Method for production of 2, 6-dimethyl-4-tert-butylacetophenone with tubular reactor

A technology of tert-butyl acetophenone and tubular reactor, which is applied in the direction of chemical instruments and methods, condensation preparation of carbonyl compounds, organic compound/hydride/coordination complex catalysts, etc. The problems of large amount of three wastes and unfriendly environment have been achieved to overcome the effects of uneven heat release, high production efficiency and easy control of reaction conditions

Inactive Publication Date: 2019-02-01
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 complex operation, long time-consuming, many by-products, low product yield, large amount of industrial three wastes, unfriendly to the environment, and the hydrochloric acid produced in the prior art will cause corrosion to the equipment and affect the equipment. The problem of service life, and a kind of method that adopts tubular reactor to produce 2,6-dimethyl-4-tert-butyl acetophenone proposed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of method that the present invention proposes adopts tubular reactor to produce 2,6-dimethyl-4-tert-butylacetophenone, comprises the following steps:

[0022] S1, according to 3 parts by weight of aluminum trichloride, 0.2 parts by weight of tricobalt tetroxide, 0.3 parts by weight of nickel powder, 5 parts by weight of 2-chloro-5-nitropyridine, 5 parts by weight of 4-nitropyrazole, tetrathiafulvalene 1 part by weight, 24 parts by weight of alumina, 1 part by weight of isopropanol, and 50 parts by weight of absolute ethanol Weigh the raw materials of the catalyst, add an appropriate amount of absolute ethanol to aluminum trichloride, stir until dissolved, and obtain an ethanol solution of aluminum chloride ; Add aluminum oxide and isopropanol to the aluminum chloride ethanol solution, stir for 15 minutes to obtain mixture A; combine tricobalt tetroxide, nickel powder, 2-chloro-5-nitropyridine, 4-nitropyrazole, tetrathiofoval Alkene and the remaining amount of abs...

Embodiment 2

[0028] A kind of method that the present invention proposes adopts tubular reactor to produce 2,6-dimethyl-4-tert-butylacetophenone, comprises the following steps:

[0029] S1, according to 3.9 parts by weight of aluminum trichloride, 0.3 parts by weight of tricobalt tetroxide, 0.4 parts by weight of nickel powder, 8 parts by weight of 2-chloro-5-nitropyridine, 8 parts by weight of 4-nitropyrazole, tetrathiafulvalene 2 parts by weight, 26 parts by weight of alumina, 2 parts by weight of isopropanol, and 65 parts by weight of absolute ethanol Weigh the raw materials of the catalyst, add an appropriate amount of absolute ethanol to aluminum trichloride, stir until dissolved, and obtain an ethanol solution of aluminum chloride ; Add aluminum oxide and isopropanol to the aluminum chloride ethanol solution, stir for 20 minutes to obtain mixture A; mix tricobalt tetroxide, nickel powder, 2-chloro-5-nitropyridine, 4-nitropyrazole, tetrathiofoval Alkene and the remaining amount of abs...

Embodiment 3

[0035] A kind of method that the present invention proposes adopts tubular reactor to produce 2,6-dimethyl-4-tert-butylacetophenone, comprises the following steps:

[0036] S1, according to 4.8 parts by weight of aluminum trichloride, 0.5 parts by weight of tricobalt tetroxide, 0.6 parts by weight of nickel powder, 10 parts by weight of 2-chloro-5-nitropyridine, 10 parts by weight of 4-nitropyrazole, and tetrathiafulvalene 3 parts by weight, 28 parts by weight of alumina, 3 parts by weight of isopropanol, and 80 parts by weight of absolute ethanol Weigh the raw materials of the catalyst, add an appropriate amount of absolute ethanol to aluminum chloride, stir until dissolved, and obtain an ethanol solution of aluminum chloride ; Add aluminum oxide and isopropanol to the aluminum chloride ethanol solution, stir for 25min to obtain mixture A; mix tricobalt tetroxide, nickel powder, 2-chloro-5-nitropyridine, 4-nitropyrazole, tetrathiofoval olefin and the rest of absolute ethanol ...

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PUM

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Abstract

The invention provides a method for production of 2, 6-dimethyl-4-tert-butylacetophenone with a tubular reactor. The method includes the steps of: S1, preparing an aluminum chloride ethanol solution,adding alumina and isopropanol to obtain a mixture A, conducting ultrasonic dispersion on cobaltosic oxide, nickel powder, 2-chloro-5-nitropyridine, 4-nitropyrazole, tetrathiafulvalene and anhydrous ethanol, adding a mixture A and then performing treatment to obtain a catalyst; S2, mixing dichloroethane with the catalyst to obtain a mixture B; S3, subjecting the mixture B, acetyl chloride and 1, 3-dimethyl-5-tert-butylbenzene to acylation reaction in a tubular reactor, and discharging the reaction liquid from an upper discharge hole; and S4, centrifuging the reaction liquid, and respectively treating the supernatant and filter cake, thus obtaining the recovered catalyst and 2, 6-dimethyl-4-tert-butylacetophenone. The method provided by the invention utilizes the tubular reactor for continuous production, and has the advantages of simple operation, short time, few three industrial wastes, few by-product and high yield.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for producing 2,6-dimethyl-4-tert-butylacetophenone by using a tubular 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. 2,6-dimethyl-4-tert-butyl acetophenone is the main raw material for the synthesis of ketone musk, and with the increase of demand for ketone musk, 2,6-dimethyl-4-tert-butyl acetophenone The demand is also increasing, and the current method of producing 2,6-dimethyl-4-tert-butylacetophenone is mainly based on 1,3-dimethyl-5-tert-butylbenzene and acetyl chloride as raw materials , in the presence of aluminum trichloride, through batch production, but this method requires complex operation of pouring the kett...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/76C07C45/46B01J31/28
CPCB01J31/28C07C45/46C07C49/76
Inventor 郜时国江秀全王福田刘国朋路翠翠邹宗鹏
Owner 濮阳市欧亚化工科技有限公司
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