CN107867989A - A kind of method for refining benzophenone - Google Patents
A kind of method for refining benzophenone Download PDFInfo
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- CN107867989A CN107867989A CN201610852515.3A CN201610852515A CN107867989A CN 107867989 A CN107867989 A CN 107867989A CN 201610852515 A CN201610852515 A CN 201610852515A CN 107867989 A CN107867989 A CN 107867989A
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- benzophenone
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- purity
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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
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method for refining benzophenone, slightly yellowish green benzophenone is dissolved in solvent orange 2 A, is heated to 42 DEG C, solvent B is added dropwise, is cooled back to 30 DEG C, obtains white needles, product purity more than 99.95% (GC analyses).Compared with prior art, the present invention can be refining to obtain the benzophenone of high-purity 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, spices 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 spices are determined
Pastil, breath of the spices with sweet tea can be assigned, 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, its 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 medicine and agricultural chemicals.Due to present Market competition, it is necessary 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, carry
The quality of high benzophenone is also that domestic many producers need solve the problems, such as.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind removes existing process
The impurity of obtained benzophenone is produced, improves the method for refining benzophenone of the quality of product.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method for refining benzophenone, it is characterised in that this method dissolves benzophenone in a solvent, enters
Row crystallization, obtains the benzophenone of high-quality, specifically includes following steps：
(1) crude product of solvent orange 2 A and benzophenone will be added in reactor, 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 reactor；
(4) reactor is cooled to 20-30 DEG C, stirred 2 hours；
(5) solidliquid mixture obtained after cooling is filtered, gained solid phase is the benzophenone that purity is more than 99.95%.
Solvent orange 2 A described in step (1) includes but is 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 orange 2 A are 5: (3.2~4.8).
The crude product of benzophenone described in step (1) and the weight ratio of solvent orange 2 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 is not limited to dichloromethane, ethyl acetate, isopropanol, ketone or water.
Benzophenone and solvent B weight ratio described in step (3) are 5: (0.5~1.5).
Benzophenone and solvent B weight ratio described in step (3) are 5: 1.
The temperature cooled in step (4) is 30 DEG C.
Compared with prior art, instant invention overcomes in the production technology of existing benzophenone, because of raw material sources not
With reason, some impurity can be produced, cause the outward 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 high quality, product purity more than 99.95% (GC analyses), Ke Yiman
The requirement of sufficient medication chemistry, value-added content of product is also improved while production cost is controlled.
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, filter, dry, weigh, count 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,
Dry, weigh, count 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, filter, dry, weigh, count 264 grams, the single rate of recovery is 88%, purity ＞ 99.95%.
Claims (2)
- A kind of 1. method for refining benzophenone, it is characterised 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 of solvent orange 2 A and benzophenone will be added in reactor, 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 reactor；(4) reactor is cooled to 20-30 DEG C, stirred 2 hours；(5) solidliquid mixture obtained after cooling is filtered, gained solid phase is the benzophenone that purity is more than 99.95%.
- 2. a kind of method for refining benzophenone according to claim 1, it is characterised in that described in step (1) Solvent orange 2 A include petroleum ether, hexamethylene, n-hexane or methyl tertiary butyl ether(MTBE).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610852515.3A CN107867989A (en) | 2016-09-26 | 2016-09-26 | A kind of method for refining benzophenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610852515.3A CN107867989A (en) | 2016-09-26 | 2016-09-26 | A kind of method for refining benzophenone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107867989A true CN107867989A (en) | 2018-04-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610852515.3A Pending CN107867989A (en) | 2016-09-26 | 2016-09-26 | A kind of method for refining benzophenone |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108586224A (en) * | 2018-06-27 | 2018-09-28 | 天津大学 | A kind of method of benzophenone purifies and separates |
| CN108663246A (en) * | 2018-05-18 | 2018-10-16 | 中国烟草总公司郑州烟草研究院 | Benzophenone purity rubric substance and preparation method thereof |
| CN108693267A (en) * | 2018-05-18 | 2018-10-23 | 中国烟草总公司郑州烟草研究院 | 4- methyl benzophenone purity rubric substances and preparation method thereof |
| 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
- 2016-09-26 CN CN201610852515.3A patent/CN107867989A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108663246A (en) * | 2018-05-18 | 2018-10-16 | 中国烟草总公司郑州烟草研究院 | Benzophenone purity rubric substance and preparation method thereof |
| CN108693267A (en) * | 2018-05-18 | 2018-10-23 | 中国烟草总公司郑州烟草研究院 | 4- methyl benzophenone purity rubric substances and preparation method thereof |
| CN108693267B (en) * | 2018-05-18 | 2020-12-08 | 中国烟草总公司郑州烟草研究院 | 4-methylbenzophenone purity standard substance and preparation method thereof |
| CN108586224A (en) * | 2018-06-27 | 2018-09-28 | 天津大学 | A kind of method of benzophenone purifies and separates |
| CN108586224B (en) * | 2018-06-27 | 2021-05-25 | 天津大学 | Method for purifying and separating benzophenone |
| CN115417757A (en) * | 2022-08-10 | 2022-12-02 | 三峡大学 | Method for separating 4-chlorobenzophenone or benzophenone from benzophenone tail distillation waste |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180403 |