil may have an initial boiling point of from 150 to 200 ℃ and an end point of from 650 to 700 ℃.
More preferably, the Fischer-Tropsch synthesis oil may have an initial boiling point of from 180 to 200 ℃ and an end point of from 650 to 680 ℃.
In some embodiments of the present invention, in step (a), the complexing reaction is preferably carried out by adding the complexing agent to the fischer-tropsch synthesis oil, mixing thoroughly and reacting. Wherein the Fischer-Tropsch synthetic oil: the mass ratio of the complexing agent can be (50-1): 1, preferably (20-1): 1.
in the present invention, in the step (a), the conditions of the complexation reaction include: the temperature may be from-5 ℃ to 100 ℃, preferably from-5 ℃ to 80 ℃; the time can be from 0.5 to 72 hours, preferably from 1 to 48 hours.
Preferably, in order to make the complexation reaction proceed more fully and further separate the residual normal paraffin from the Fischer-Tropsch synthesis oil, the conditions of the complexation reaction further comprise stirring, and the stirring speed can be 30-800 rpm, and is preferably 100-600 rpm.
In some embodiments of the present invention, in step (B), the first filtration separation may employ a filtration separation means conventional in the art, preferably one of suction filtration, pressure filtration and centrifugation. The temperature of the first filtering separation may be-35 ℃ to 100 ℃.
Preferably, the temperature of the first filtering separation may be-35 ℃ to 60 ℃ in order to obtain a better filtering separation effect on the reaction product.
In the invention, after the first filtration and separation, the obtained cerate is a complex reaction product and is white pasty, and the main components of the cerate comprise the complexed normal alkane, the complexing agent and a small amount of attached isoparaffin; the obtained dewaxed oil is a product, wherein the content of isoparaffin is higher than 98wt%, and the content of residual normal paraffin is very low, so that compared with the Fischer-Tropsch synthetic oil before being treated by the method, the cloud point of the dewaxed oil is greatly reduced, the low-temperature flow property is greatly improved, and the dewaxed oil can meet the raw material index requirements of high-quality diesel oil and lubricating oil base oil.
In some embodiments of the present invention, preferably, the method for lowering cloud point of fischer-tropsch synthesis oil further comprises: heating the cerate and carrying out second filtration and separation in sequence to obtain normal alkane and the complexing agent; wherein the complexing agent is returned to the step (A) for recycling.
In the present invention, the cerate is heated in order to decompose the cerate to remove and recover the normal alkane complexed therein. The heating may be performed in a manner conventional in the art, and is not particularly limited in the present application. The heating conditions include: the temperature can be 80-200 ℃, and the time can be 1-72h; preferably, the temperature may be 80-180 ℃ and the time may be 2-48h.
In the present invention, the conditions for the second filtration separation are not particularly limited as long as sufficient separation of the normal paraffin and the complexing agent can be achieved.
In the present invention, the above-mentioned recycling may be performed by returning the complexing agent obtained by the second filtration and separation to the step (a) as a dewaxing complexing agent alone, or by returning the complexing agent mixed with a fresh complexing agent to the step (a) as a dewaxing complexing agent together.
In a third aspect, the invention provides the use of a complexing agent as described in the first aspect above for reducing the cloud point of a fischer-tropsch synthesis oil.
The present invention will be described in detail below by way of examples. In the following examples and comparative examples,
the preparation process of the complexing agent used in the invention is as follows:
(1) Placing the component A in a grinder for grinding treatment to obtain component A powder with the particle size of 100-200 meshes;
(2) Placing the component B in a grinder for grinding treatment to obtain component B powder with the particle size of 80-100 meshes;
(3) And fully mixing the component A powder and the component B powder which are respectively prepared according to the mass ratio, and then kneading and molding in a kneading machine to obtain the complexing agent.
The complexing agents (designated as L1-L11, respectively) used in examples 1-11 were prepared using the procedure described above, and the compositional parameters of the complexing agents are shown in Table 1.
TABLE 1
The Fischer-Tropsch synthetic oil is purchased from coal oil preparation companies of national energy group Ningxia coal industry group Limited liability companies.
Example 1
(A) Adding a complexing agent L1 into Fischer-Tropsch synthetic oil (cloud point is 42 ℃, initial boiling point is 200 ℃ and final boiling point is 650 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L1 is 10), wherein the reaction temperature is-5 ℃, the reaction time is 48h, and the stirring speed is 300 revolutions per minute, so as to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product at-35 ℃ to obtain dewaxed oil P1 and cerate;
(C) And heating the cerate at 80 ℃ for 2h, and then carrying out second filtration and separation to obtain the n-alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 2
The procedure is as in example 1, except that a complexing agent L2 is used. Other conditions were the same as in example 1. Dewaxed oil P2 is obtained.
Example 3
The procedure is as in example 1, except that a complexing agent L3 is used. Other conditions were the same as in example 1. Dewaxed oil P3 was obtained.
Example 4
(A) Adding a complexing agent L4 into Fischer-Tropsch synthetic oil (the cloud point is 23 ℃, the initial boiling point is 200 ℃ and the final boiling point is 680 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L4 is 20: 1), wherein the reaction temperature is 50 ℃, the reaction time is 10h, and the stirring speed is 600 revolutions per minute, so as to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product at the temperature of 60 ℃ to obtain dewaxed oil P4 and cerate;
(C) And heating the cerate for 35h at the temperature of 100 ℃, and then carrying out second filtration and separation to obtain the normal alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 5
(A) Adding a complexing agent L5 into Fischer-Tropsch synthetic oil (the cloud point is-30 ℃, the initial boiling point is 180 ℃ and the final boiling point is 680 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L5 is 1:1), the reaction temperature is 80 ℃, the reaction time is 1h, and the stirring speed is 100 r/min, so as to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product at the temperature of-5 ℃ to obtain dewaxed oil P5 and cerate;
(C) And heating the cerate for 48h at 150 ℃, and then carrying out second filtration and separation to obtain the normal alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 6
(A) Adding a complexing agent L6 into Fischer-Tropsch synthetic oil (the cloud point is 60 ℃, the initial boiling point is 200 ℃ and the final boiling point is 660 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L6 is 5:1), wherein the reaction temperature is 20 ℃, the reaction time is 25h, and the stirring speed is 500 r/min, so as to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product at the temperature of-15 ℃ to obtain dewaxed oil P6 and cerate;
(C) And heating the cerate for 10 hours at 180 ℃, and then carrying out second filtration and separation to obtain the normal alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 7
(A) Adding a complexing agent L7 into Fischer-Tropsch synthetic oil (cloud point is-14 ℃, initial boiling point is 150 ℃ and final boiling point is 650 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L7 is 30: 1), wherein the reaction temperature is 100 ℃, the reaction time is 50h, and the stirring speed is 700 revolutions per minute, so as to obtain a reaction product;
(B) Performing first filtration separation on the reaction product at 100 ℃ to obtain dewaxed oil P7 and cerate;
(C) And heating the cerate for 20h at the temperature of 90 ℃, and then carrying out second filtration and separation to obtain the n-alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 8
(A) Adding a complexing agent L8 into Fischer-Tropsch synthetic oil (cloud point is 60 ℃, initial boiling point is 160 ℃ and final boiling point is 650 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L8 is 50: 1), wherein the reaction temperature is 40 ℃, the reaction time is 0.5h, and the stirring speed is 30 r/min, so as to obtain a reaction product;
(B) Performing first filtration separation on the reaction product at 60 ℃ to obtain dewaxed oil P8 and cerate;
(C) And heating the cerate for 1h at the temperature of 200 ℃, and then carrying out second filtration and separation to obtain the n-alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 9
(A) Adding a complexing agent L9 into Fischer-Tropsch synthetic oil (cloud point is 15 ℃, initial boiling point is 175 ℃ and final boiling point is 650 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L9 is 25: 1), wherein the reaction temperature is 0 ℃, the reaction time is 20h, and the stirring speed is 400 r/min, so as to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product at the temperature of 0 ℃ to obtain dewaxed oil P9 and cerate;
(C) And heating the cerate for 55 hours at 160 ℃, and then carrying out second filtration and separation to obtain the normal alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 10
(A) Adding a complexing agent L10 into Fischer-Tropsch synthetic oil (cloud point is-30 ℃, initial boiling point is 160 ℃ and final boiling point is 690 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L10 is 40: 1), wherein the reaction temperature is 70 ℃, the reaction time is 72h, and the stirring speed is 800 revolutions per minute, so as to obtain a reaction product;
(B) Performing first filtration separation on the reaction product at-35 ℃ to obtain dewaxed oil P10 and cerate;
(C) And heating the cerate for 72 hours at the temperature of 120 ℃, and then carrying out second filtration and separation to obtain the normal alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Example 11
(A) Adding a complexing agent L11 into Fischer-Tropsch synthetic oil (the cloud point is 35 ℃, the initial boiling point is 155 ℃ and the final boiling point is 700 ℃), and carrying out a complexing reaction under the stirring condition (the mass ratio of the Fischer-Tropsch synthetic oil to the complexing agent L11 is 35: 1), wherein the reaction temperature is 20 ℃, the reaction time is 60h, and the stirring rate is 200 r/min, so as to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product at 10 ℃ to obtain dewaxed oil P11 and cerate;
(C) And heating the cerate for 60h at 110 ℃, and then carrying out second filtration and separation to obtain the normal alkane and the complexing agent. Recovering the normal alkane, and returning the complexing agent to the step (A) for recycling.
Comparative example 1
The procedure is as in example 1, except that the complexing agent, component A: the mass ratio of the component B is 60. Other conditions were the same as in example 1. Dewaxed oil D1 was obtained.
Comparative example 2
The procedure of example 1 was followed except that the Fischer-Tropsch synthesis oil: the mass ratio of the complexing agent L1 is 55. Other conditions were the same as in example 1. Dewaxed oil D2 was obtained.
Comparative example 3
The procedure is as in example 1, except that the reaction temperature in step (A) is 110 ℃. Other conditions were the same as in example 1. Dewaxed oil D3 was obtained.
Comparative example 4
The procedure is as in example 1, except that the reaction time in step (A) is 0.2h. Other conditions were the same as in example 1. Dewaxed oil D4 was obtained.
Comparative example 5
The procedure is as in example 1, except that the complexing agent does not comprise component B. Other conditions were the same as in example 1. Dewaxed oil D5 was obtained.
Comparative example 6
The procedure is as in example 1, except that the complexing agent does not comprise component A. Other conditions were the same as in example 1. Dewaxed oil D6 was obtained.
Comparative example 7
Adding the prepared dewaxing liquid (the mass ratio of urea to isopropanol to water is 5: 4) into Fischer-Tropsch synthetic oil (the cloud point is 42 ℃, the initial boiling point is 200 ℃, and the final boiling point is 650 ℃) at 50 ℃, wherein the weight ratio of the Fischer-Tropsch synthetic oil: the mass ratio of the dewaxing liquid is 1:3. stirring for 48h at the stirring speed of 300 r/min and the temperature of 50 ℃, and then filtering and separating at-10 ℃ to obtain dewaxed oil, an alcohol-water solution and cerate;
heating the dewaxed oil to 90 ℃ to remove isopropanol to obtain dewaxed oil D7; recovering isopropanol from the alcohol aqueous solution by distillation to obtain 85wt% isopropanol aqueous solution; adding water into the cerate and heating to 80 ℃ to obtain urea aqueous solution and normal alkane.
Test example
The dewaxed oils (P1 to P11, D1 to D7) obtained in examples 1 to 11 and comparative examples 1 to 7 were subjected to a cloud point test and an isoparaffin content test, and the cloud point of the dewaxed oil was compared with the cloud point of the Fischer-Tropsch synthesis oil before the dewaxing treatment,
cloud point: measuring with an automatic pour point and cloud point tester (Haicheng, manufacturer, model HCP-852);
content of isoparaffin: the measurement was carried out by gas chromatography (manufacturer Agilent, model 7890B).
The test results are shown in table 2.
TABLE 2
As can be seen from the results of examples 1 to 11 and the comparative example, when the Fischer-Tropsch synthetic oil is treated by the complexing agent and the method, compared with the Fischer-Tropsch synthetic oil before treatment, the cloud point of the obtained product dewaxed oil is remarkably reduced in different ranges, so that the low-temperature fluidity is remarkably improved, and the specific expression is as follows: for the raw oil with high self cloud point (such as the Fischer-Tropsch synthetic oil used in examples 1-3, 6 and 8), the cloud point is greatly reduced after the treatment; for raw oils with lower self-cloud points (such as the Fischer-Tropsch synthesis oils used in examples 4, 9 and 11), a significant decrease in cloud point after treatment also occurs; for feedstock oils with lower cloud points (such as the Fischer-Tropsch synthesis oils used in examples 5, 7 and 10), the cloud point reduction effect is also significant, since the cloud point of the feedstock oil itself is already at a lower level, although there is a difference between the cloud point reduction and the former two after the treatment. In examples 1 to 11, the isoparaffin content in the obtained dewaxed oil can reach more than 98wt%, and the normal paraffin recovery rate is high. In contrast, comparative examples 1 to 7, which did not employ the complexing agent or method of the present invention, did not exhibit the desired cloud point reduction and low temperature flow improvement effects of the dewaxed oil obtained after the treatment, as compared with example 1.
In particular, comparative example 1, comparative example 5 and comparative example 6 do not adopt the complexing agent in the invention, and have poor dewaxing effect, so that the cloud point reduction amplitude and the isoparaffin content of the product dewaxed oil are lower than those of example 1; comparative example 5, in which component B was not contained in the complexing agent, and comparative example 6, in which component a was not contained in the complexing agent, both obtained cloud point lowering effects significantly lower than those of example 1 (in which both component a and component B were contained in the complexing agent); comparative example 7 using a conventional solvent dewaxing process, the product dewaxed oil had a significantly lower cloud point reduction and isoparaffin content than example 1, which is significantly different from the technical effects of the present application.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. The complexing agent for reducing the cloud point of Fischer-Tropsch synthetic oil is characterized by comprising a component A and a component B, wherein the component A is at least one of cellulose, glucose, urea, thiourea, acetamide and propionamide, and the component B is at least one of kieselguhr, argil, kaolin, titanium dioxide and pseudo-boehmite; wherein,
the component A: the mass ratio of the component B is (1-50): 1.
2. the complexing agent according to claim 1 wherein component a is at least one of cellulose, urea, thiourea, propionamide;
the component B is at least one of argil, kaolin and titanium dioxide;
the component A: the mass ratio of the component B is (2-40): 1.
3. a method of reducing the cloud point of a fischer-tropsch synthesis oil, the method comprising:
(A) Carrying out a complex reaction on Fischer-Tropsch synthetic oil and a complexing agent to obtain a reaction product;
(B) Carrying out first filtration separation on the reaction product to obtain dewaxed oil and cerate;
wherein, in step (a), the complexing agent is the complexing agent of claim 1 or 2.
4. The method according to claim 3, wherein in the step (A), the Fischer-Tropsch synthesis oil is a product obtained by subjecting an oil product prepared by a Fischer-Tropsch synthesis process to isomerization treatment;
preferably, the cloud point of the Fischer-Tropsch synthetic oil is from-30 ℃ to 60 ℃;
preferably, the initial boiling point of the Fischer-Tropsch synthetic oil is 150-200 ℃, and further preferably 180-200 ℃; the final boiling point of the Fischer-Tropsch synthetic oil is 650-700 ℃, and the final boiling point is more preferably 650-680 ℃.
5. The process of claim 3 or 4, wherein in step (A), the Fischer-Tropsch synthesis oil: the mass ratio of the complexing agent is (1-50): 1, preferably (1-20): 1.
6. the method according to any one of claims 3 to 5, wherein in step (A), the conditions of the complexation reaction include: the temperature is-5 ℃ to 100 ℃, preferably-5 ℃ to 80 ℃; the time is 0.5 to 72 hours, preferably 1 to 48 hours;
preferably, the conditions of the complexation reaction further comprise agitation, the rate of agitation being from 30 to 800 rpm, preferably from 100 to 600 rpm.
7. The method of any one of claims 3-6, wherein in step (B), the conditions of the first filtering separation comprise: the temperature is from-35 ℃ to 100 ℃, preferably from-35 ℃ to 60 ℃.
8. The method of any of claims 3-7, wherein the method further comprises: heating the cerate and carrying out second filtering separation to obtain normal alkane and the complexing agent;
wherein the complexing agent is returned to the step (A) for recycling.
9. The method of claim 8, wherein the heated conditions comprise: the temperature is 80-200 ℃, preferably 80-180 ℃; the time is 1-72h, preferably 2-48h.
10. Use of the complexing agent of claim 1 or 2 to lower the cloud point of a fischer-tropsch synthesis oil.
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