CN105601462A - High-purity benzene purification method - Google Patents
High-purity benzene purification method Download PDFInfo
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- CN105601462A CN105601462A CN201610091976.3A CN201610091976A CN105601462A CN 105601462 A CN105601462 A CN 105601462A CN 201610091976 A CN201610091976 A CN 201610091976A CN 105601462 A CN105601462 A CN 105601462A
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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 invention relates to a high-purity benzene purification method and belongs to the technical field of purification technologies of chemical products. The high-purity benzene purification method is characterized by comprising the following steps that benzene is dissolved in a solvent, specific adsorption is conducted on thiophene in the benzene solution through a molecular imprinting adsorption column for the thiophene under the pressure of 0.05-0.10 MPa and at the temperature of 30-60 DEG C; molecular sieve column moisture removal is conducted on the benzene solution subjected to adsorption, and then the purposes of benzene multistage melt crystallization and purification are achieved by adopting a melt crystallization method. The adsorption column for adsorption is prepared by adopting a molecular imprinting technology, and the thiophene in the benzene solution can be effectively removed by relying on the specific adsorption capability of the adsorption column. No solvent is needed in the melt crystallization and purification process, the pollution of the solvent to a product is avoided, the solvent recovery process is also omitted, the investment in equipment is saved, and the purified product is high in purity and yield.
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 has strong aromaTaste. Benzene is flammable, poisonous, is also a kind of carcinogen. Benzene is that a kind of hydrocarbon is also the simplest aromatic hydrocarbons. It is insoluble inWater, is soluble in organic solvent, and itself also can be used as organic solvent. Benzene is a kind of petrochemical industry base stock. The output of benzene and lifeThe technical merit of producing is one of mark of a national petrochemical industry development level. The ring system that benzene has, phenyl ring, is the simplestAromatic ring. Benzene molecular removes the later structure of hydrogen phenyl, represents with Ph. Therefore benzene also can be expressed as PhH.
Fusion-crystallization and conventional chemical separating method (absorption, rectifying, extraction) and some novel isolation technics are (overcriticalExtraction, adsorbing separation, chromatographic isolation, film separate) to compare, this technology has the following advantages:
1, separable go out the product purity processed of the general rectifying of high purity product and recrystallization in 99% left and right, and fusion-crystallization processingProduct purity can reach more than 99.9% even 99.99%, therefore can meet medical product, food additives, spices, biochemical systemProduct, reagent product are to highly purified requirement.
2, be suitable for extremely difficult separation of the conventional rectifying such as extraordinary system material as close in boiling point, isomer, chiral material,But sometimes just quite simple with fusion-crystallization; The material very high to heat-sensitive substance, weak solution, boiling point, fusion-crystallization also veryBe suitable for.
3, low-temperature operation is generally normal pressure, low-temperature operation, safety simple to operate, to equipment without excessive demand, because under low temperatureCorrosivity declines. Without too high requirement, do not need flower great number to invest for heating furnace and high-vacuum apparatus system, therefore thermal sourceCan reduce costs and equipment investment.
4, environmentally friendlyly do not need product to be dried with desolvation compared with using the recrystallization of solvent, therefore subtractLack dry step, cost rising, environmental pollution, the cryogenic freezing operation of having avoided solvent circle to enter to cause.
5, the energy consumption of energy-conservation general fusion-crystallization is only the 10%-30% of rectifying.
Summary of the invention
The technical problem that the present invention solves is: proposes a kind of pollution of solvent to product of having exempted from, reduced again solvent recovery process,The high pure benzene method of purification that purity is high, yield is high of refined product.
In order to solve the problems of the technologies described above, the technical scheme that the present invention proposes is: a kind of high pure benzene method of purification, described purification sideMethod comprises the steps: benzene to be dissolved in methyl alcohol or oxolane, at 0.05～0.10MPa pressure, 30～60 DEG C of temperature through thiopheneThe thiophene in benzole soln is carried out specific adsorption by the molecular engram adsorption column of fen; Benzole soln after absorption is carried out to molecular sieve columnMoisture, then purify to realize the multistage fusion-crystallization of benzene by the method for fusion-crystallization; The method of described fusion-crystallization is for adopting crystallizationDevice, is preheated to 70～80 DEG C by described crystallizer, makes the thick product of the benzene as raw material being placed in one be molten condition; Described in inciting somebody to actionThe benzene of melting is cooled to the crystallization temperature of described benzene with 10 DEG C～20 DEG C/h, makes benzene crystallization; Product Separation of Solid and Liquid after crystallization, willSolid product, as raw material, is recovered in raffinate in storage tank; With 2 DEG C～6 DEG C/h speed by described crystallizer be warming up to 0 DEG C～5 DEG C, insulation, makes described solid product partial melting, and the not crystalline mother solution of discharge is as described raw material; Be opposite to described crystallizerThe crystalline solid obtaining in interior is warming up to whole meltings, and the crystalline solid obtaining is afterwards as the raw material of next stage crystallization.
Preferably, repeat and carry out multistage crystallization, obtain high pure benzene, described repeats as starting repetition from fusion-crystallizationCrystallization: make the thick product of the benzene as raw material being placed in one be molten condition; The benzene of described melting is lowered the temperature with 10 DEG C～20 DEG C/hTo the crystallization temperature of described benzene, make benzene crystallization; Product Separation of Solid and Liquid after crystallization, using solid product as raw material, returns raffinateClose in storage tank; With 2 DEG C～6 DEG C/h speed, described crystallizer is warming up to 0 DEG C～5 DEG C, insulation, makes described solid productPartial melting, the not crystalline mother solution of discharge is as described raw material; The crystalline solid obtaining in being opposite in described crystallizer heats upTo all meltings, the crystalline solid obtaining is afterwards as the raw material of next stage crystallization.
Beneficial effect of the present invention.
High pure benzene of the present invention is purified and has been prepared adsorption column by molecular imprinting and adsorb, and relies on its specificity having to inhaleAttached ability, can effectively remove the thiophene in benzole soln; Without solvent, avoid solvent to product in fusion-crystallization purification processPollute, reduced again solvent recovery process, saved equipment investment, the purity of refined product is high, yield is high.
Detailed description of the invention
Embodiment 1
A kind of high pure benzene method of purification, described method of purification comprises the steps: benzene to be dissolved in methyl alcohol or oxolane, 0.05～At 0.10MPa pressure, 30～60 DEG C of temperature, through the molecular engram adsorption column of thiophene, the thiophene in benzole soln is carried out to specific adsorption;Benzole soln after absorption is carried out to molecular sieve column and anhydrate point, then method by fusion-crystallization is to realize the multistage fusion-crystallization purification of benzeneObject.
The method of described fusion-crystallization, for adopting crystallizer, is preheated to 70～80 DEG C by described crystallizer, makes the conduct being placed in oneThe thick product of benzene of raw material is molten condition; The benzene of described melting is cooled to the crystallization temperature of described benzene, makes with 10 DEG C～20 DEG C/hBenzene crystallization; Product Separation of Solid and Liquid after crystallization, using solid product as raw material, is recovered in raffinate in storage tank; With 2 DEG C～6DEG C/described crystallizer is warming up to 0 DEG C～5 DEG C by h speed, and insulation, makes described solid product partial melting, the not crystallization mother of dischargeLiquid is as described raw material; The crystalline solid obtaining in being opposite in described crystallizer is warming up to whole meltings, the knot obtaining afterwardsCrystal is as the raw material of next stage crystallization;
Multistage crystallization is carried out in repeating step operation, obtains high pure benzene. Described repeats as start repetition crystallization from fusion-crystallization:Make the thick product of the benzene as raw material being placed in one be molten condition; Described in the benzene of described melting is cooled to 10 DEG C～20 DEG C/hThe crystallization temperature of benzene, makes benzene crystallization; Product Separation of Solid and Liquid after crystallization, using solid product as raw material, is recovered in storage by raffinateIn batch can; With 2 DEG C～6 DEG C/h speed, described crystallizer is warming up to 0 DEG C～5 DEG C, insulation, makes described solid product part moltenMelt, the not crystalline mother solution of discharge is as described raw material; The crystalline solid obtaining in being opposite in described crystallizer is warming up to allMelting, the crystalline solid obtaining is afterwards as the raw material of next stage crystallization.
The concrete technical scheme being not limited to described in above-described embodiment of the present invention, all employings are equal to that to replace the technical scheme forming equalFor the protection domain of the present invention's requirement.
Claims (2)
1. a high pure benzene method of purification, is characterized in that: described method of purification comprises the steps: benzene to be dissolved in methyl alcohol or fourHydrogen furans, at 0.05～0.10MPa pressure, 30～60 DEG C of temperature through the molecular engram adsorption column of thiophene by the thiophene in benzole solnSpecific adsorption is carried out in fen; Benzole soln after absorption is carried out to molecular sieve column and anhydrate point, then method by fusion-crystallization is with realizationThe multistage fusion-crystallization of benzene is purified; The method of described fusion-crystallization, for adopting crystallizer, is preheated to 70～80 DEG C by described crystallizer,Make the thick product of the benzene as raw material being placed in one be molten condition; Described in the benzene of described melting is cooled to 10 DEG C～20 DEG C/hThe crystallization temperature of benzene, makes benzene crystallization; Product Separation of Solid and Liquid after crystallization, using solid product as raw material, is recovered in storage by raffinateIn batch can; With 2 DEG C～6 DEG C/h speed, described crystallizer is warming up to 0 DEG C～5 DEG C, insulation, makes described solid product part moltenMelt, the not crystalline mother solution of discharge is as described raw material; The crystalline solid obtaining in being opposite in described crystallizer is warming up to allMelting, the crystalline solid obtaining is afterwards as the raw material of next stage crystallization.
2. high pure benzene method of purification according to claim 1, is characterized in that: repeat and carry out multistage crystallization, obtainHigh pure benzene, described repeats as start repetition crystallization from fusion-crystallization: the thick product of the benzene as raw material being placed in one isMolten condition; The benzene of described melting is cooled to the crystallization temperature of described benzene with 10 DEG C～20 DEG C/h, makes benzene crystallization; After crystallizationProduct Separation of Solid and Liquid, using solid product as raw material, is recovered in raffinate in storage tank; With 2 DEG C～6 DEG C/h speed by described knotBrilliant device is warming up to 0 DEG C～5 DEG C, and insulation, makes described solid product partial melting, and the not crystalline mother solution of discharge is as described raw material;The crystalline solid obtaining in being opposite in described crystallizer is warming up to whole meltings, and the crystalline solid obtaining is afterwards tied as next stageBrilliant 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107253896A (en) * | 2017-06-05 | 2017-10-17 | 北京化工大学 | A kind of method that benzene is reclaimed in the dirty benzene of the overhead product of the benzene column from isopropyl benzene apparatus |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839324A (en) * | 1970-12-22 | 1974-10-01 | Inventa Ag | Process for the purification of caprolactam |
| 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 |
-
2016
- 2016-02-19 CN CN201610091976.3A patent/CN105601462B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839324A (en) * | 1970-12-22 | 1974-10-01 | Inventa Ag | Process for the purification of caprolactam |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107253896A (en) * | 2017-06-05 | 2017-10-17 | 北京化工大学 | A kind of method that benzene is reclaimed in the dirty benzene of the overhead product of the benzene column from isopropyl benzene apparatus |
| 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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| CN105601462B (en) | 2017-08-25 |
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