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Method for purifying 4-acetyl-1-methyl naphthalene in acetyl methyl naphthalene mixture

A technology of acetyl-methylnaphthalene mixture and acetyl group, which is applied in the field of purifying 4-acetyl-1-methylnaphthalene, can solve the problems of high requirements for rectification equipment, large production investment cost, and large environmental impact, and achieve improvement The effect of purity and yield, simple method and low cost

Active Publication Date: 2019-05-17
湖北海力环保科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Since the 4-acetyl-1-methylnaphthalene synthesized by the Friedel-Crafts reaction has multiple isomers, and the isomers have close boiling points, the main separation methods are rectification purification and recrystallization, but rectification purification is difficult to obtain high Pure products, and rectification has high requirements for equipment, high production investment costs, limited product purity, and poor economic benefits; recrystallization purification consumes a large amount of solvent, has a large impact on the environment, and is difficult to obtain high-purity products

Method used

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  • Method for purifying 4-acetyl-1-methyl naphthalene in acetyl methyl naphthalene mixture

Examples

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Effect test

Embodiment 1

[0015] A method for purifying 4-acetyl-1-methylnaphthalene from an acetylmethylnaphthalene mixture. The acetylmethylnaphthalene mixture is placed in a melting crystallization device, the temperature is lowered from normal temperature to 12°C, and the uncrystallized mother liquor is released , and then the crystallized solid starts to heat up and sweat from 12°C, the sweating temperature is 15-37°C, and the average heating rate is 2.5°C / h. Stop sweating until the sweat product content reaches 99.0%. Finally, the sweat is discharged, and the crystalline solid in the melting and crystallization device is heated and melted to obtain 4-acetyl-1-methylnaphthalene.

[0016] The purity of the 4-acetyl-1-methylnaphthalene obtained in this example is 99.2%.

Embodiment 2

[0018] A method for purifying 4-acetyl-1-methylnaphthalene from an acetylmethylnaphthalene mixture. The acetylmethylnaphthalene mixture is placed in a melting crystallization device, the temperature is lowered from normal temperature to 12°C, and the uncrystallized mother liquor is released , and then the crystallized solid starts to heat up and sweat from 12°C, the sweating temperature is 15-37°C, and the average heating rate is 1.5°C / h. Stop sweating until the sweat product content reaches 99.0%. Finally, the sweat is discharged, and the crystalline solid in the melting and crystallization device is heated and melted to obtain 4-acetyl-1-methylnaphthalene.

[0019] The purity of the 4-acetyl-1-methylnaphthalene obtained in this example is 99.4%.

Embodiment 3

[0021] A method for purifying 4-acetyl-1-methylnaphthalene from an acetylmethylnaphthalene mixture. The acetylmethylnaphthalene mixture is placed in a melting crystallization device, the temperature is lowered from normal temperature to 12°C, and the uncrystallized mother liquor is released , and then the crystallized solid starts to heat up and sweat from 12°C, the sweating temperature is 15-37°C, and the average heating rate is 0.5°C / h. Stop sweating until the sweat product content reaches 99.0%. Finally, the sweat is discharged, and the crystalline solid in the melting and crystallization device is heated and melted to obtain 4-acetyl-1-methylnaphthalene.

[0022] The purity of the 4-acetyl-1-methylnaphthalene obtained in this example is 99.5%.

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Abstract

The invention relates to a method for purifying 4-acetyl-1-methyl naphthalene in an acetyl methyl naphthalene mixture. The melting point difference between 4-acetyl-1-methyl naphthalene and other acetyl methyl naphthalene is adopted to obtain the 4-acetyl-1-methyl naphthalene with high purity. The acetyl methyl naphthalene mixture is put into a melting crystallization device, and the temperature is reduced from normal temperature to 10-15 DEG C, a mother solution without crystallization is released, and then the crystallized solid is started to heat up and sweat from 10-15 DEG C, the sweatingtemperature is 15-37 DEG C, after the end point of sweating is reached, sweating is stopped, and sweat is discharged; and finally, the crystalline solid in the melting crystallization device is heatedand melted to obtain the 4-acetyl-1-methyl naphthalene. According to the method for purifying the 4-acetyl-1-methyl naphthalene in the acetyl methyl naphthalene mixture, under the condition of not reducing the productive rate, the 4-acetyl-1-methyl naphthalene with the purity larger than 99.0% is obtained, and the operation is easy to operate.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a method for purifying 4-acetyl-1-methylnaphthalene from a mixture of acetylmethylnaphthalene. Background technique [0002] The chemical structural formula of 4-acetyl-1-methylnaphthalene is: [0003] [0004] There are seven isomers of acetylmethylnaphthalene in the mixture of acetylmethylnaphthalene, among which 4-acetyl-1-methylnaphthalene is an important intermediate for the synthesis of 1,4-naphthalene dicarboxylic acid. 1,4-Naphthalene dicarboxylic acid is widely used in the production of optical brighteners, heat-stable polymers and plasticizers, and is also an important dye intermediate. 4-acetyl-1-methylnaphthalene itself is also an important intermediate in organic synthesis. [0005] Since the 4-acetyl-1-methylnaphthalene synthesized by the Friedel-Crafts reaction has multiple isomers, and the boiling points of the isomers are close, the main separation ...

Claims

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Application Information

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IPC IPC(8): C07C45/78C07C49/788C07C45/81
Inventor 王力胡水郑玲邓兵
Owner 湖北海力环保科技股份有限公司
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