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Method for synthesizing p-alkylacetophenone by adopting microchannel reactor

A micro-channel reactor, alkyl acetophenone technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, condensation preparation of carbonyl compounds, etc. , the corrosion of equipment by hydrochloric acid, etc., to achieve the effect of overcoming uneven heat release, effective contact, and easy control of reaction conditions

Inactive Publication Date: 2019-01-18
濮阳市欧亚化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problems of complex operation, long time consumption, low yield, large amount of three industrial wastes, unfriendly to the environment, and the hydrochloric acid produced corrodes the equipment and affects the service life of the equipment in the prior art. A proposed method for the synthesis of p-alkylacetophenones using a microchannel reactor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of method that adopts microchannel reactor to synthesize p-alkylacetophenone that the present invention proposes comprises the following steps:

[0024] S1, the preparation of composite catalyst:

[0025] A, the aluminum chloride of 3 weight parts is joined in the dehydrated alcohol of 30 weight parts, stirs until dissolving, obtains aluminum chloride ethanolic solution, for subsequent use;

[0026] B. Mix 0.6 parts by weight of ferric oxide, 10 parts by weight of bibenzylpyridine, 5 parts by weight of 6-chloro-7-azapurine and 1 part by weight of tetrathiafulvalene, and add 20 parts by weight of dehydrated ethanol, stirred at 50°C for 2h, kept warm for 30min, and cooled down to room temperature to obtain a mixed dispersion; set aside;

[0027] C, the mixed dispersion liquid that step B is made joins in the aluminum chloride ethanol solution that step A prepares with the speed of 5g / min, stirs 20min, then the chitosan of 30 weight parts is added, continues to sti...

Embodiment 2

[0032] A kind of method that adopts microchannel reactor to synthesize p-alkylacetophenone that the present invention proposes comprises the following steps:

[0033] S1, the preparation of composite catalyst:

[0034] A, the aluminum trichloride of 3.9 weight parts is joined in the dehydrated alcohol of 39 weight parts, stirs until dissolving, obtains aluminum chloride ethanolic solution, for subsequent use;

[0035] B, the ferric oxide of 0.9 parts by weight, the bibenzylpyridine of 13 parts by weight, the 6-chloro-7-azapurine of 7 parts by weight and the tetrathiafulvalene of 2 parts by weight are mixed, and add 26 parts by weight dehydrated ethanol, stirred at 54°C for 1.5h, kept warm for 25min, and cooled down to room temperature to obtain a mixed dispersion; set aside;

[0036] C, the mixed dispersion liquid that step B is made joins in the aluminum chloride ethanolic solution that step A prepares with the speed of 5g / min, stirs 20min, then the chitosan of 38 weight par...

Embodiment 3

[0041] A kind of method that adopts microchannel reactor to synthesize p-alkylacetophenone that the present invention proposes comprises the following steps:

[0042] S1, the preparation of composite catalyst:

[0043] A, the aluminum trichloride of 4.8 weight parts is joined in the dehydrated alcohol of 48 weight parts, stirs until dissolving, obtains aluminum chloride ethanolic solution, for subsequent use;

[0044] B, the ferric oxide of 1.2 parts by weight, the bibenzylpyridine of 16 parts by weight, the 6-chloro-7-azapurine of 8 parts by weight and the tetrathiafulvalene of 3 parts by weight are mixed, and add 32 parts by weight dehydrated ethanol, stirred at 58°C for 1 hour, kept warm for 20 minutes, and cooled to room temperature to obtain a mixed dispersion; set aside;

[0045] C, the mixed dispersion liquid that step B is made joins in the aluminum chloride ethanol solution that step A prepares with the speed of 5g / min, stirs 20min, then the chitosan of 46 parts by w...

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Abstract

The invention provides a method for synthesizing p-alkylacetophenone by adopting a microchannel reactor. The method comprises the following steps: S1, preparing a composite catalyst: A, preparing an aluminum chloride ethanol solution; B, preparing mixed dispersion liquid by utilizing a mixture of ferroferric oxide, bibenzyl pyridine 6-chloro-7-deazapurine and tetrathiafulvalene as well as absoluteethyl alcohol; and C, adding the mixed dispersion liquid into the aluminum chloride ethanol solution, and then adding chitosan to prepare the composite catalyst; S2, dropwise adding acetyl chloride into dichloroethane and the composite catalyst to obtain a mixed material; S3, enabling 1,3-dimethyl-5-tert-butyl benzene and the mixed material to be subjected to acylation reaction in the microchannel reactor, and enabling reaction liquid to flow out of an outlet; and S4, centrifuging the reaction liquid to respectively treat supernate and a filter cake to obtain a recyclable composite catalyst and p-alkylacetophenone. According to the method provided by the invention, the microchannel reactor is utilized to continuously produce, the operation is simple, the consumed time consumed is short, the three industrial wastes are fewerlittle, and the yield is high.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing p-alkylacetophenone by using a microchannel reactor. Background technique [0002] Ketone musk is 3,5-dinitro-2,6-dimethyl-4-tert-butylacetophenone, a kind of nitro musk, with a soft musky aroma, soluble in almost all spices, synthetic route Short, is widely used in perfume essence, soap essence, cosmetic essence and other fields. p-Alkylacetophenone is the main raw material for the synthesis of musk ketones. With the increase of the demand for musk ketones, the demand for p-alkylacetophenones also increases. The current methods for producing p-alkylacetophenones are mainly Using p-alkylbenzene and acetyl chloride as raw materials, in the presence of aluminum trichloride, through batch production, but this method requires complicated operation of pouring the kettle, which takes a long time and has a low yield. Usually only 74% to 78%. In addi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/46C07C49/76B01J31/28B01J19/00
CPCB01J19/0093B01J31/28C07C45/46C07C49/76Y02P20/584
Inventor 刘国朋邹宗鹏江秀全郜时国王福田路翠翠
Owner 濮阳市欧亚化工科技有限公司
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