CN105601462B - A kind of high pure benzene method of purification - Google Patents
A kind of high pure benzene method of purification Download PDFInfo
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- CN105601462B CN105601462B CN201610091976.3A CN201610091976A CN105601462B CN 105601462 B CN105601462 B CN 105601462B CN 201610091976 A CN201610091976 A CN 201610091976A CN 105601462 B CN105601462 B CN 105601462B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
- C07C7/13—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers by molecular-sieve technique
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
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Abstract
The present invention relates to a kind of high pure benzene method of purification, belong to the purifying technology field of chemical products.The invention discloses a kind of high pure benzene method of purification, it is characterised in that the method for purification comprises the following steps：Benzene is dissolved in solvent, the thiophene in benzole soln is carried out specific adsorption by the molecular engram adsorption column through thiophene at a temperature of 0.05~0.10MPa pressure, 30~60 DEG C；Benzole soln after absorption is subjected to molecular sieve column and removes moisture, then by the method for fusion-crystallization to realize the purpose of the multistage fusion-crystallization purification of benzene.The present invention is prepared for adsorption column by molecular imprinting technology and adsorbed, and the specific adsorption ability having by it can effectively remove the thiophene in benzole soln；Without solvent in fusion-crystallization purification process, it is to avoid pollution of the solvent to product, solvent recovery process is reduced again, equipment investment is saved, and the purity of refined product is high, high income.
Description
Technical field
The present invention relates to a kind of high pure benzene method of purification, belong to the purifying technology field of chemical products.
Background technology
Benzene (Benzene, C6H6) is a kind of colourless, pleasantly sweet transparency liquid at normal temperatures, and with strong fragrance
Smell.Benzene is flammable, poisonous, is also a kind of carcinogen.Benzene is that a kind of hydrocarbon is also simplest aromatic hydrocarbons.It is insoluble in
Water, is soluble in organic solvent, and itself can also be used as organic solvent.Benzene is a kind of petrochemical industry base stock.The yield of benzene and life
The technical merit of production is one of mark of a national oil development of chemical industry level.The ring system that benzene has, phenyl ring, is most simple
Aromatic ring.Benzene molecular removes a later structure of hydrogen phenyl, is represented with Ph.Therefore benzene is also referred to as PhH.
Fusion-crystallization and conventional chemical separating method (absorption, rectifying, extraction) and some new isolation technics are (super to face
Boundary's extraction, adsorbing separation, chromatographic isolation, UF membrane) to compare, the technology has advantages below：
1st, the product purity of the general rectifying of high purity product and recrystallization processing is may separate out 99% or so, and fusion-crystallization
The product purity of processing can reach more than 99.9% even 99.99%, therefore can meet medical product, food additives, spices,
The requirement of biochemical product, reagent manufacture to high-purity.
2nd, it is suitable for the close material of extraordinary thing system such as boiling point, isomer, chiral material etc. extremely difficult with conventional rectifying
Separation, but it is sometimes just comparatively simple with fusion-crystallization；To heat-sensitive substance, weak solution, boiling point very high material, fusion-crystallization
It is applicable very much.
3rd, low-temperature operation is usually normal pressure, low-temperature operation, safety simple to operate, to equipment without excessive demand, because low temperature
Lower corrosivity declines.To thermal source without too high requirement, it is not necessary to which flower enormous investment is used for heating furnace and high-vacuum apparatus system, because
This can reduce cost and equipment investment.
4th, compared with the environmentally friendly recrystallization with using solvent, it is not necessary to product is dried with desolvation, because
This reduces dry step, it is to avoid cost rise, environmental pollution, cryogenic freezing are operated caused by solvent circle enters.
5th, the energy consumption for saving general fusion-crystallization is only the 10%-30% of rectifying.
The content of the invention
Present invention solves the technical problem that being：A kind of pollution for having exempted from solvent to product is proposed, solvent recovery is reduced again
Process, the purity height of refined product, the high pure benzene method of purification of high income.
In order to solve the above-mentioned technical problem, technical scheme proposed by the present invention is：A kind of high pure benzene method of purification, it is described to carry
Pure method comprises the following steps：Benzene is dissolved in methanol or tetrahydrofuran, at a temperature of 0.05~0.10MPa pressure, 30~60 DEG C
Thiophene in benzole soln is carried out specific adsorption by the molecular engram adsorption column through thiophene；Benzole soln after absorption is subjected to molecule
Sieve post removes moisture, then by the method for fusion-crystallization to realize that the multistage fusion-crystallization of benzene is purified；The method of the fusion-crystallization is
Using crystallizer, the crystallizer is preheated to 70~80 DEG C, it is in molten to make the benzene crude product as raw material being placed in one
State；The benzene of the melting is cooled to the crystallization temperature of the benzene with 10 DEG C~20 DEG C/h, benzene is crystallized；Product after crystallization is consolidated
Liquid is separated, and using solid product as raw material, raffinate is recovered in storage tank；With 2 DEG C~6 DEG C/h speed by the crystallizer liter
Temperature is to 0 DEG C~5 DEG C, and insulation makes the solid product partial melting, the non-crystalline mother solution of discharge is used as the raw material；It is opposite to
The crystalline solid obtained in the crystallizer carries out being warming up to whole meltings, what the crystalline solid obtained afterwards was crystallized as next stage
Raw material.
It is preferred that, carry out multistage crystallization is repeated, high pure benzene is obtained, described repeats as since fusion-crystallization
Repeat to crystallize：It is in molten condition to make the benzene crude product as raw material being placed in one；By the benzene of the melting with 10 DEG C~20 DEG C/
H is cooled to the crystallization temperature of the benzene, crystallizes benzene；Product separation of solid and liquid after crystallization, will be residual using solid product as raw material
Liquid is recovered in storage tank；The crystallizer is warming up to 0 DEG C~5 DEG C with 2 DEG C~6 DEG C/h speed, insulation produces the solid phase
Thing partial melting, the non-crystalline mother solution of discharge is used as the raw material；The crystalline solid obtained in being opposite in the crystallizer is carried out
Whole meltings are warming up to, the raw material that the crystalline solid obtained afterwards is crystallized as next stage.
Beneficial effects of the present invention.
The high pure benzene purification of the present invention is prepared for adsorption column by molecular imprinting technology and adsorbed, the spy having by it
Different in nature adsorption capacity, can effectively remove the thiophene in benzole soln；In fusion-crystallization purification process without solvent, it is to avoid solvent pair
The pollution of product, reduces solvent recovery process again, saves equipment investment, the purity height of refined product, high income.
Embodiment
Embodiment 1
A kind of high pure benzene method of purification, the method for purification comprises the following steps：Benzene is dissolved in methanol or tetrahydrofuran,
0.05~0.10MPa pressure, at a temperature of 30~60 DEG C the molecular engram adsorption column through thiophene the thiophene in benzole soln is carried out it is special
Opposite sex absorption；Benzole soln after absorption is subjected to molecular sieve column and removes moisture, then by the method for fusion-crystallization to realize that benzene is multistage
The purpose of fusion-crystallization purification.
The crystallizer is preheated to 70~80 DEG C, makes to be placed in one by the method for the fusion-crystallization to use crystallizer
The benzene crude product as raw material be in molten condition；The benzene of the melting is cooled to the crystallization of the benzene with 10 DEG C~20 DEG C/h
Temperature, crystallizes benzene；Product separation of solid and liquid after crystallization, using solid product as raw material, raffinate is recovered in storage tank；With
The crystallizer is warming up to 0 DEG C~5 DEG C by 2 DEG C~6 DEG C/h speed, and insulation makes the solid product partial melting, discharge is not
Crystalline mother solution is used as the raw material；The crystalline solid obtained in being opposite in the crystallizer carries out being warming up to whole meltings, afterwards
The raw material that obtained crystalline solid is crystallized as next stage；
Repeat step operation carries out multistage crystallization, obtains high pure benzene.Described repeats as the weight since fusion-crystallization
Complex crystallization：It is in molten condition to make the benzene crude product as raw material being placed in one；By the benzene of the melting with 10 DEG C~20 DEG C/h
The crystallization temperature of the benzene is cooled to, benzene is crystallized；Product separation of solid and liquid after crystallization, will be residual using solid product as raw material
Liquid is recovered in storage tank；The crystallizer is warming up to 0 DEG C~5 DEG C with 2 DEG C~6 DEG C/h speed, insulation produces the solid phase
Thing partial melting, the non-crystalline mother solution of discharge is used as the raw material；The crystalline solid obtained in being opposite in the crystallizer is carried out
Whole meltings are warming up to, the raw material that the crystalline solid obtained afterwards is crystallized as next stage.
The concrete technical scheme being not limited to described in above-described embodiment of the present invention, the technology of all use equivalent substitution formation
Scheme is the protection domain of application claims.
Claims (2)
1. a kind of benzene method of purification, it is characterised in that：The method of purification comprises the following steps：Benzene is dissolved in methanol or tetrahydrochysene furan
Mutter, the molecular engram adsorption column through thiophene enters the thiophene in benzole soln at a temperature of 0.05~0.10MPa pressure, 30~60 DEG C
Row specific adsorption；Benzole soln after absorption is subjected to molecular sieve column and removes moisture, then by the method for fusion-crystallization to realize benzene
Multistage fusion-crystallization purification；The crystallizer is preheated to 70~80 DEG C, made by the method for the fusion-crystallization to use crystallizer
The benzene crude product as raw material being placed in one is in molten condition；The benzene of the melting is cooled to 10 DEG C~20 DEG C/h described
The crystallization temperature of benzene, crystallizes benzene；Product separation of solid and liquid after crystallization, using solid product as raw material, storage is recovered in by raffinate
In batch can；The crystallizer is warming up to 0 DEG C~5 DEG C with 2 DEG C~6 DEG C/h speed, insulation melts the solid product part
Melt, the non-crystalline mother solution of discharge is used as the raw material；The crystalline solid obtained in being opposite in the crystallizer be warming up to entirely
Portion is melted, the raw material that the crystalline solid obtained afterwards is crystallized as next stage.
2. benzene method of purification according to claim 1, it is characterised in that：Carry out multistage crystallization is repeated, benzene, institute is obtained
That states repeats to repeat to crystallize since fusion-crystallization：It is in molten to make the benzene crude product as raw material being placed in one
State；The benzene of the melting is cooled to the crystallization temperature of the benzene with 10 DEG C~20 DEG C/h, benzene is crystallized；Product after crystallization is consolidated
Liquid is separated, and using solid product as raw material, raffinate is recovered in storage tank；With 2 DEG C~6 DEG C/h speed by the crystallizer liter
Temperature is to 0 DEG C~5 DEG C, and insulation makes the solid product partial melting, the non-crystalline mother solution of discharge is used as the raw material；It is opposite to
The crystalline solid obtained in the crystallizer carries out being warming up to whole meltings, what the crystalline solid obtained afterwards was crystallized as next stage
Raw material.
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| CN201610091976.3A CN105601462B (en) | 2016-02-19 | 2016-02-19 | A kind of high pure benzene method of purification |
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| CN105601462A CN105601462A (en) | 2016-05-25 |
| CN105601462B true CN105601462B (en) | 2017-08-25 |
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| CN107253896B (en) * | 2017-06-05 | 2020-02-18 | 北京化工大学 | Method for recovering benzene from benzene column top product polluted benzene in cumene device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CH549020A (en) * | 1970-12-22 | 1974-05-15 | Inventa Ag | METHOD FOR PURIFYING LACTAMEN. |
| CN101885658A (en) * | 2010-07-17 | 2010-11-17 | 天津市化学试剂研究所 | Method for preparing n-dotriacontane |
| CN102617265A (en) * | 2011-01-30 | 2012-08-01 | 江苏永鹏科技实业有限公司 | Refined crude benzene and method for extracting thiophene |
| CN102701997A (en) * | 2012-07-09 | 2012-10-03 | 江苏飞亚化学工业有限责任公司 | Process for purifying dialkyl diphenylamine |
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