Process for preparing paraphthaloyl chloride

A technology of terephthaloyl chloride and terephthalic acid, applied in the field of chemical raw material preparation, can solve the problems of poor operation safety and protection, unrecyclable by-products, poor product quality controllability and the like, and achieves safe and convenient operation, The effect of high mechanical strength and good paintability

Active Publication Date: 2020-10-30
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, for the synthesis of terephthaloyl chloride technology, there are the following problems: (1) in the selection of chlorinating reagents, traditional chlorinating agents (for example: SOCl 2 , PCl 5 , PCl 3 ) will cause damage to the ecological environment, corrode equipment, pollute the environment, and have poor operational safety and protection; (2) By-products can hardly be recycled and can only be treated as "three wastes"; (3) Product quality controllability poor

Method used

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  • Process for preparing paraphthaloyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] First, add 149.52g carbon tetrachloride, 49.84g (0.3mol) terephthalic acid, 0.11g (0.0008mol) aluminum trichloride to the three-necked flask, raise the temperature to 40°C, add 59.78g (0.4 mol) methyltrichlorosilane, heat preservation reaction for 6h, hydrogen chloride gas enters the absorption device. After the reaction was completed, the solvent carbon tetrachloride was evaporated under reduced pressure for mechanical use, and then terephthaloyl chloride was evaporated under reduced pressure, cooled, crystallized, and dried to obtain 59.05 g of terephthaloyl chloride with a yield of 96.96%. 99.23% pure. After cooling the mother liquor and adding water to quench the aluminum chloride, the by-product polymethylsilsesquioxane was subjected to solid-liquid separation and dried to obtain 25.94 g of high-quality polymethylsilsesquioxane with a yield of 96.66%.

Embodiment 2

[0035] First, add 199.36g carbon tetrachloride, 49.84g (0.3mol) terephthalic acid, 0.4g (0.00246mol) ferric trichloride to the three-necked flask, raise the temperature to 50°C, and add 61.28g (0.41 mol) methyltrichlorosilane, heat preservation reaction for 8h, hydrogen chloride gas enters the absorption device. After the reaction was completed, the solvent carbon tetrachloride was evaporated under reduced pressure for mechanical use, and then terephthaloyl chloride was evaporated under reduced pressure, cooled, crystallized, and dried to obtain 59.61 g of terephthaloyl chloride with a yield of 97.88%. 99.32% pure. After cooling the mother liquor and adding water to quench ferric chloride, the by-product polymethylsilsesquioxane was subjected to solid-liquid separation and dried to obtain 26.07 g of high-quality polymethylsilsesquioxane with a yield of 97.12%.

Embodiment 3

[0037] First, add 299.04g carbon tetrachloride, 49.84g (0.3mol) terephthalic acid, 0.67g (0.00258mol) tin tetrachloride to the three-necked flask, raise the temperature to 60°C, add 64.27g (0.43 mol) methyltrichlorosilane, heat preservation reaction for 6h, hydrogen chloride gas enters the absorption device. After the reaction was completed, the solvent carbon tetrachloride was evaporated under reduced pressure for mechanical use, and then terephthaloyl chloride was evaporated under reduced pressure, cooled, crystallized, and dried to obtain 60.07 g of terephthaloyl chloride with a yield of 98.63%. 99.21% purity. After cooling the mother liquor and adding water to quench tin tetrachloride, the by-product polymethylsilsesquioxane was subjected to solid-liquid separation and dried to obtain 226.39 g of high-quality polymethylsilsesquioxane with a yield of 98.33%.

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Abstract

The invention relates to a new process for preparing paraphthaloyl chloride. The process comprises the following steps: reacting terephthalic acid with methyltrichlorosilane at 40-77 DEG C for 6-12 hours by using carbon tetrachloride as a solvent and Lewis acid as a catalyst, and introducing hydrogen chloride gas into an absorption device to prepare hydrochloric acid; after the reaction is finished, evaporating the solvent carbon tetrachloride under reduced pressure for reuse, evaporating the product paraphthaloyl chloride under reduced pressure, cooling, crystallizing and drying to obtain thehigh-quality paraphthaloyl chloride; cooling mother liquor, adding water to quench the Lewis acid, carrying out solid-liquid separation on byproduct polymethylsilsesquioxane, and drying to obtain polymethylsilsesquioxane with favorable quality.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical raw materials, and in particular relates to a process for preparing terephthaloyl dichloride. Background technique [0002] Terephthaloyl chloride is actually a kind of "ancient" compound, which was synthesized as early as the beginning of the 20th century, but it has been developed and utilized on a large scale in the past 30 to 40 years. Terephthaloyl chloride is a derivative of aromatic carboxylic acid, an important organic synthesis raw material and chemical intermediate, and was identified as a national key new product in 2010. [0003] Terephthaloyl chloride is an important organic chemical raw material, which can be used to synthesize polyamide, polyaramid, polyester, polyarylsulfone fiber and other high-temperature-resistant and high-strength composite materials. For example, aramid 1414 is a polymer of terephthaloyl chloride and p-phenylenediamine. Its toughness and stren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/30C07C51/60C01B7/03C08G77/04C08G77/06C09D183/04C09D5/25C09J183/04G03F7/075
CPCC07C51/60C01B7/035C08G77/045C09D183/04C09D5/18C09J183/04G03F7/0757C07C63/30
Inventor 李培培杨旭梁辉张晓霞王灏赵相柱
Owner QINGDAO UNIV OF SCI & TECH
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