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A kind of technology for preparing terephthaloyl chloride

A technology of terephthaloyl chloride and terephthalic acid, which is 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, etc., and achieves safe and convenient operation, The effect of high mechanical strength and good paintability

Active Publication Date: 2022-04-26
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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  • A kind of technology for preparing terephthaloyl 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, heat up to 40°C, and add 59.78g (0.4 mol) methyl trichlorosilane, the reaction is kept for 6h, and the hydrogen chloride gas enters the absorption device. After the reaction, the solvent carbon tetrachloride was first evaporated under reduced pressure and applied mechanically, then terephthaloyl chloride was evaporated under reduced pressure, cooled, crystallized, and dried to obtain terephthaloyl chloride 59.05g, yield 96.96%, Purity 99.23%. After cooling the mother liquor and adding water to quench aluminum trichloride, the by-product polymethylsilsesquioxane is separated from the solid-liquid, 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 chloride to the three-necked flask, heat up to 50°C, and add 61.28g (0.41 g (0.41 g) dropwise under stirring for 3h mol) methyl trichlorosilane, the reaction is kept for 8h, and the hydrogen chloride gas enters the absorption device. After the reaction, the solvent carbon tetrachloride was first evaporated under reduced pressure and applied mechanically, then terephthaloyl chloride was evaporated under reduced pressure, cooled, crystallized, and dried to obtain terephthaloyl chloride 59.61g, yield 97.88%, Purity 99.32%. The mother liquor is cooled and water is added to quench ferric chloride, and the by-product polymethylsilsesquioxane is subjected to solid-liquid separation and drying to obtain 26.07 g of high-quality polymethylsilsesquioxane with a yield of 97.12%.

Embodiment 3

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

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Abstract

A new process for preparing terephthaloyl chloride, carbon tetrachloride is used as solvent, Lewis acid is used as catalyst, terephthalic acid and methyl trichlorosilane are reacted at 40-77°C for 6-12h, hydrogen chloride gas enters the absorption device to produce into hydrochloric acid. After the reaction is completed, the solvent carbon tetrachloride is evaporated under reduced pressure for mechanical use, and then the product terephthaloyl chloride is evaporated under reduced pressure, the temperature is lowered, crystallized, and dried to obtain high-quality terephthaloyl chloride. After cooling the mother liquor and adding water to quench the Lewis acid, the by-product polymethylsilsesquioxane is subjected to solid-liquid separation and dried to obtain polymethylsilsesquioxane with good quality.

Description

technical field [0001] The invention belongs to the technical field of chemical raw material preparation, and in particular relates to a process for preparing terephthaloyl chloride. Background technique [0002] Terephthaloyl chloride is actually a kind of "ancient" compound. It was synthesized as early as the early 20th century, but it took nearly 30 to 40 years to develop and utilize it on a large scale. Terephthaloyl chloride is a derivative of aromatic carboxylic acid, an important organic synthesis raw material and chemical intermediate, and was recognized as a national key new product in 2010. [0003] Terephthaloyl chloride is an important organic chemical raw material, which can be used to synthesize high temperature resistant and high strength aggregate materials such as polyamide, polyaramid, polyester and polyaramid. For example, aramid 1414 is a polymer of terephthaloyl chloride and p-phenylenediamine. Its toughness and strength are 2 times and 6 times that of ...

Claims

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Application Information

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Patent Type & Authority Patents(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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