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Method for producing p-methylacetophenone with fixed-bed reactor

A fixed-bed reactor, the technology of p-methylacetophenone, which is applied in the fields of food and chemical industry, can solve the problems such as catalyst can not be recycled, equipment is corroded after treatment, large reaction investment consumption, etc., and achieves easy scale and continuous production. , The effect of low design cost and simple structure

Inactive Publication Date: 2013-06-05
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional reaction process for synthesizing p-methylacetophenone is mainly based on simple batch reactors, which have shortcomings such as small reaction capacity, insufficient reaction, large reaction investment consumption, and poor economic benefits.
At present, the domestic method of synthesizing p-methylacetophenone is mainly obtained by the acylation reaction of toluene and acetic anhydride under the catalysis of Lewis acid or protonic acid, etc., and the catalyst itself cannot be recycled, which seriously corrodes the equipment and after-sales service. Deal with serious pollution and other defects

Method used

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  • Method for producing p-methylacetophenone with fixed-bed reactor
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  • Method for producing p-methylacetophenone with fixed-bed reactor

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Embodiment 1

[0034] Reaction section: MCM-41 catalyst bed is installed in the fixed bed reactor, and the catalyst bed packing method is random; at the temperature of 60°C and the pressure of 0.05MPa, the molar ratio of 1:0.1 Toluene and acetic anhydride are pre-mixed uniformly, and are sent into a fixed-bed reactor with a raw material feeding pump to carry out acylation reaction to obtain p-methylacetophenone crude product, the conversion rate of acetic anhydride is 35.7%, and the yield of p-methylacetophenone 95%;

[0035] Refining section: The crude product of p-methylacetophenone is purified by batch distillation to obtain p-methylacetophenone product with a purity of 99%.

Embodiment 2

[0037] Reaction section: HZSM-5 catalyst bed is installed in the fixed bed reactor, and the catalyst bed packing method is random; at the temperature of 80°C and the pressure of 0.3MPa, the molar ratio of 1:2 Toluene and acetyl chloride are pre-mixed uniformly, and are sent into a fixed-bed reactor with a raw material feed pump to carry out acylation reaction to obtain the crude product of p-methylacetophenone, the conversion rate of toluene is 52%, and the yield of p-methylacetophenone is 96%;

[0038] Refining section: The crude p-methylacetophenone is purified by batch distillation to obtain p-methylacetophenone product with a purity of 99.5%.

Embodiment 3

[0040] Reaction section: The fixed bed reactor is equipped with a Mont-K10 catalyst bed, and the catalyst bed is packed in random type; under the conditions of temperature 160 ° C and pressure 0.5 MPa, the molar ratio of 1:15 Toluene and acetic acid are sent into the fixed-bed reactor respectively with raw material feeding pump and carry out acylation reaction to obtain p-methylacetophenone crude product, the conversion rate of toluene is 65%, and the yield of p-methylacetophenone is 96%;

[0041] Refining section: The crude p-methylacetophenone is purified by batch distillation to obtain p-methylacetophenone product with a purity of 99.1%.

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Abstract

The invention discloses a method for producing p-methylacetophenone with a fixed-bed reactor, which comprises the following steps: (1) reaction section: under the conditions of 60-300 DEG C and 0.05-30 MPa, evenly mixing toluene and an acylation reagent, sending the mixture into a fixed-bed reactor by a raw material feeding pump to carry out acylation reaction, thereby obtaining a p-methylacetophenone crude product, wherein the fixed-bed reactor is filled with a catalyst bed layer; and (2) refinement section: purifying the p-methylacetophenone crude product by a rectification technique to obtain the high-purity p-methylacetophenone product. Compared with the traditional technical process, the technical process disclosed by the invention is simple to operate, and has the advantages of low investment cost, high product purity and the like; and meamwhile, the reactor has a simple structure, is stable for operation and convenient for control, and can easily implement large-scale and continuous production.

Description

technical field [0001] The invention relates to a method for producing and synthesizing p-methylacetophenone with a fixed-bed reactor, belonging to the technical fields of food and chemical industry. Background technique [0002] As we all know, p-methylacetophenone is an important fine chemical intermediate in the field of food and chemical industry. It has a fragrance similar to hawthorn flower, and has a fragrance like honey and strawberry. The fragrance of flowers and fruits is sharp and sweet. It is widely used in It can be used to prepare various flavors, intermediates of herbicides, etc. It can also be used as a food additive, and also an intermediate for the production of other high value-added products. Its natural products exist in rosewood essential oil and mimosa flower oil. [0003] The synthesis of p-methylacetophenone at the stage of basic research in laboratories at home and abroad is limited to batch experiments, and there are few continuous experiments on i...

Claims

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Application Information

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IPC IPC(8): C07C49/76C07C45/46
Inventor 曾爱武佟天下陈志华贾鹏飞
Owner TIANJIN UNIV
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