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New compounding technology for 2,4,6-trimethyl phenylacetyl chloride

A technology of trimethylphenylacetyl and trimethylphenylacetic acid, applied in the new synthesis process field of 2,4,6-trimethylphenylacetyl chloride, which can solve the problem of vacuum degree, high temperature equipment requirements of heat transfer oil, chlorination Eliminates problems such as loss of reagents and large distillation residues, which is not conducive to energy saving and consumption reduction, and achieves the effect of low requirements for production equipment, low price, and easy operation

Active Publication Date: 2017-02-22
SUQIAN COSMOS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the actual production process, the loss of chlorinating agent is greater than 3% (molar equivalent), and the amount of distillation residue is more than 1.5% (mass percentage), which is not conducive to energy saving and consumption reduction in production
[0006] It can be seen that there are problems in the existing 2,4,6-trimethylphenylacetyl chloride synthesis technology, that is, the vacuum degree, heat transfer oil temperature and equipment requirements are high, the process conditions are harsh, the loss of chlorinating agent and the distillation residue are too much, pollute the environment and affect the content of finished products

Method used

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  • New compounding technology for 2,4,6-trimethyl phenylacetyl chloride
  • New compounding technology for 2,4,6-trimethyl phenylacetyl chloride
  • New compounding technology for 2,4,6-trimethyl phenylacetyl chloride

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Experimental program
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Effect test

Embodiment 1

[0060] Step (1), add 166.4g of toluene and 5.0g of N,N dimethylformamide into the reaction kettle, start stirring, add 832g (4.7moL) of 2,4,6-trimethylphenylacetic acid in one batch, mix stir well;

[0061] Step (2), adjust the temperature of the reactor to 15°C, add 565.2g (4.75mol) of thionyl chloride dropwise, and the sulfur dioxide and hydrogen chloride gas produced by the reaction will be processed after passing through the condenser. After the dropwise addition, gradually increase the reaction temperature To 55°C, heat preservation reaction for 5h;

[0062] Step (3), after the reaction is completed, filter the reaction system, and carry out distillation and recovery of toluene at a vacuum degree of 500 Pa and a temperature of 120 ° C. After recovery, the remaining system is filtered under reduced pressure to obtain the product 2,4,6-trimethylbenzene Acetyl chloride.

[0063] The product is a yellow liquid. Product in the present embodiment 1 is carried out gas chromat...

Embodiment 2

[0065] Step (1) Add 221.2g of toluene and 4.5g of N,N dimethylformamide into the reaction kettle, start stirring, add 885.0g (5.0moL) of 2,4,6-trimethylphenylacetic acid in one batch, mix stir well;

[0066] Step (2) Adjust the temperature of the reactor to 15°C, add 624.8g (5.25mol) of thionyl chloride dropwise, and then process the sulfur dioxide and hydrogen chloride gas produced by the reaction through the condenser. After the dropwise addition, gradually increase the reaction temperature to 60°C, keep warm for 4 hours;

[0067] Step (3) After the reaction is completed, filter the reaction system, carry out distillation and recovery of toluene at a vacuum degree of 600Pa and a temperature of 115°C, and perform vacuum filtration on the remaining system after recovery to obtain the product 2,4,6-trimethylphenylethyl ether acid chloride.

[0068] The product is a yellow liquid. Product in this embodiment 2 is carried out gas chromatography detection, and the result is as f...

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Abstract

The invention discloses a new compounding technology for 2,4,6-trimethyl phenylacetyl chloride. The new compounding technology comprises the following steps: introducing a low-boiling-point solvent; changing the mode and times of feeding 2,4,6-trimethyl phenylacetic acid; treating acid gas generated in a reaction process; after completing reaction, distilling and recovering the solvent, thereby acquiring the product in higher purity. The method is simple in operation and mild in reaction condition; the corrosion to equipment is reduced and the technology is green and environmentally friendly; the prepared product is high in quality; the purity is more than or equal to 99%.

Description

technical field [0001] The invention relates to a preparation method of an organic intermediate, in particular to a new synthesis process of 2,4,6-trimethylphenylacetyl chloride. Background technique [0002] 2,4,6-Trimethylphenylacetyl chloride is an organic intermediate with a wide range of uses. Used as a photoinitiator in photopolymerizable materials and unsaturated resin models; used as a stabilizer in plastics and paints to improve their light resistance and heat resistance; in medicine, used to prepare antibiotics and antihistamines; It can also be used to prepare coatings, dyes, moldings, adhesives, composite fiber materials, etc. [0003] A kind of synthetic method of 2,4,6-trimethylphenylacetyl chloride is disclosed in CN102633626A: drop into chlorinating agent (SOCl 2 ) and N,N-dimethylformamide (DMF, catalyst) to the reaction kettle, put 2,4,6 trimethylphenylacetic acid in batches, control the temperature for reaction, after the reaction is completed, directly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C57/72
CPCC07C51/60C07C57/72
Inventor 马瑞张乐唐梁平卓宝
Owner SUQIAN COSMOS CHEM
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