CN108203370A - A kind of method for refining benzophenone - Google Patents
A kind of method for refining benzophenone Download PDFInfo
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- CN108203370A CN108203370A CN201611187438.0A CN201611187438A CN108203370A CN 108203370 A CN108203370 A CN 108203370A CN 201611187438 A CN201611187438 A CN 201611187438A CN 108203370 A CN108203370 A CN 108203370A
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- benzophenone
- solvent
- refining
- cooled
- reaction kettle
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
Abstract
The present invention relates to a kind of methods for refining benzophenone, and slightly yellowish green benzophenone is dissolved in solvent A, are heated to 42 DEG C, and solvent B is added dropwise, is cooled back to 30 DEG C, obtains white needles, more than 99.95% product purity (GC analyses).Compared with prior art, the present invention can be refining to obtain the benzophenone of high purity and high quality, meet the requirement of medication chemistry, value-added content of product is also improved while production cost is controlled.
Description
Technical field
The present invention relates to a kind of method of refined purification, more particularly, to a kind of method for refining benzophenone.
Background technology
Benzophenone is the important intermediate of organic synthesis, is widely used in organic coating, dyestuff, adhesive, ink, modeling
The fields such as material, medicine, daily-use chemical industry, fragrance food, agricultural chemical insecticide and electronic chemical product.As free radical photo-initiation and height
The ultra-violet absorber of molecular material uses, and can make photoactive coating and photopolymer plate.It is usually used in producing in medical industry
Perhexiline, benzatropine hydrobromate and diphenhydramine hydrochloride.This product is also that styrene polymerization inhibitor and fragrance are determined
Pastil can assign breath of the fragrance with sweet tea, and the exploitation used in many perfume and soap derived product is particularly powerful, particularly radiates
Coating material solidified, paper-making industry.Benzophenone also can be widely used in food processing industry, dosage (mg/kg)：Soft drink 0.5；Ice river in Henan Province
Leaching 0.61；Candy 1.7；In baked goods 2.4.In addition, benzophenone can easily be reduced into benzhydrol, and then it is converted into
Halogenated diphenyl methane, they are all the raw materials for manufacturing drug and pesticide.Due to present Market competition, need to reduce product into
It is original to improve the market competitiveness.Simultaneously, the benzophenone of high-purity can also be applied to field of medicine and chemical technology, so, it carries
The quality of high benzophenone is also that domestic many producers need solve the problems, such as.
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of removing prior arts
Produce the obtained impurity of benzophenone, improve product quality for the method that refines benzophenone.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method for refining benzophenone, which is characterized in that this method by benzophenone dissolve in a solvent, into
Row crystallization, obtains the benzophenone of high-quality, specifically includes following steps：
(1) crude product for solvent A and benzophenone being added in reaction kettle, is heated to 40-50 DEG C；
(2) obtained solution is cooled to 30-40 DEG C；
(3) solvent B is added drop-wise in reaction kettle；
(4) reaction kettle is cooled to 20-30 DEG C, stirred 2 hours；
(5) solidliquid mixture obtained after cooling is filtered, gained solid phase is more than 99.95% benzophenone for purity.
Solvent A described in step (1) includes but not limited to petroleum ether, hexamethylene, n-hexane or methyl tertiary butyl ether(MTBE).
The crude product of benzophenone described in step (1) and the weight ratio of solvent A are 5: (3.2~4.8).
The crude product of benzophenone described in step (1) and the weight ratio of solvent A are 5: 4.
The temperature being heated in step (1) is 42 DEG C.
The temperature cooled in step (2) is 35 DEG C.
Solvent B described in step (3) includes but not limited to dichloromethane, ethyl acetate, isopropanol, ketone or water.
Benzophenone and solvent B weight ratios described in step (3) are 5: (0.5~1.5).
Benzophenone and solvent B weight ratios described in step (3) are 5: 1.
The temperature cooled in step (4) is 30 DEG C.
Compared with prior art, the present invention overcomes in the production technology of existing benzophenone, because of raw material sources not
With reason, some impurity can be generated, cause the appearance of product slightly yellow green the defects of, in order to remove some foreign pigments,
Benzophenone can be dissolved in petroleum ether (60~90 DEG C of petroleum ether), be heated to 42 DEG C, ethyl acetate is added dropwise, is cooled back to 30
DEG C, obtain the benzophenone white needles of high purity and high quality, more than 99.95% product purity (GC analyses), Ke Yiman
The requirement of sufficient medication chemistry also improves value-added content of product while production cost is controlled.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
300 grams of benzophenone is dissolved in 288 grams of petroleum ether, is heated to 50 DEG C, reaction solution is in faint yellow, cooling
To 40 DEG C, 90 grams of ethyl acetate are added dropwise, after being added dropwise, is cooled to 30 DEG C, stirs 2 hours, obtain white needles
Solid filters, dry, weighs, and counts 242 grams, the single rate of recovery is 80.6%, purity ＞ 99.95%.
Embodiment 2
300 grams of benzophenone is dissolved in 240 grams of petroleum ether, is heated to 42 DEG C, reaction solution is in faint yellow, is cooled to
35 DEG C, 90 grams of ethyl acetate are added dropwise, after being added dropwise, is cooled to 30 DEG C, stirs 2 hours, obtain white needles, filter,
It is dry, it weighs, counts 246 grams, the single rate of recovery is 82%, purity ＞ 99.95%.
Embodiment 3
300 grams of benzophenone is dissolved in 240 grams of petroleum ether, is heated to 42 DEG C, reaction solution is in faint yellow, cooling
To 35 DEG C, 60 grams of ethyl acetate are added dropwise, after being added dropwise, is cooled to 30 DEG C, stirs 2 hours, obtain white needles
Solid filters, dry, weighs, and counts 264 grams, the single rate of recovery is 88%, purity ＞ 99.95%.
Claims (2)
- A kind of 1. method for refining benzophenone, which is characterized in that this method dissolves benzophenone in a solvent, carries out Crystallization, obtains the benzophenone of high-quality, specifically includes following steps：(1) crude product for solvent A and benzophenone being added in reaction kettle, is heated to 40-50 DEG C；(2) obtained solution is cooled to 30-40 DEG C；(3) solvent B is added drop-wise in reaction kettle；(4) reaction kettle is cooled to 20-30 DEG C, stirred 2 hours；(5) solidliquid mixture obtained after cooling is filtered, gained solid phase is more than 99.95% benzophenone for purity.
- 2. a kind of method for refining benzophenone according to claim 1, which is characterized in that described in step (1) Solvent A include petroleum ether, hexamethylene, n-hexane or methyl tertiary butyl ether(MTBE).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611187438.0A CN108203370A (en) | 2016-12-20 | 2016-12-20 | A kind of method for refining benzophenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611187438.0A CN108203370A (en) | 2016-12-20 | 2016-12-20 | A kind of method for refining benzophenone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108203370A true CN108203370A (en) | 2018-06-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611187438.0A Pending CN108203370A (en) | 2016-12-20 | 2016-12-20 | A kind of method for refining benzophenone |
Country Status (1)
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| CN (1) | CN108203370A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417757A (en) * | 2022-08-10 | 2022-12-02 | 三峡大学 | Method for separating 4-chlorobenzophenone or benzophenone from benzophenone tail distillation waste |
-
2016
- 2016-12-20 CN CN201611187438.0A patent/CN108203370A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417757A (en) * | 2022-08-10 | 2022-12-02 | 三峡大学 | Method for separating 4-chlorobenzophenone or benzophenone from benzophenone tail distillation waste |
| CN115417757B (en) * | 2022-08-10 | 2023-09-19 | 三峡大学 | Method for separating 4-chlorobenzophenone or benzophenone from benzophenone tailing waste material |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180626 |
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| WD01 | Invention patent application deemed withdrawn after publication |