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Method for recycling trimethylacetic acid from pivaloyl chloride rectification raffinate

A technology of pivaloyl chloride and pivalic acid, which is applied in the field of chemical technology, can solve the problems that pivalic acid components cannot be effectively recovered, and the environmental pollution of waste liquid is discharged, so as to reduce the pressure on environmental protection, reduce the generation of three wastes, and improve the utilization rate effect

Pending Publication Date: 2018-02-23
山东民基新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the technical defect of prior art, provides a kind of method that reclaims pivalic acid from pivaloyl chloride rectification raffinate, to solve the pivaloyl chloride distillation method of prior art, the distillate raffinate contained The technical problem that the pivalic acid component cannot be effectively recovered
[0005] Another technical problem to be solved by the present invention is that there is an environmental pollution problem in the discharge waste liquid of the conventional pivaloyl chloride distillation method in the prior art

Method used

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  • Method for recycling trimethylacetic acid from pivaloyl chloride rectification raffinate
  • Method for recycling trimethylacetic acid from pivaloyl chloride rectification raffinate

Examples

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Effect test

Embodiment 1

[0018] Add 2500kg of residual liquid into the hydrolysis tank, turn on mechanical stirring, heat to 39~41℃ under 10kpa gauge pressure, add 175kg of water to the reactor at a rate of 100L / h, control the temperature of the hydrolysis tank at 60~61℃; adjust to 50L / h 200kg of water was added at the speed of h, and the vacuum degree was controlled to -10kpa during the period. After the water was added, the temperature was kept for 1 hour, and then it was allowed to stand for 0.5 hours. The lower layer first separates black water-containing phosphorous acid, and then red and yellow pivalic acid, which is sent to the distillation section of the pivalic acid production workshop for decolorization and refining.

Embodiment 2

[0020] Add 2300kg of residual liquid into the hydrolysis tank, turn on mechanical stirring, heat to 38~42℃ under vacuum degree of -8kpa, add 184kg of water to the reactor at a rate of 100L / h, control the temperature of the hydrolysis tank at 59~62℃; adjust to Add 207kg of water at a rate of 50L / h, during which the vacuum degree is controlled to -10kpa, after the addition of water, the temperature is kept for 1h, and the layer is left to stand for 0.5h. The lower layer first separates black water-containing phosphorous acid, and then red and yellow pivalic acid, which is sent to the distillation section of the pivalic acid production workshop for decolorization and refining.

Embodiment 3

[0022] Add 2500kg of residual liquid into the hydrolysis tank, turn on mechanical stirring, heat to 37~43℃ under 6kpa gauge pressure, add 175kg of water to the reactor at a rate of 100L / h, control the temperature of the hydrolysis tank at 58~63℃; adjust to 50L / h Add 175kg of water at the speed of h, and control the vacuum degree to -9kpa during the period. After the addition of water, the temperature is kept and reacted for 1 hour, and then it is allowed to stand for 0.5h. The lower layer first separates black water-containing phosphorous acid, and then red and yellow pivalic acid, which is sent to the distillation section of the pivalic acid production workshop for decolorization and refining.

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Abstract

The invention provides a method for recycling trimethylacetic acid from pivaloyl chloride rectification raffinate. According to the technical scheme, the method has the experiment ideas that components and contents of pivaloyl chloride rectification raffinate are analyzed firstly on the basis of experiment means, on the basis, procedures such as hydrolysis, layering and rectification are confirmedaccording to chemical properties of pivaloyl chloride and trimethylacetic anhydride, and trimethylacetic acid is recycled. Specifically, the method comprises the following steps: firstly, adding a certain amount of pivaloyl chloride rectification raffinate, controlling specific temperature and pressure, adding a proper amount of water for hydrolysis reactions for multiple times to sequentially convert pivaloyl chloride and trimethylacetic anhydride into trimethylacetic acid, leaving to stand to layer water-containing phosphorous acid and a crude trimethylacetic acid product, feeding back thecrude trimethylacetic acid product to a trimethylacetic acid rectification procedure, and performing decoloring refining. By adopting the method provided by the invention, more than 90% of the pivaloyl chloride rectification raffinate can be converted into trimethylacetic acid, so that the utilization rates of raw materials are increased, the wastes are reduced, the environment protection burden of companies is alleviated, and meanwhile the production cost of products is effectively reduced.

Description

Technical field [0001] The invention relates to the technical field of chemical processes, and further relates to the optimization and improvement of the preparation process of pivaloyl chloride, and in particular to a method for recovering pivalic acid from the residual liquid of pivaloyl chloride rectification. Background technique [0002] Pivaloyl chloride is a very important acylation reagent, mainly used as a pharmaceutical intermediate, as the main raw material in the preparation of many amides and phenolic lipid drugs; currently it has been used in amoxicillin, cefadroxil and cefazol Production of drugs such as morpholine and dipivaloyl adrenaline. It is also widely used in the production of pesticide intermediates, such as chloropivaloyl chloride. In chemical synthesis, it is used to protect the amino group while increasing the steric hindrance, and it is easy to obtain a product at a specific position. [0003] In the prior art pivaloyl chloride preparation process, rec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04C07C51/087C07C51/42C07C53/124
CPCC07C51/04C07C51/087C07C51/42C07C53/124
Inventor 张海朋李建军安磊张瑞许自杰张红梅王建芹祝新涛
Owner 山东民基新材料科技有限公司
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