CN105498280B - A kind of method of the reversible solvent assisting oil-sand separation of hydrophily - Google Patents
A kind of method of the reversible solvent assisting oil-sand separation of hydrophily Download PDFInfo
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- CN105498280B CN105498280B CN201510999342.3A CN201510999342A CN105498280B CN 105498280 B CN105498280 B CN 105498280B CN 201510999342 A CN201510999342 A CN 201510999342A CN 105498280 B CN105498280 B CN 105498280B
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- 239000002904 solvent Substances 0.000 title claims abstract description 116
- 239000003027 oil sand Substances 0.000 title claims abstract description 64
- 230000002441 reversible effect Effects 0.000 title claims abstract description 62
- 230000010148 water-pollination Effects 0.000 title claims abstract description 50
- 238000000926 separation method Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000605 extraction Methods 0.000 claims abstract description 84
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000003960 organic solvent Substances 0.000 claims abstract description 61
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 239000004576 sand Substances 0.000 claims abstract description 52
- 238000009938 salting Methods 0.000 claims abstract description 47
- 238000005406 washing Methods 0.000 claims abstract description 41
- 238000004064 recycling Methods 0.000 claims abstract description 38
- 238000011084 recovery Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims description 61
- 150000003512 tertiary amines Chemical class 0.000 claims description 53
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- 150000003863 ammonium salts Chemical class 0.000 claims description 26
- 239000012266 salt solution Substances 0.000 claims description 23
- 150000001412 amines Chemical class 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- 238000000638 solvent extraction Methods 0.000 claims description 13
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 12
- 239000012074 organic phase Substances 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 150000003335 secondary amines Chemical class 0.000 claims description 6
- -1 N- phenpromethamine Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001409 amidines Chemical class 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000011280 coal tar Substances 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- HTLZVHNRZJPSMI-UHFFFAOYSA-N N-ethylpiperidine Chemical compound CCN1CCCCC1 HTLZVHNRZJPSMI-UHFFFAOYSA-N 0.000 claims description 3
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 claims description 3
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical class CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 3
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 claims description 3
- OBYVIBDTOCAXSN-UHFFFAOYSA-N n-butan-2-ylbutan-2-amine Chemical compound CCC(C)NC(C)CC OBYVIBDTOCAXSN-UHFFFAOYSA-N 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 claims description 2
- JSHASCFKOSDFHY-UHFFFAOYSA-N 1-butylpyrrolidine Chemical class CCCCN1CCCC1 JSHASCFKOSDFHY-UHFFFAOYSA-N 0.000 claims description 2
- UHOPWFKONJYLCF-UHFFFAOYSA-N 2-(2-sulfanylethyl)isoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(CCS)C(=O)C2=C1 UHOPWFKONJYLCF-UHFFFAOYSA-N 0.000 claims description 2
- DJEQZVQFEPKLOY-UHFFFAOYSA-N N,N-dimethylbutylamine Chemical compound CCCCN(C)C DJEQZVQFEPKLOY-UHFFFAOYSA-N 0.000 claims description 2
- 125000003368 amide group Chemical group 0.000 claims description 2
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 2
- ORSUTASIQKBEFU-UHFFFAOYSA-N n,n-diethylbutan-1-amine Chemical compound CCCCN(CC)CC ORSUTASIQKBEFU-UHFFFAOYSA-N 0.000 claims description 2
- ZYWUVGFIXPNBDL-UHFFFAOYSA-N n,n-diisopropylaminoethanol Chemical compound CC(C)N(C(C)C)CCO ZYWUVGFIXPNBDL-UHFFFAOYSA-N 0.000 claims description 2
- UVBMZKBIZUWTLV-UHFFFAOYSA-N n-methyl-n-propylpropan-1-amine Chemical class CCCN(C)CCC UVBMZKBIZUWTLV-UHFFFAOYSA-N 0.000 claims description 2
- HUAZGNHGCJGYNP-UHFFFAOYSA-N propyl butyrate Chemical compound CCCOC(=O)CCC HUAZGNHGCJGYNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 1
- QMHNQZGXPNCMCO-UHFFFAOYSA-N n,n-dimethylhexan-1-amine Chemical class CCCCCCN(C)C QMHNQZGXPNCMCO-UHFFFAOYSA-N 0.000 claims 1
- 229950010364 phenpromethamine Drugs 0.000 claims 1
- 239000010426 asphalt Substances 0.000 abstract description 18
- 238000004821 distillation Methods 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000001172 liquid--solid extraction Methods 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 50
- 239000003921 oil Substances 0.000 description 47
- 239000001569 carbon dioxide Substances 0.000 description 25
- 229910002092 carbon dioxide Inorganic materials 0.000 description 25
- 239000007789 gas Substances 0.000 description 19
- 239000000203 mixture Substances 0.000 description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- 239000000654 additive Substances 0.000 description 12
- 230000000996 additive effect Effects 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 6
- 238000013019 agitation Methods 0.000 description 6
- 239000008346 aqueous phase Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 230000003519 ventilatory effect Effects 0.000 description 6
- 238000003912 environmental pollution Methods 0.000 description 5
- 238000005065 mining Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 210000002966 serum Anatomy 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000011859 microparticle Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- DEQYTNZJHKPYEZ-UHFFFAOYSA-N ethyl acetate;heptane Chemical group CCOC(C)=O.CCCCCCC DEQYTNZJHKPYEZ-UHFFFAOYSA-N 0.000 description 2
- JYGYEBCBALMPDC-UHFFFAOYSA-N heptane;propan-2-one Chemical group CC(C)=O.CCCCCCC JYGYEBCBALMPDC-UHFFFAOYSA-N 0.000 description 2
- KDCIHNCMPUBDKT-UHFFFAOYSA-N hexane;propan-2-one Chemical compound CC(C)=O.CCCCCC KDCIHNCMPUBDKT-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- QYNZYUUXSVZDJO-UHFFFAOYSA-N n-propylbutan-2-amine Chemical compound CCCNC(C)CC QYNZYUUXSVZDJO-UHFFFAOYSA-N 0.000 description 2
- 239000004058 oil shale Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000013517 stratification Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- KPAMAAOTLJSEAR-UHFFFAOYSA-N [N].O=C=O Chemical compound [N].O=C=O KPAMAAOTLJSEAR-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000004915 dibutylamino group Chemical group C(CCC)N(CCCC)* 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000002358 oil sand bitumen Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- VSRBKQFNFZQRBM-UHFFFAOYSA-N tuaminoheptane Chemical compound CCCCCC(C)N VSRBKQFNFZQRBM-UHFFFAOYSA-N 0.000 description 1
- 229960003986 tuaminoheptane Drugs 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
- C10G1/045—Separation of insoluble materials
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method of the reversible solvent assisting oil-sand separation of hydrophily, liquid-solid extraction organic solvent and the reversible solvent salting liquid of hydrophily, for oil-sand extraction and separation, carry out simultaneously into extraction equipment at ranging from 15 60 DEG C of pitch separation temperatures.Product discharge and reagent recycling organic solvent are collected at 70 200 DEG C through distillation, and distillation residual organic substances are asphaltic products.Reach clean discharging through a small amount of washing, residual sand product under residual sand room temperature after oil-sand separation.The reversible solvent salting liquid recovered temperature of hydrophily after use is 40 100 DEG C, and the reversible solvent of hydrophily and water after recycling can be recycled, energy saving and environmentally friendly；Assist separation method bitumen recovery efficient, up to 99%, remaining organic matter is few in residual sand.
Description
Technical field
The present invention relates to a kind of separation methods that asphalt component is isolated from oil-sand, belong to technical field of chemical separation,
More particularly to using a kind of new additive agent secondary organic solvent extraction and separation oil sands bitumen method and additive and residual solids
Post-processing approach.
Background technology
Oil-sand is a kind of by sand grains, pitch, water, clay and the natural minerals of a small amount of mineral composition, and appearance is in black or black
Brown.It is found for the first time in Canadian Alberta province within 1902, is a kind of unconventional energy resource, global oil-sand resource amount is about
It is 3.74 × 1012Bucket.
Oil-sand resource of the Canada containing more than 75% whole world, the exploitation for the oil-sand that takes the lead in carrying out in countries in the world is with grinding
Study carefully, possess the most ripe technology in the whole world at present.The oil-sand resource of China is mainly distributed on the ground such as Tarim, Xinjiang and Guizhou, mesh
It is preceding not yet to realize industrialized production.The method of oil-sand exploitation mainly has strip mining transformation and in-situ extraction, the former is suitable for oil-sand ore deposit
Buried depth is less than 75 meters of oily placer mining, and the latter is more than the exploitation of 75 meters of oil-sand ore deposit for oil-sand ore deposit buried depth.Just
For strip mining transformation, mainly there is that thermokalite washing process, solvent extraction technology, thermal cracking process etc. are several, it is industrial at present to use
Comparative maturity is thermokalite WATER-WASHING METHOD, which first crushes oil-sand, be re-fed into heat alkali liquid and be mixed, then to mixing slurry
Gas is passed through in liquid to be made in pitch flotation, after collecting pitch and adding in alkane dilution to reduce its viscosity, is sent to refinery's progress
Refining obtains various oil products.The technical operation is simple, but has the disadvantage that and technical bottleneck：Water consumption is big, high energy consumption, tail
Ore deposit processing is extremely difficult, environmental pollution is serious, has been subjected to all over the world, especially the attention of mining area local resident and matter
It doubts.Searching environmental protection, economy, the oil sand separating method of sustainable development are extremely urgent.
Solvent extraction can be eliminated to a certain extent due to it is suitable for the separation of lipophile and hydrophily oil-sand
Emulsion reduces the pollution to environment, has obtained extensive attention.Compared with traditional WATER-WASHING METHOD, extracted using solvent
Without sand in the oil obtained, and water is not used in overall process, reduce energy consumption, improve extraction efficiency, reduced pair
The pollution of environment.There is also some the technical issues of to be solved for traditional solvent extraction technology：Efficiently, economic solvent is not easy
In acquisition；It is larger etc. to remain on solvent recovery difficulty in solid particles of sand.
It is dedicated to research there are many experts and scholars at present to extract using additive secondary solvent, so as to reach raising oil-sand
Bitumen extraction rate reduces the fine sand entrainment in pitch and reduces the purpose of dissolvent residual in residual sand.CN 102391185A(2012)
The additive for using ionic liquid as solvent extraction oil-sand pitch is reported, bitumen extraction rate can be improved, but due to ion
Liquid involves great expense, although can be recycled by way of evaporating moisture, its loss in the process still limits it
Commercial Application.US 4929341 (1990) report ammonium sulfate, acetone, sulfuric acid etc. can promote organic solvent (tetrachloro-ethylene,
Carbon tetrachloride, petroleum ether, toluene, benzene etc.) to the effect of extracting of oil-sand, but this technology need to extract 4 hours right and lefts can obtain compared with
Good effect.Comprehensive forefathers are encountered about the patented technology that additive secondary solvent abstraction technique is used to detach oil-sand
A common problem be exactly process problem about suspension microparticle in sand residual after extraction and extract liquor, some technologies can reach
Higher extraction efficiency, but can not solve the problems, such as solvent recovery in residue, what is had can solve solvent recovery in residue
Problem, but economic cost is too high, can not industrializing implementation, these are also why solvent extraction technology always can not up to now
Really the reason of input industrial application；Therefore, solvent extraction will obtain industrialization and use, it is necessary to which solution remains on molten in solid
Agent and the recycling of pitch organic matter and the synthtic price index such as additive recycling problem and entire process economics, environmentally friendly running.
The reversible tertiary amine of hydrophily is a kind of novel intelligent solvent occurred in recent years.This tertiary amine can be in water and titanium dioxide
It is dissolved in water under carbon existence condition by generating tertiary amine bicarbonate, and in the item for heating or being passed through the inert gases such as nitrogen
Carbon dioxide is can release under part, with water stratification, so as to be reduced to hydrophobic tertiary amine, realizes the reversible process of hydrophily.
Based on current research, introduce the reversible tertiary amine auxiliary extraction of hydrophily in traditional organic solvent, separation it is better, simultaneously
The organic solvent and tertiary amine used is more easy to recycle, and prospects for commercial application is boundless.
Invention content
The purpose of the present invention is research, one kind has fewer environmental impacts, low energy consumption, water consumption is few, simple and practicable and efficiently extract
The separation method of asphalt component in oil-sand.This method is taken in the reversible tertiary amine salting liquid secondary organic solvent separation oil-sand of hydrophily
Asphalt component, can be at 15-60 DEG C of temperature, normal pressure by the drip in oil-sand by coordinating the corresponding technique in the present invention
Green component efficiently separates.
The technical solution adopted by the present invention to solve the technical problems is：
A kind of method of organic solvent separation oil-sand, organic solvent add in the reversible solvent of hydrophily as auxiliary when extracting oil-sand
Help additive.
Moreover, the reversible solvent of hydrophily is：It can be under water and carbon dioxide existence condition by generating corresponding carbon
Sour hydrogen salt and be dissolved in water, and carbon dioxide is can release under conditions of heating or being passed through the inert gases such as nitrogen, with water
Layering, is reduced to hydrophobic solvent containing N, realizes the organic matter containing N of the reversible process of hydrophily.
Moreover, in the reversible solvent of hydrophily tertiary amines for triethylamine, N, N- dimethyl cyclohexyl amines, N, N- dimethylbenzyls
Amine, N, N- dimethyl butylamines, N-ethylpiperidine, N- methyl-di-n-propylamines, N- butyl pyrrolidines, N, N- diethyl butylamine, N, N- bis-
Penta amidine of tuaminoheptane, N, N- phenpromethamines, N, N, N '-triethyl group, the own amidine of N, N, N '-tributyl, diisopropyl ethanolamine,
4,4- diethoxies-N, N- dimethyl butylamine, 4- diethylin ethyl butyrate, 5- dipropyls amido -2 pentanone, dibutylamino second
Alcohol；Secondary amine class is di-n-propylamine, 3- sec-butylamine guanidine-acetic acids propyl ester, 3- isopropylamine bases propyl butyrate, 3- sec-butylamine bases propyl propionate, N-
Propyl sec-butylamine, di-sec-butyl amine.
Moreover, the organic solvent is the single organic solvent of benzene,toluene,xylene or Reformed Gasoline or is acetone-alkane
Hydro carbons complex solvent, ethyl acetate-alkanes complex solvent.
Moreover, the acetone-alkanes complex solvent is acetone-normal heptane, acetone-n-hexane, and acetone-cycloalkane, third
Ketone-petroleum ether or acetone-naphtha.
Moreover, the ethyl acetate-alkanes complex solvent is ethyl acetate-normal heptane, ethyl acetate-hexane, second
Acetoacetic ester-cycloalkane, ethyl acetate-light petrol or ethyl acetate-naphtha.
Moreover, the raw material amine of the reversible solvent salting liquid of hydrophily is 1 with water volume ratio:1-10；Hydrophily is reversible molten
Agent salting liquid adds the 1-5L/kg that volume is with oil-sand mass ratio；Organic solvent volume is 1-12 times of L/kg with oil-sand mass ratio.
A kind of method of recyclable organic solvent separation oil-sand, step are as follows：
(1) the reversible solvent salting liquid of synthesis hydrophilic；
(2) hybrid extraction：Organic solvent and the reversible solvent salting liquid of hydrophily carry out oil-sand extraction simultaneously into extraction equipment
Take separation；The 1-5L/kg that the reversible solvent salting liquid addition volume of hydrophily is with oil-sand mass ratio；Organic solvent volume and oil-sand
Mass ratio is 1-12 times of L/kg；
(3) separation of solid and liquid：Mixing solid-liquid after extraction is stood, the upper phase organic solvent/coal tar isolated
Mixture is detached, and solvent recovery uses, pitch oil refinement；
(4) the grains of sand+the ammonium salt solution for standing rear lower is washed, the residual sand after washing is discharged by bottom；
(5) ammonium salt solution is passed through reaction kettle, is pumped into air and heats 40-100 DEG C simultaneously, recycling amine and recycling after reaction
Water is recycled, and completes whole circular response.
(6) the recycling of ammonium salt and water：Ammonium salt two level stood in the ammonium salt solution and washing kettle separated in the middle part of slot is dilute
Solution is passed through reaction kettle, and air is passed through into reaction kettle, recycling amine and recycle-water after reaction, and unreacted air is arranged from kettle top
Go out.
Moreover, (4) the step stands the grains of sand+ammonium salt solution progress reextraction of rear lower after, then washed；Institute
Stating reextraction step is：Lower floor's ammonium salt solution+grains of sand are subjected to two level extraction, add the organic of the quality such as 1-3 times of solid
Solvent extraction is stood after extraction；By upper organic phase by the processing of step (3), the grains of sand+ammonium salt solution of lower part carries out water again
It washes.
Moreover, the organic solvent is the single organic solvent of benzene,toluene,xylene or Reformed Gasoline or is acetone-alkane
Hydro carbons complex solvent, ethyl acetate-alkanes complex solvent.
The beneficial effects of the invention are as follows：
1st, the reversible solvent salting liquid of hydrophily is applied to the separation of oil sands bitumen by this method, is collectively formed with organic solvent
Environment-friendly type Diversity release agent；Hybrid separation agent improves bitumen recovery rate, can reach 99%, is remained in residual sand organic
Object is few；Residual sand after extraction can remove the ammonium salt on grains of sand surface, energy-saving and water-saving environmental protection with a small amount of washing.
2nd, the present invention makes the reversible solvent of hydrophily can be real in whole process with water by the flow process of reasonable design
It now recycles, and operating condition is mild, it is greatly cost-effective.
3rd, the present invention adds organic solvent extract in oil-sand separation, and the oil sands bitumen oil extracted is not required to additionally add
Diluent is added to be diluted pitch, extract liquor is directly delivered to refinery, solvent recycling is then demultiplex out, reduces centre
Link has saved intermediary operation cost.
4th, it is proposed that being extracted using the method for multistage (1-2 grades) extractions to oil-sand, extraction effect is not only increased
Rate；Moreover, extraction process can operate continuously, stability is good, ensure that the continuity of production, improves production efficiency.
Description of the drawings
Fig. 1：The process flow chart of separation method of the present invention.
Stock number：1. amine, 2. water, 3. carbon dioxide, 4. ammonium salt solutions, 5. cycle solvents, 6. oil-sands or oil shale mine,
7. organic solvent/ammonium salt solution/grains of sand mixed serum I, the 8. ammonium salt solutions+grains of sand, 9. solvents/pitch oil mixture, 10. cycles
Solvent, 11. organic solvents/ammonium salt solution/grains of sand mixed serum II, 12. solvents/pitch oil mixture, 13. grains of sand+a small amount of ammonium
Salting liquid, 14. ammonium salt solutions, 15. fresh waters, the grains of sand after 16. washings, 17. ammonium salt weak solutions, 18. air, 19. recycling amine,
20. recycle-water, 21. solvents/pitch oil mixture, product after 22. refinings, 23. recycling designs.
Device is numbered：24. amine recycling can, 25. water recovery tanks, 26. reaction kettles I, 27. level-one extraction kettles, 28. cycle solvents
Tank, 29. level-ones stand slot, 30. two level extraction kettles, and 31. two levels stand slot, 32. washing kettles, 33. reaction kettles II, 34. solvents/drip
Green oil tank, 35. refined units.
Specific embodiment
Below in conjunction with the accompanying drawings and pass through specific embodiment the invention will be further described, following embodiment is descriptive
, it is not limited, it is impossible to which protection scope of the present invention is limited with this.
The present invention provides a kind of application of reversible solvent of hydrophily as the auxiliary additive of organic solvent separation oil-sand, institute
The reversible solvent of hydrophily is stated as triethylamine, N, N- dimethyl cyclohexyl amines, N, N- dimethyl benzylamines and any satisfaction：It can be in water
It is dissolved in water under carbon dioxide existence condition by generating bicarbonate, and is heating or be passed through the inert gases such as nitrogen
Under conditions of can release carbon dioxide, with water stratification, be reduced to hydrophobic amine, realize the uncle of the reversible process of hydrophily
Amine or secondary amine.Organic solvent can be the single organic solvent of benzene,toluene,xylene or Reformed Gasoline or be acetone-alkanes
Complex solvent, ethyl acetate-alkanes complex solvent.
The acetone-alkanes complex solvent is acetone-normal heptane, acetone-n-hexane, acetone-cycloalkane, acetone-stone
Oily ether or acetone-naphtha.The ethyl acetate-alkanes complex solvent is ethyl acetate-normal heptane, ethyl acetate-just oneself
Alkane, ethyl acetate-cycloalkane, ethyl acetate-light petrol or ethyl acetate-naphtha.
According to the guidance of above application, the present invention also provides a kind of reversible solvent secondary organic solvent extraction oils of hydrophily
The method of sand separation, the separation method extract oil-sand using organic solvent, the reversible solvent of hydrophily as additive not
Bitumen recovery rate can only be improved, additionally it is possible to effectively reduce the fine content in recycling pitch, while reduce the solvent in residual sand
Content, additive can recycle, and reduce environmental pollution, saved solvent materials, improve comprehensive utilization of energy rate, tool
Body step is as follows：
(1) the raw material tertiary amine of the reversible solvent salting liquid of synthesis hydrophilic and water volume ratio are 1:1-10；(2) hydrophily is reversible molten
Agent salting liquid adds the 1-5L/kg that volume is with oil-sand mass ratio；Organic solvent volume is 1-12 times of L/kg with oil-sand mass ratio；
(3) leaching organic solvent and the reversible solvent salting liquid of hydrophily are simultaneously into extraction equipment, for oil-sand extraction and separation, drip
It is carried out at ranging from 15-60 DEG C of green separation temperature；(4) product discharge and reagent recycling organic solvent are received at 70-200 DEG C through distillation
Collection, distillation residual organic substances are asphaltic products；(5) the residual sand after oil-sand separation and the reversible solvent salting liquid room temperature warp of hydrophily
A small amount of washing, residual sand product reach clean discharging；(6) the reversible solvent salting liquid recovered temperature of hydrophily after use is 40-100
DEG C, amine and water after recycling can be recycled.
The present invention provides a set of closing realized substantially also according to the addition of reversible tertiary amine auxiliary additive and recycling feature
The equipment and process matched therewith of cycle, are described as follows：
The core apparatus of oil-sand solvent extraction and separation is the level-one extraction kettle 27 and two level with mechanical agitator of sealing
Extraction kettle 31.The reversible solvent salting liquid of hydrophily synthesizes in reaction kettle I 26.Level-one extraction kettle 27 plays main extraction and separation and makees
It is to continue to extract remaining pitch in treated the residual sand of level-one extraction kettle 27 with, two level extraction kettle 30；From two
The residual sand separated in grade extraction tank 30, because containing a small amount of ammonium salt solution, it is impossible to direct emission, in the present invention using washing
Kettle 32 discharges again after being washed to it.Stand what slot 29,31 came out from what level-one extraction kettle 27 and two level extraction kettle 30 connected
Liquid phase is sent to refined unit；The reacted kettle II 33 of the reversible solvent salting liquid of hydrophily isolated from two level standing slot 31 generates amine
And water, it is recycled, reduces environmental pollution, saved solvent materials, improve comprehensive utilization of energy rate.
The concrete operation step of process implementing：
(1) the synthesis of the reversible solvent salting liquid of hydrophily：Amine 1 is with water 2 respectively from amine recycling can 24 and water recovery tank 25 with same
The flow of sample is passed through with mechanical agitator reaction kettle I 26, is stirred, and 3 autoreaction kettle middle and lower part of carbon dioxide is passed through, with kettle
Middle liquid phase is contacted and is reacted, and unreacted carbon dioxide is discharged from kettle top exhaust pipe, stops reaction after the 1h that ventilates, will be synthetic
The reversible solvent salting liquid 4 of hydrophily be passed through level-one extraction kettle 27；
(2) hybrid extraction：Oil-sand/oil shale mine 6 from mining area is sent into level-one extraction kettle 27 and a certain proportion of parent in kettle
Aqueous reversible solvent salting liquid 4 and cycle solvent (extraction organic solvent) 5 at 25-100 DEG C carry out that extraction 2- is mixed
After 60min, organic solvent/ammonium salt solution/sand grains mixed serum I 7 is sent into level-one standing slot 29 and is stood, it is solid so as to reach
Liquid detaches purpose；
(3) separation of solid and liquid：Level-one stands coagulation ammonium salt solution+grains of sand 8 that 29 bottom of slot comes out and is delivered to two level extraction
In kettle 30, the cycle solvent of the quality such as 1-3 times of solid is added at 25-100 DEG C, carries out washing extraction 2-60min, and extraction has
Solvent/ammonium salt solution/sand grains mixed serum II 11 is also fed into two level and stands slot 31；
(4) solvent/pitch oil mixture separation：Liquid phase solvent/the coal tar isolated in two-stage defecator 30,31 is mixed
It closes object 9,12 and is delivered to the progress of refinery unit 35 solvent/coal tar separation and pitch oil refinement, detach and obtain from refinery unit 35
The recycling design 23 obtained is delivered to cycle solvent tank 28 and is recycled；21 refined unit 35 of solvent/pitch oil mixture
Product 22 after being refined afterwards；
(5) the grains of sand of 31 bottom of two level standing slot+a small amount of ammonium salt solution 13 is delivered in washing kettle 32 and is washed, and washes
Residual sand 16 afterwards is discharged by bottom；
(6) the recycling of ammonium salt and water：Two level is stood in the ammonium salt solution 14 and washing kettle 32 that 31 middle part of slot is separated
Ammonium salt weak solution 17 is passed through reaction kettle II 33, and air 18 is passed through by kettle middle and lower part through pump and is contacted with reaction solution in kettle, reaction kettle folder
It is passed through in set and is steam heated to 40-100 DEG C, the recycling amine 19 and recycle-water 20 after reaction each lead into amine recycling can 24 and water returns
Closed cans 25, unreacted air are discharged from kettle top.
This method uses additive recycling method, reduces environmental pollution；Using multistage (1-2 grades) extractions, cooperation
Using mechanical settling tank, it is continuous to ensure that production is able to, improves extraction efficiency and yield, also saves solvent；It will extract
The solid particle generated in journey is divided into two parts and is handled, and improves treatment effect, reduces environmental pollution, takes full advantage of
The energy；The microparticle being suspended in using the removing of suspension isolation technics in extract liquor, reduces operational load；It is handled using WATER-WASHING METHOD
Microparticle can reduce discharge pressure with effective use of energy sources.
In the following, being illustrated to the present invention with following embodiment, but it is not limited to following embodiment.
Embodiment 1：
Several reversible tertiary amine secondary solvent extraction oil sands bitumen methods of different hydrophilic.
Three kinds of reversible solvents of hydrophily are respectively adopted：Triethylamine, N, N- dimethyl cyclohexyl amines, N, N- dimethyl benzylamines, N-
Ethyl piperidine.Toluene is extractant.
The reversible tertiary amine of 5L hydrophilies is passed through from amine recycling can 24 and water recovery tank 25 in reaction kettle I 26 respectively with 5L water, is beaten
Reaction kettle mechanical agitation is opened, rotating speed 300rpm opens carbon dioxide valve, carbon dioxide is passed through from reaction kettle middle and lower part,
Gas velocity is 5L/min, closes carbon dioxide gas valve after ventilatory response 1h, stops stirring, reaction solution is passed through level-one extraction kettle
27.Oil-sand 5kg is sent into level-one extraction kettle 27 and is mixed with tertiary amine salting liquid and 15L toluene, at 25 DEG C, carries out mixing extraction
25min reduces mixing speed, is mutually sent into upper strata organic solvent after level-one stands 29 solid-liquor separation of slot and is mutually sent to solvent/drip
Green oil tank 34 is stored, while level-one is stood the residual sand of bottom and tertiary amine salting liquid in 29 slots and is sent into two level extraction kettle 30
In, the cycle solvent of the quality such as 3 times of solids is added at 25 DEG C, carries out washing extraction 25min, slot is stood subsequently into two level
31, organic solvent is mutually sent to solvent/pitch oil tank 34 and is stored, and tertiary amine salting liquid is sent into reaction kettle II 33, and two level is stood
The residual sand in 31 bottom of slot is sent into washing kettle 32, while 5L water is added in into kettle, and stirring washing 10min stands 20min, bottom after washing
The residual sand in portion is discharged by discharge port, and upper aqueous phase is sent to reaction kettle II 33.Tertiary amine salting liquid is passed through at 70 DEG C in reaction kettle II 33
Air, gas velocity 5L/min, ventilate 1h after stand 20min, upper organic phase is sent to reversible solvent recovery tank 1, and lower floor's water phase is sent
To water (or alcohol) recycling can 2.Solvent/pitch the oil mixture 21 for being stored in solvent/pitch oil tank 34 is sent to refining through oil pipeline
Factory's refined unit 35.
The reversible tertiary amine assisting oil-sand extraction bitumen recovery rate of 1 several different hydrophilics of table
Embodiment 2：
Several reversible secondary amine secondary solvent extraction oil sands bitumen methods of different hydrophilic.
Three kinds of reversible solvents of hydrophily are respectively adopted：Di-n-propylamine, 3- sec-butylamine guanidine-acetic acids propyl ester, N- propyl sec-butylamine,
Di-sec-butyl amine.Toluene is extractant.
The reversible secondary amine of 5L hydrophilies is passed through from amine recycling can 24 and water recovery tank 25 in reaction kettle I 26 respectively with 5L water, is beaten
Reaction kettle mechanical agitation is opened, rotating speed 300rpm opens carbon dioxide valve, carbon dioxide is passed through from reaction kettle middle and lower part,
Gas velocity is 5L/min, closes carbon dioxide gas valve after ventilatory response 1h, stops stirring, reaction solution is passed through level-one extraction kettle
27.Oil-sand 5kg is sent into level-one extraction kettle 27 and is mixed with tertiary amine salting liquid and 15L toluene, at 25 DEG C, carries out mixing extraction
25min reduces mixing speed, is mutually sent into upper strata organic solvent after level-one stands 29 solid-liquor separation of slot and is mutually sent to solvent/drip
Green oil tank 34 is stored, while level-one is stood the residual sand of bottom and tertiary amine salting liquid in 29 slots and is sent into two level extraction kettle 30
In, the cycle solvent of the quality such as 3 times of solids is added at 25 DEG C, carries out washing extraction 25min, slot is stood subsequently into two level
31, organic solvent is mutually sent to solvent/pitch oil tank 34 and is stored, and tertiary amine salting liquid is sent into reaction kettle II 33, and two level is stood
The residual sand in 31 bottom of slot is sent into washing kettle 32, while 5L water is added in into kettle, and stirring washing 10min stands 20min, bottom after washing
The residual sand in portion is discharged by discharge port, and upper aqueous phase is sent to reaction kettle II 33.Tertiary amine salting liquid is passed through at 70 DEG C in reaction kettle II 33
Air, gas velocity 5L/min, ventilate 1h after stand 20min, upper organic phase is sent to reversible solvent recovery tank 1, and lower floor's water phase is sent
To water (or alcohol) recycling can 2.Solvent/pitch the oil mixture 21 for being stored in solvent/pitch oil tank 34 is sent to refining through oil pipeline
Factory's refined unit 35.
The reversible secondary amine assisting oil-sand extraction bitumen recovery rate of 2 several different hydrophilics of table
Embodiment 3：
The reversible tertiary amine assisting oil-sand separation method of hydrophily of several different organic solvents.
Six kinds of organic solvents are respectively adopted to be extracted, single organic solvent is using toluene, dimethylbenzene；Double solvents uses
Toluene and normal heptane volume ratio 1:3；Acetone and normal heptane volume ratio 1：3；Ethyl acetate and normal heptane volume ratio 1:3 solvent.
5L triethylamines are passed through from amine recycling can 24 and water recovery tank 25 in reaction kettle I 26 respectively with 5L water, open reaction kettle
Mechanical agitation, rotating speed 300rpm open carbon dioxide valve, carbon dioxide, gas velocity 5L/ are passed through from reaction kettle middle and lower part
Carbon dioxide gas valve is closed after min, ventilatory response 1h, stops stirring, reaction solution is passed through level-one extraction kettle 27.Oil-sand 5kg
It is sent into level-one extraction kettle 27 to mix with tertiary amine salting liquid and 15L solvents, at 25 DEG C, carries out that extraction 25min is mixed, reduce
Upper strata organic solvent after level-one stands 29 solid-liquor separation of slot is mutually sent into and is mutually sent to solvent/pitch oil tank 34 by mixing speed
It is stored, while level-one is stood into the residual sand of bottom and tertiary amine salting liquid in 29 slots and is sent into two level extraction kettle 30, add in 3 times
The cycle solvent of the quality such as solid carries out washing extraction 25min, slot 31, organic solvent is stood subsequently into two level at 25 DEG C
It is mutually sent to solvent/pitch oil tank 34 to be stored, tertiary amine salting liquid is sent into reaction kettle II 33, and two level stands the residual sand in 31 bottom of slot
Washing kettle 32 is sent into, while 5L water is added in into kettle, stirring washing 10min stands 20min, the residual sand in bottom is by discharging after washing
Mouth discharge, upper aqueous phase are sent to reaction kettle II 33.Tertiary amine salting liquid is passed through air at 70 DEG C in reaction kettle II 33, and gas velocity is
20min is stood after 5L/min, the 1h that ventilates, upper organic phase is sent to tertiary amine recycling can 1, and lower floor's water phase is sent to water recovery tank 2.It is stored in
The solvent of solvent/pitch oil tank 34/pitch oil mixture 21 is sent to refinery's refined unit 35 through oil pipeline.
The reversible tertiary amine assisting oil-sand extraction bitumen recovery rate of hydrophily of 3 several different organic solvents of table
Embodiment 4：
Several reversible tertiary amine dosage assisting oil-sand separation methods of different hydrophilic.
Organic solvent uses ethyl acetate：Normal heptane=1:3, the reversible tertiary amine dosage of hydrophily and oil-sand ratio (V/W) are divided
It Wei 1：2、1:1、2:1、3:1、4:1.
5L triethylamines are passed through from amine recycling can 24 and water recovery tank 25 in reaction kettle I 26 respectively with 5L water, open reaction kettle
Mechanical agitation, rotating speed 300rpm open carbon dioxide valve, carbon dioxide, gas velocity 5L/ are passed through from reaction kettle middle and lower part
Carbon dioxide gas valve is closed after min, ventilatory response 1h, stops stirring, reaction solution is passed through level-one extraction kettle 27.Oil-sand 5kg
It is sent into level-one extraction kettle 27 to mix with the tertiary amine salting liquid and 15L solvents of certain volume, at 25 DEG C, carries out mixing extraction
25min reduces mixing speed, is mutually sent into upper strata organic solvent after level-one stands 29 solid-liquor separation of slot and is mutually sent to solvent/drip
Green oil tank 34 is stored, while level-one is stood the residual sand of bottom and tertiary amine salting liquid in 29 slots and is sent into two level extraction kettle 30
In, the cycle solvent of the quality such as 3 times of solids is added at 25 DEG C, carries out washing extraction 25min, slot is stood subsequently into two level
31, organic solvent is mutually sent to solvent/pitch oil tank 34 and is stored, and tertiary amine salting liquid is sent into reaction kettle II 33, and two level is stood
The residual sand in 31 bottom of slot is sent into washing kettle 32, while 5L water is added in into kettle, and stirring washing 10min stands 20min, bottom after washing
The residual sand in portion is discharged by discharge port, and upper aqueous phase is sent to reaction kettle II 33.Tertiary amine salting liquid is passed through at 70 DEG C in reaction kettle II 33
Air, gas velocity 5L/min, ventilate 1h after stand 20min, upper organic phase is sent to tertiary amine recycling can 1, and lower floor's water phase is sent to water
Recycling can 2.Solvent/pitch the oil mixture 21 for being stored in solvent/pitch oil tank 34 is sent to refinery's refined unit through oil pipeline
35。
The reversible tertiary amine dosage assisting oil-sand extraction bitumen recovery rate of 4 several different hydrophilics of table
Embodiment 5：
The reversible tertiary amine assisting oil-sand separation method of hydrophily of several consumption of organic solvent.
Organic solvent uses ethyl acetate：Normal heptane=1:3, the reversible tertiary amine aqueous solution 5L of hydrophily, consumption of organic solvent
It is respectively 2 with oil-sand ratio (V/W):1、3:1、4:1、5:1、6:1.
5L triethylamines are passed through from amine recycling can 24 and water recovery tank 25 in reaction kettle I 26 respectively with 5L water, open reaction kettle
Mechanical agitation, rotating speed 300rpm open carbon dioxide valve, carbon dioxide, gas velocity 5L/ are passed through from reaction kettle middle and lower part
Carbon dioxide gas valve is closed after min, ventilatory response 1h, stops stirring, reaction solution is passed through level-one extraction kettle 27.Oil-sand 5kg
It is sent into level-one extraction kettle 27 to mix with the solvent of tertiary amine salting liquid and certain volume, at 25 DEG C, carries out mixing extraction
25min reduces mixing speed, is mutually sent into upper strata organic solvent after level-one stands 29 solid-liquor separation of slot and is mutually sent to solvent/drip
Green oil tank 34 is stored, while level-one is stood the residual sand of bottom and tertiary amine salting liquid in 29 slots and is sent into two level extraction kettle 30
In, the cycle solvent of certain volume is added at 25 DEG C, carries out washing extraction 25min, and slot 31 is stood subsequently into two level, it is organic
Solvent is mutually sent to solvent/pitch oil tank 34 and is stored, and tertiary amine salting liquid is sent into reaction kettle II 33, and two level stands 31 bottom of slot
Residual sand is sent into washing kettle 32, while 5L water is added in into kettle, stirring washing 10min, stands 20min after washing, the residual sand in bottom by
Discharge port is discharged, and upper aqueous phase is sent to reaction kettle II 33.Tertiary amine salting liquid is passed through air, gas velocity at 70 DEG C in reaction kettle II 33
For 5L/min, 20min is stood after the 1h that ventilates, upper organic phase is sent to tertiary amine recycling can 1, and lower floor's water phase is sent to water recovery tank 2.It deposits
In solvent/pitch oil mixture 21 of solvent/pitch oil tank 34 refinery's refined unit 35 is sent to through oil pipeline.
The reversible tertiary amine oil-sand extraction bitumen recovery rate of 5 several solvent dosages of table auxiliary hydrophily
Embodiment 6：
The reversible tertiary amine assisting oil-sand separation method of hydrophily of several different temperatures.
Organic solvent uses ethyl acetate：Normal heptane=1:3, the reversible tertiary amine aqueous solution 5L of hydrophily, consumption of organic solvent
15L, temperature are respectively 15 DEG C, 25 DEG C, 35 DEG C, 45 DEG C.
5L triethylamines are passed through from tertiary amine recycling can 24 and water recovery tank 25 in reaction kettle I 26 respectively with 5L water, open reaction
Kettle mechanical agitation, rotating speed 300rpm open carbon dioxide valve, are passed through carbon dioxide from reaction kettle middle and lower part, gas velocity is
Carbon dioxide gas valve is closed after 5L/min, ventilatory response 1h, stops stirring, reaction solution is passed through level-one extraction kettle 27.Oil-sand
5kg is sent into level-one extraction kettle 27 and is mixed with tertiary amine salting liquid and 15L solvents, under certain temperature, carries out mixing extraction
25min reduces mixing speed, is mutually sent into upper strata organic solvent after level-one stands 29 solid-liquor separation of slot and is mutually sent to solvent/drip
Green oil tank 34 is stored, while level-one is stood the residual sand of bottom and tertiary amine salting liquid in 29 slots and is sent into two level extraction kettle 30
In, the cycle solvent of the quality such as 3 times of solids is added under certain temperature, is carried out washing extraction 25min, is stood subsequently into two level
Slot 31, organic solvent are mutually sent to solvent/pitch oil tank 34 and are stored, and tertiary amine salting liquid is sent into reaction kettle II 33, and two level is quiet
It putting the residual sand in 31 bottom of slot and is sent into washing kettle 32, while 5L water is added in into kettle, stirring washing 10min stands 20min after washing,
The residual sand in bottom is discharged by discharge port, and upper aqueous phase is sent to reaction kettle II 33.Tertiary amine salting liquid leads at 70 DEG C in reaction kettle II 33
Enter air, 20min stood after gas velocity 5L/min, the 1h that ventilates, upper organic phase is sent to tertiary amine recycling can 1, lower floor's water phase send to
Water recovery tank 2.Solvent/pitch the oil mixture 21 for being stored in solvent/pitch oil tank 34 is sent to refinery through oil pipeline and refines list
Member 35.
The reversible tertiary amine assisting oil-sand extraction bitumen recovery rate of hydrophily of 6 several temperature of table
Claims (1)
- A kind of 1. method of recyclable organic solvent separation oil-sand, it is characterised in that：Step is as follows：(1) the reversible solvent salting liquid of synthesis hydrophilic；(2) hybrid extraction：Organic solvent and the reversible solvent salting liquid of hydrophily carry out oil-sand extraction point simultaneously into extraction equipment From；The 1-5L/kg that the reversible solvent salting liquid addition volume of hydrophily is with oil-sand mass ratio；Organic solvent volume and oil-sand quality Than for 1-12L/kg；(3) separation of solid and liquid：Mixing solid-liquid after extraction is stood, the upper phase organic solvent isolated/coal tar mixing Object is detached, and solvent recovery uses, pitch oil refinement；(4) the grains of sand+the ammonium salt solution for standing rear lower is washed, the residual sand after washing is discharged by bottom；(5) ammonium salt solution is passed through reaction kettle, is pumped into air and heats 40-100 DEG C simultaneously, recycling amine and recycle-water after reaction, into Row recycles, and completes whole circular response；(6) the recycling of ammonium salt and water：Two level is stood into the ammonium salt weak solution in the ammonium salt solution and washing kettle separated in the middle part of slot Reaction kettle is passed through, air is passed through into reaction kettle, recycling amine and recycle-water after reaction, unreacted air are discharged from kettle top；(4) the step stands the grains of sand+ammonium salt solution progress reextraction of rear lower after, then washed；The reextraction Step is：Lower floor's ammonium salt solution+grains of sand are subjected to two level extraction, add the organic solvent extraction of the quality such as 1-3 times of solid, extraction It is stood after taking；By upper organic phase by the processing of step (3), the grains of sand+ammonium salt solution of lower part is washed again；The organic solvent is the single organic solvent of benzene,toluene,xylene or Reformed Gasoline or is compounded for acetone-alkanes Solvent, ethyl acetate-alkanes complex solvent；In the reversible solvent of hydrophily tertiary amines for triethylamine, N, N- dimethyl cyclohexyl amines, N, N- dimethyl benzylamines, N, N- bis- Methylbutylamine, N-ethylpiperidine, N- methyl-di-n-propylamines, N- butyl pyrrolidines, N, N- diethyl butylamine, N, N- dimethylhexylamines, Penta amidine of N, N- phenpromethamine, N, N, N '-triethyl group, the own amidine of N, N, N '-tributyl, diisopropyl ethanolamine, 4,4- diethyls Oxygroup-N, N- dimethyl butylamine, 4- diethylin ethyl butyrate, 5- dipropyls amido -2 pentanone, dibutylamino ethyl alcohol；Secondary amine class For di-n-propylamine, 3- sec-butylamine guanidine-acetic acids propyl ester, 3- isopropylamine bases propyl butyrate, 3- sec-butylamine bases propyl propionate, N- propyl Zhong Ding Base amine, di-sec-butyl amine.
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| CN107596733A (en) * | 2017-09-11 | 2018-01-19 | 扬州大学 | A kind of method for carrying out extract and separate to the blend of organic matter and water using triethylamine |
| CN107760353B (en) * | 2017-11-14 | 2020-05-26 | 天津大学 | Method for oil-solid separation by adopting reversible extraction solvent |
| CN108862953B (en) * | 2018-06-29 | 2021-05-28 | 西南石油大学 | Method for treating oily waste by adopting acid-base switch mixed solvent system |
| CN108862954B (en) * | 2018-06-29 | 2021-05-28 | 西南石油大学 | Method for treating oily waste by adopting switch type mixed solvent system |
| CN111203006B (en) * | 2020-01-21 | 2022-08-02 | 西南石油大学 | Separation agent for emulsifying oily wastewater, preparation method and separation method |
| CN113332751A (en) * | 2021-06-25 | 2021-09-03 | 太原理工大学 | Process for using dipropylamine as reversible extraction solvent |
| CN114891533B (en) * | 2022-05-20 | 2023-06-02 | 成都理工大学 | CO (carbon monoxide) 2 Method for oil phase separation or oil-containing solid waste cleaning in response to single-cycle ionic liquid system |
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