CN103664480A - Method for refining petrobenzene and thiophene by using ionic liquid complex solvent - Google Patents
Method for refining petrobenzene and thiophene by using ionic liquid complex solvent Download PDFInfo
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Abstract
The invention creates and provides a method for refining petrobenzene and thiophene by using an ionic liquid complex solvent. Coking crude benzene is pretreated to form crude benzene in a pretreatment procedure, crude benzene is extracted and rectified twice in the ionic liquid complex solvent during a benzene refining procedure to form a 99.99% benzene product and crude thiophene, a thiophene product with purity of more than 99.7% is also obtained by extracting and rectifying crude thiophene twice with the ionic liquid complex solvent in the thiophene refining procedure, yield is more than 97%, and all the ionic liquid complex solvent is recycled after being refined and recycled through a recovery tower. In the method, the quality of the benzene product reaches A-level standard of petrobenzene national standard, the benzene product can substitute petrobenzene in use, meanwhile, thiophene is recycled efficiently, and the economic benefit increased therefrom is more than 50%; the ionic liquid has good thermal stability, low vapor pressure and high polarity, the complex solvent formed by the ionic liquid has high selectivity, relative volatility among the constituents is increased, dosage of an extraction agent is reduced, and process energy consumption and production cost are respectively reduced by 25% and 40%, so that energy-saving effect is remarkable.
Description
Technical field
The invention relates to coked crude benzene refining technical field, relates in particular to a kind of method that adopts ionic liquid composite solvent turpentole benzene and thiophene.
Background technology
Benzene is important Organic Chemicals, and industrial use is very extensive, and its main source is the crude benzol that coking and steel industry produce.Along with the raising of chemical industry to benzene purity requirement, high-purity sulfurless benzene that refining depth purifies is more and more important.The composition of crude benzol is very complicated, and the existence of sulfide thiophene has a strong impact on the refining effect of benzene.Thiophene is the important synthesis material of fine chemicals, is mainly used in the production of medicine, dyestuff, makeup etc.Because existing crude benzene refining technology cannot reclaim thiophene, can only rely on external import, cause price very expensive.So say in a sense, the degree that thiophene reclaims is to weigh the important factor of crude benzene refining process economy.
Although acid wash crude benzene refining technology technique is simple, operational condition is gentle, applied widely, but destroyed the thiophene with high industrial value, acid cleaning process has produced acid tar and the waste residue that cannot process in a large number simultaneously, serious environment pollution, and country has prohibited this technology of using; Shortening method complex process, facility investment are large, severe reaction conditions, and portioned product is caused yield low by hydrogenation, cannot reclaim valuable thiophene resource, and the high request of catalyst performance has also been limited to the industrial application of this method.In recent years, in industry, developed and take extracting rectifying as basic crude benzene refining technology, aspect production technique, done a large amount of improvements, improved the purity of benzene, but the organic efficiency of thiophene has been not high.Ru Luo state China wait that people (CN1552682A) take that coking-light benzene or coking-light benzene distillation cutting obtain containing benzene-toluene fraction or containing thiophene benzene-toluene fraction, be raw material, adopt two-stage extracting rectifying to reclaim thiophene, have to the thiophene enriched material of content 20%.
Summary of the invention
In order to improve the deficiency of existing Technology, the quality that improves benzene makes it to reach the standard of petroleum benzene, the thiophene resource of efficient recovery high added value, the invention provides a kind of ionic liquid composite solvent that adopts by the method for coked crude benzene refining petroleum benzene and thiophene simultaneously.The method can obtain high pure benzene and high-purity thiophene simultaneously, and technical process is simple, and energy consumption and production cost are low, without useless solid discharging of waste liquid, free from environmental pollution, is a kind of method of commercial benzene and thiophene of economic environmental protection.
For solving the problems of the technologies described above, the technical scheme that the invention adopts is: the method that adopts ionic liquid composite solvent turpentole benzene and thiophene, adopt ionic liquid composite solvent as extraction agent, the coking crude benzene organic mixture that comprises benzene is carried out to separation, and concrete technology comprises rectifying pre-treatment, benzene refining, refining three operations of thiophene.
Described double solvents is ionic liquid-ionic liquid composite solvent or ionic liquid-organic solvent double solvents; Wherein ionic liquid is that positively charged ion is the non-AlCl of imidazol ion
3type ionic liquid; Organic solvent is one or more the mixture in ethylene glycol, tetramethylene sulfone, glycols, methyl-sulphoxide, monoethanolamine, gamma-butyrolactone, alpha-pyrrolidone, N-N-formyl morpholine N-, N-Methyl pyrrolidone, DMF.
Preferably, described double solvents is that ionic liquid 1-butyl-3-methyl imidazolium a tetrafluoro borate and organic solvent ethylene glycol are according to mass ratio 1:(1-5) mix or ionic liquid 1-butyl-3-methyl imidazolium a tetrafluoro borate and 1-ethyl-3-methylimidazole acetate according to mass ratio 1:(1-3) mix.
The described coking crude benzene that comprises benzene also comprises the sulfide of alkane, naphthenic hydrocarbon, alkene, cycloolefin, aromatic hydrocarbons and thiophene.
Described rectifying pretreatment process comprises lightness-removing column and weight-removing column, coking crude benzene enter lightness-removing column by conventional distillation take off light after, overhead extraction boiling point is lower than the light constituent of benzene, tower reactor material enters weight-removing column and takes off heavy rear tower reactor extraction boiling point higher than the heavy constituent of benzene by conventional distillation, tower top obtains crude benzol, enters benzene refining operation.
Preferably, the working pressure of described lightness-removing column is 50-101kPa, and tower top temperature is 50-80 ℃, and tower reactor temperature is 90-110 ℃; The working pressure of described weight-removing column is 50-101kPa, and tower top temperature is 55-85 ℃, and tower reactor temperature is 95-120 ℃.
Described benzene refining operation comprises extraction lightness-removing column one, extraction weight-removing column one and regenerator column one, first the middle and lower part charging from extraction lightness-removing column one by the crude benzol obtaining after rectifying pretreatment process, ionic liquid composite solvent is from the middle and upper part charging of extraction lightness-removing column one, residual light constituent in overhead extraction crude benzol, tower reactor material enters extraction weight-removing column one by the middle and lower part that extracts weight-removing column one; Ionic liquid composite solvent, from the middle and upper part charging of extraction weight-removing column one, obtains benzaldehyde product by tower top, and tower reactor material enters regenerator column one; Ionic liquid composite solvent after regeneration is by the tower reactor extraction of regenerator column one and return to extraction lightness-removing column one and extraction weight-removing column one recycles, and the tower top of regenerator column one obtains thick thiophene, enters thiophene refining step.
Preferably, the solvent ratio in described extraction lightness-removing column one is (1-10): 1, and reflux ratio: (2-5): 1, working pressure is 50-101kPa, and tower top temperature is 50-75 ℃, and tower reactor temperature is 90-120 ℃; Solvent ratio in described extraction weight-removing column one is (1-10): 1, and reflux ratio: (2-5): 1, working pressure is 50-101kPa, tower top temperature is 55-80 ℃, tower reactor temperature 95-125 ℃; The working pressure of described regenerator column one is 20-101kPa.
Described thiophene refining step comprises extraction lightness-removing column two, extraction weight-removing column two and regenerator column two, first the middle and lower part charging from extraction lightness-removing column two by the thick thiophene obtaining after benzene refining operation, ionic liquid composite solvent is from the middle and upper part charging of extraction lightness-removing column two, residual benzene and other light constituents in the thick thiophene of overhead extraction, tower reactor material enters extraction weight-removing column two by the middle and lower part that extracts weight-removing column two; Ionic liquid composite solvent, from the middle and upper part charging of extraction weight-removing column two, obtains thiophene product by tower top, and tower reactor material enters regenerator column two; Ionic liquid composite solvent after regeneration is by the tower reactor extraction of regenerator column two and return to extraction lightness-removing column two and extraction weight-removing column two recycles, and the tower top of regenerator column two obtains residual heavy constituent.
Preferably, the solvent ratio (1-10) in described extraction lightness-removing column two: 1, reflux ratio: (2-5): 1, working pressure 50-101kPa, tower top temperature 60-75 ℃, tower reactor temperature 95-130 ℃; Solvent ratio (1-10) in described extraction weight-removing column two: 1, reflux ratio: (2-5): 1, working pressure 50-101kPa, tower top temperature 65-85 ℃, tower reactor temperature 105-150 ℃; The working pressure of described regenerator column two is 20-101kPa.
The advantage that the invention has with positively effect is: (1) is compared with existing extraction rectification technique, the selectivity of ionic liquid composite solvent of the present invention is high, strengthened the relative volatility between component, Solvent quantity is reduced, the energy consumption of technique and production cost have declined respectively 25% and 40%, energy-saving effect highly significant.In addition, ionic liquid thermostability is high, vapour pressure is extremely low, and lossless in use procedure, nontoxic, non-corrosiveness have increased the security of production process;
(2) compare with acid wash, the inventive method effectively reduces the loss of benzene in treating process, and the rate of recovery of benzene has improved more than 5%, and whole technological process does not produce useless solid waste liquid, non-environmental-pollution problem;
(3) compare with shortening method, the technical process of the inventive method is simple, and cost of equipment and running cost are low, and cost of equipment is less than 1/2 of catalytic hydrogenation process, and running cost is only the 1/2-1/3 of catalytic hydrogenation process;
(4) the present invention has obtained 99.99% benzaldehyde product, the indexs such as its look number, bromine valency, ctystallizing point, sulphur nitrogen impurity content all reach petroleum benzene GB primary standard, can replace petroleum benzene to use, simultaneously high efficiente callback thiophene, its purity is greater than 99.7%, the rate of recovery is greater than 97%, compares with existing Technology, and the economic benefit that the present invention increases thus reaches more than 50%.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the disclosed method of the present invention
Embodiment
The coking crude benzene that comprises benzene in the present invention also comprises the sulfide of alkane, naphthenic hydrocarbon, alkene, cycloolefin, aromatic hydrocarbons and thiophene etc.The ionic liquid composite solvent adopting can be the double solvents of ionic liquid and ionic liquid, can be also the double solvents of ionic liquid and organic solvent, and ionic liquid wherein can be that positively charged ion is the non-AlCl of imidazol ion
3type ionic liquid, preferably 1-ethyl-3-methylimidazole acetate, 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-ethyl-3-methylimidazole dimethyl phosphate salt, 1-octyl group-3-Methylimidazole three fluoro sulfonates; Organic solvent can be one or more the mixture in ethylene glycol, tetramethylene sulfone, glycols, methyl-sulphoxide, monoethanolamine, gamma-butyrolactone, alpha-pyrrolidone, N-N-formyl morpholine N-, N-Methyl pyrrolidone, DMF.About choosing of ionic liquid and organic solvent, be mainly to take on the impact of relative volatility between difficult separated portion, selectivity to be index, also should to consider the thermostability of selected species, security etc.
By following examples, the present invention is described in detail, although provided embodiment, also should be included under the condition that does not depart from the technology of the present invention scope, to those skilled in the art apparent various change.
Embodiment 1
Press technical process shown in accompanying drawing 1, the coking crude benzene that certain coking plant produces of take is raw material, consists of: benzene 64.8%(mass content, as follows), thiophene 5.2%, all the other are weight component.
Pretreatment process:
(1) first coking crude benzene removes light constituent at lightness-removing column, the working pressure of lightness-removing column is 101kPa, 80 ℃ of tower top temperatures, 100 ℃ of tower reactor temperature, overhead extraction boiling point is lower than the light constituent of benzene, be mainly the unsaturated hydrocarbons such as H2S, CS2, amylene, ethylene methacrylic, pentamethylene, hexene, hexane, methylcyclopentane, tower reactor material enters weight-removing column;
(2) from the material of lightness-removing column tower reactor, enter weight-removing column and remove heavy constituent, weight-removing column working pressure 50kPa, 55 ℃ of tower top temperatures, 95 ℃ of tower reactor temperature, tower reactor extraction boiling point, higher than the heavy constituent of benzene, is mainly toluene, ethylbenzene, dimethylbenzene, vinylbenzene etc., and tower top obtains crude benzol, consist of: benzene 89.4%, thiophene 7.1%, light constituent 2.2%, heavy constituent 1.3%, enter benzene refining operation.
Benzene refining operation:
(1) crude benzol and ionic liquid composite solvent are respectively from extracting middle and lower part, the middle and upper part charging of lightness-removing column one, ionic liquid composite solvent is the double solvents that 1-butyl-3-methyl imidazolium tetrafluoroborate and 1-ethyl-3-methylimidazole acetate form with mass ratio 1:1, solvent ratio 8:1, reflux ratio 2:1, working pressure 101kPa, 75 ℃ of tower top temperatures, 120 ℃ of tower reactor temperature, remaining light constituent in overhead extraction crude benzol, tower reactor material enters extraction weight-removing column one;
(2) the tower reactor material from extraction lightness-removing column one enters extraction weight-removing column one middle and lower part, ionic liquid composite solvent used (identical with the double solvents in lightness-removing column one), from this tower middle and upper part, come in to expect, solvent ratio 8:1, reflux ratio 2:1, working pressure 101kPa, 80 ℃ of tower top temperatures, 125 ℃ of tower reactor temperature, tower top obtains 99.99% benzaldehyde product, the indexs such as its look number, bromine valency, ctystallizing point, sulphur nitrogen impurity content all reach petroleum benzene GB primary standard, can replace petroleum benzene to use, and tower reactor material enters recovery tower one;
(3) refine and reclaim ionic liquid composite solvent in recovery tower one, working pressure is 20kPa, ionic liquid composite solvent after recovery returns to extraction lightness-removing column one by flow metering and extraction weight-removing column one recycles, tower top obtains thick thiophene, consist of: benzene and other light constituents 1%, thiophene 83.8%, heavy constituent 15.2%, enter thiophene refining step.
Thiophene refining step:
(1) thick thiophene and ionic liquid composite solvent are respectively from extracting middle and lower part, the middle and upper part charging of lightness-removing column two, ionic liquid composite solvent is identical with the catalyzer adopting in benzene refining operation, solvent ratio 8:1, reflux ratio 2:1, working pressure 101kPa, 75 ℃ of tower top temperatures, 130 ℃ of tower reactor temperature, benzene and other light constituents of remnants in the thick thiophene of overhead extraction, tower reactor material enters extraction weight-removing column two;
(2) the tower reactor material from extraction lightness-removing column two enters extraction weight-removing column two middle and lower parts, ionic liquid composite solvent (identical with the catalyzer adopting in benzene refining operation) comes in from this tower middle and upper part to expect, solvent ratio 8:1, reflux ratio 2:1, working pressure 50kPa, 65 ℃ of tower top temperatures, 105 ℃ of tower reactor temperature, tower top obtains 99.9% thiophene product, the rate of recovery 98%, and tower reactor material enters recovery tower two;
(3) refine and reclaim ionic liquid composite solvent in recovery tower two, working pressure 20kPa, the ionic liquid composite solvent after recovery returns to extraction lightness-removing column two by flow metering and extraction weight-removing column two recycles.
Embodiment 2
Press technical process shown in accompanying drawing 1, raw material is with embodiment 1.
Pretreatment process:
(1) first coking crude benzene removes light constituent at lightness-removing column, lightness-removing column working pressure 50kPa, 50 ℃ of tower top temperatures, 90 ℃ of tower reactor temperature, overhead extraction boiling point is lower than the light constituent of benzene, be mainly the unsaturated hydrocarbons such as H2S, CS2, amylene, ethylene methacrylic, pentamethylene, hexene, hexane, methylcyclopentane, tower reactor material enters weight-removing column;
(2) from the material of lightness-removing column tower reactor, enter weight-removing column and remove heavy constituent, weight-removing column working pressure 101kPa, 85 ℃ of tower top temperatures, 105 ℃ of tower reactor temperature, tower reactor extraction boiling point is higher than the heavy constituent of benzene, be mainly toluene, ethylbenzene, dimethylbenzene, vinylbenzene etc., tower top obtains crude benzol, consists of: benzene 89.4%, thiophene 7.2%, light constituent 2.3%, heavy constituent 1.1%, enters benzene refining operation.
Benzene refining operation:
(1) crude benzol and ionic liquid composite solvent are respectively from extracting middle and lower part, the middle and upper part charging of lightness-removing column one, ionic liquid composite solvent is the double solvents that 1-butyl-3-methyl imidazolium tetrafluoroborate and 1-ethyl-3-methylimidazole acetate form with mass ratio 1:3, solvent ratio 10:1, reflux ratio 5:1, working pressure 50kPa, 50 ℃ of tower top temperatures, 90 ℃ of tower reactor temperature, remaining light constituent in overhead extraction crude benzol, tower reactor material enters extraction weight-removing column one;
(2) from tower reactor material and the ionic liquid composite solvent of extraction lightness-removing column one (with extraction lightness-removing column one identical) respectively from extracting weight-removing column one middle and lower part, middle and upper part charging, solvent ratio 10:1, reflux ratio 5:1, working pressure 50kPa, 55 ℃ of tower top temperatures, 95 ℃ of tower reactor temperature, tower top obtains 99.99% benzaldehyde product, the indexs such as its look number, bromine valency, ctystallizing point, sulphur nitrogen impurity content all reach petroleum benzene GB primary standard, can replace petroleum benzene to use, tower reactor material enters recovery tower one;
(3) refine and reclaim ionic liquid composite solvent in recovery tower one, working pressure is 101kPa, ionic liquid composite solvent after recovery returns to extraction lightness-removing column one by flow metering and extraction weight-removing column one recycles, tower top obtains thick thiophene, consist of: benzene and other light constituents 1.2%, thiophene 85.6%, heavy constituent 13.2%, enter thiophene refining step.
Thiophene refining step:
(1) thick thiophene with ionic liquid composite solvent (identical with benzene refining operation ionic liquid composite solvent used) respectively from extracting middle and lower part, the middle and upper part charging of lightness-removing column two, solvent ratio 10:1, reflux ratio 5:1, working pressure 50kPa, 60 ℃ of tower top temperatures, 95 ℃ of tower reactor temperature, benzene and other light constituents of remnants in the thick thiophene of overhead extraction, tower reactor material enters extraction weight-removing column two;
(2) from tower reactor material and the ionic liquid composite solvent (identical with benzene refining operation ionic liquid composite solvent used) of extraction lightness-removing column two respectively from extracting weight-removing column two middle and lower parts, middle and upper part charging, solvent ratio 10:1, reflux ratio 5:1, working pressure 101kPa, 85 ℃ of tower top temperatures, 150 ℃ of tower reactor temperature, tower top obtains 99.9% thiophene product, the rate of recovery 99%, tower reactor material enters recovery tower two;
(3) refine and reclaim ionic liquid composite solvent in recovery tower two, working pressure 101kPa, the ionic liquid composite solvent after recovery returns to extraction lightness-removing column two by flow metering and extraction weight-removing column two recycles.
Embodiment 3
Raw material and operation steps are with embodiment 1, ionic liquid composite solvent is the double solvents that 1-octyl group-3-Methylimidazole three fluoro sulfonates and N-N-formyl morpholine N-form with mass ratio 3:1, solvent ratio 1:1, obtain 99.99% benzaldehyde product, the indexs such as its look number, bromine valency, ctystallizing point, sulphur nitrogen impurity content all reach petroleum benzene GB primary standard, can replace petroleum benzene to use.Thiophene refining step obtains 99.8% thiophene product, and the rate of recovery is 97%.
Embodiment 4
Raw material and operation steps are with embodiment 2, ionic liquid composite solvent is the double solvents that 1-butyl-3-methyl imidazolium tetrafluoroborate and organic solvent ethylene glycol form with mass ratio 1:1, solvent ratio is 2:1, obtain 99.99% benzaldehyde product, the indexs such as its look number, bromine valency, ctystallizing point, sulphur nitrogen impurity content all reach petroleum benzene GB primary standard, can replace petroleum benzene to use.Thiophene refining step obtains 99.7% thiophene product, and the rate of recovery is 98%.
Embodiment 5
Raw material and operation steps are with embodiment 2, ionic liquid composite solvent is the double solvents that 1-butyl-3-methyl imidazolium tetrafluoroborate and organic solvent ethylene glycol form with mass ratio 1:5, solvent ratio is 7:1, obtain 99.99% benzaldehyde product, the indexs such as its look number, bromine valency, ctystallizing point, sulphur nitrogen impurity content all reach petroleum benzene GB primary standard, can replace petroleum benzene to use.Thiophene refining step obtains 99.9% thiophene product, and the rate of recovery is 97%.
Above the embodiment of the invention is had been described in detail, but described content is only the preferred embodiment of the invention, can not be considered to for limiting practical range of the present invention.All equalization variations of doing according to the invention scope and improvement etc., within all should still belonging to this patent covering scope.
Claims (10)
1. adopt the method for ionic liquid composite solvent turpentole benzene and thiophene, it is characterized in that: adopt ionic liquid composite solvent as extraction agent, the coking crude benzene organic mixture that comprises benzene is carried out to separation, and concrete technology comprises rectifying pre-treatment, benzene refining, refining three operations of thiophene.
2. method according to claim 1, is characterized in that: described double solvents is ionic liquid-ionic liquid composite solvent or ionic liquid-organic solvent double solvents; Wherein ionic liquid is that positively charged ion is the non-AlCl of imidazol ion
3type ionic liquid; Organic solvent is one or more the mixture in ethylene glycol, tetramethylene sulfone, glycols, methyl-sulphoxide, monoethanolamine, gamma-butyrolactone, alpha-pyrrolidone, N-N-formyl morpholine N-, N-Methyl pyrrolidone, DMF.
3. method according to claim 2, is characterized in that: described double solvents is that ionic liquid 1-butyl-3-methyl imidazolium a tetrafluoro borate and organic solvent ethylene glycol are according to mass ratio 1:(1-5) mix or ionic liquid 1-butyl-3-methyl imidazolium a tetrafluoro borate and 1-ethyl-3-methylimidazole acetate according to mass ratio 1:(1-3) mix.
4. method according to claim 1, is characterized in that: the described coking crude benzene that comprises benzene also comprises the sulfide of alkane, naphthenic hydrocarbon, alkene, cycloolefin, aromatic hydrocarbons and thiophene.
5. according to the method described in claim 1-4 any one, it is characterized in that: described rectifying pretreatment process comprises lightness-removing column and weight-removing column, coking crude benzene enter lightness-removing column by conventional distillation take off light after, overhead extraction boiling point is lower than the light constituent of benzene, tower reactor material enters weight-removing column and takes off heavy rear tower reactor extraction boiling point higher than the heavy constituent of benzene by conventional distillation, tower top obtains crude benzol, enters benzene refining operation.
6. method according to claim 5, is characterized in that: the working pressure of described lightness-removing column is 50-101kPa, and tower top temperature is 50-80 ℃, and tower reactor temperature is 90-110 ℃; The working pressure of described weight-removing column is 50-101kPa, and tower top temperature is 55-85 ℃, and tower reactor temperature is 95-120 ℃.
7. according to the method described in claim 1-4 any one, it is characterized in that: described benzene refining operation comprises extraction lightness-removing column one, extraction weight-removing column one and regenerator column one, first the middle and lower part charging from extraction lightness-removing column one by the crude benzol obtaining after rectifying pretreatment process, ionic liquid composite solvent is from the middle and upper part charging of extraction lightness-removing column one, residual light constituent in overhead extraction crude benzol, tower reactor material enters extraction weight-removing column one by the middle and lower part that extracts weight-removing column one; Ionic liquid composite solvent, from the middle and upper part charging of extraction weight-removing column one, obtains benzaldehyde product by tower top, and tower reactor material enters regenerator column one; Ionic liquid composite solvent after regeneration is by the tower reactor extraction of regenerator column one and return to extraction lightness-removing column one and extraction weight-removing column one recycles, and the tower top of regenerator column one obtains thick thiophene, enters thiophene refining step.
8. method according to claim 7, is characterized in that: the solvent ratio in described extraction lightness-removing column one is (1-10): 1, and reflux ratio: (2-5): 1, working pressure is 50-101kPa, and tower top temperature is 50-75 ℃, and tower reactor temperature is 90-120 ℃; Solvent ratio in described extraction weight-removing column one is (1-10): 1, and reflux ratio: (2-5): 1, working pressure is 50-101kPa, tower top temperature is 55-80 ℃, tower reactor temperature 95-125 ℃; The working pressure of described regenerator column one is 20-101kPa.
9. according to the method described in claim 1-4 any one, it is characterized in that: described thiophene refining step comprises extraction lightness-removing column two, extraction weight-removing column two and regenerator column two, first the middle and lower part charging from extraction lightness-removing column two by the thick thiophene obtaining after benzene refining operation, ionic liquid composite solvent is from the middle and upper part charging of extraction lightness-removing column two, residual benzene and other light constituents in the thick thiophene of overhead extraction, tower reactor material enters extraction weight-removing column two by the middle and lower part that extracts weight-removing column two; Ionic liquid composite solvent, from the middle and upper part charging of extraction weight-removing column two, obtains thiophene product by tower top, and tower reactor material enters regenerator column two; Ionic liquid composite solvent after regeneration is by the tower reactor extraction of regenerator column two and return to extraction lightness-removing column two and extraction weight-removing column two recycles, and the tower top of regenerator column two obtains residual heavy constituent.
10. method according to claim 9, is characterized in that: the solvent ratio (1-10) in described extraction lightness-removing column two: 1, and reflux ratio: (2-5): 1, working pressure 50-101kPa, tower top temperature 60-75 ℃, tower reactor temperature 95-130 ℃; Solvent ratio (1-10) in described extraction weight-removing column two: 1, reflux ratio: (2-5): 1, working pressure 50-101kPa, tower top temperature 65-85 ℃, tower reactor temperature 105-150 ℃; The working pressure of described regenerator column two is 20-101kPa.
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| CN104926591A (en) * | 2015-03-30 | 2015-09-23 | 北京化工大学 | Extractive distillation method for separating benzene and thiophene |
| CN105085152A (en) * | 2014-05-05 | 2015-11-25 | 北京华和拓科技开发有限责任公司 | Novel extraction process for aromatic hydrocarbons |
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| CN114057535A (en) * | 2020-08-05 | 2022-02-18 | 中国石油化工股份有限公司 | Composite solvent for extracting, rectifying and separating aromatic hydrocarbon from hydrocarbon mixture and application method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1552682A (en) * | 2003-05-28 | 2004-12-08 | 北京石油化工学院 | Method for preparing purified petroleum benzine and concentrating thiofuran by cruden benzol |
| CN101260314A (en) * | 2008-05-04 | 2008-09-10 | 中国科学院过程工程研究所 | Oil oxidation-extraction desulfurization technique based on ionic liquid composite solvent |
| CN103044385A (en) * | 2013-01-04 | 2013-04-17 | 北京旭阳化工技术研究院有限公司 | Method for extracting thiophene in coking benzene with ionic liquid |
-
2013
- 2013-11-11 CN CN201310558092.0A patent/CN103664480A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1552682A (en) * | 2003-05-28 | 2004-12-08 | 北京石油化工学院 | Method for preparing purified petroleum benzine and concentrating thiofuran by cruden benzol |
| CN101260314A (en) * | 2008-05-04 | 2008-09-10 | 中国科学院过程工程研究所 | Oil oxidation-extraction desulfurization technique based on ionic liquid composite solvent |
| CN103044385A (en) * | 2013-01-04 | 2013-04-17 | 北京旭阳化工技术研究院有限公司 | Method for extracting thiophene in coking benzene with ionic liquid |
Non-Patent Citations (4)
| Title |
|---|
| 周霞萍等: "焦化轻苯回收噻吩及其衍生物的技术进展", 《煤化工》 * |
| 瞿东蕙等: "焦化苯中噻吩脱除与回收的研究进展", 《广州化工》 * |
| 程林生: "粗苯萃取精制新工艺的开发应用", 《山西化工》 * |
| 胡义等: "离子液体在回收模拟粗苯中噻吩的研究", 《化学工程》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105085152A (en) * | 2014-05-05 | 2015-11-25 | 北京华和拓科技开发有限责任公司 | Novel extraction process for aromatic hydrocarbons |
| CN104926591A (en) * | 2015-03-30 | 2015-09-23 | 北京化工大学 | Extractive distillation method for separating benzene and thiophene |
| CN104844559A (en) * | 2015-05-21 | 2015-08-19 | 天津大学 | Device and method for extracting thiophene before coking crude benzene hydrogenation |
| CN105498274A (en) * | 2015-11-24 | 2016-04-20 | 长安大学 | An aqueous two-phase system and applications thereof in flavone separation from 'Starking' apple peel |
| CN106083513A (en) * | 2016-08-05 | 2016-11-09 | 北京交通大学海滨学院 | A kind of temperature control type ionic liquid aromatics separation system and method |
| CN108003915A (en) * | 2016-10-28 | 2018-05-08 | 中国石油化工股份有限公司 | The double solvents and method of aromatic hydrocarbons and alkane in a kind of extracting separation diesel oil distillate |
| CN108003915B (en) * | 2016-10-28 | 2020-05-19 | 中国石油化工股份有限公司 | Composite solvent and method for extracting and separating aromatic hydrocarbon and alkane in diesel oil fraction |
| CN110128348A (en) * | 2019-04-28 | 2019-08-16 | 东南大学 | A kind of separating technology of the simple glyoxaline compound based on the preparation of Radziszewski reaction method |
| CN110128348B (en) * | 2019-04-28 | 2021-04-27 | 东南大学 | Separation process of simple imidazole compound prepared based on Radziszewski reaction method |
| CN114057535A (en) * | 2020-08-05 | 2022-02-18 | 中国石油化工股份有限公司 | Composite solvent for extracting, rectifying and separating aromatic hydrocarbon from hydrocarbon mixture and application method thereof |
| CN114057535B (en) * | 2020-08-05 | 2024-03-12 | 中国石油化工股份有限公司 | Composite solvent for extracting, rectifying and separating aromatic hydrocarbon from hydrocarbon mixture and application method |
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