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3, 3 ', 4, 4'-biphenyltetracarboxylic acid reaction crystallization method

A technology of biphenyltetracarboxylic acid and sodium biphenyltetracarboxylic acid is applied in the separation/purification of carboxylic acid compounds, the preparation of carboxylate, organic chemistry, etc. cost reduction effect

Pending Publication Date: 2022-07-22
河北海力香料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the current 3,3',4,4'-biphenyldianhydride production process, 3,3',4,4'-biphenyltetracarboxylic acid sodium solution is used to prepare 3,3',4,4'-biphenyltetracarboxylic acid to produce The content of the product can only reach 99wt%, and there is a problem of low content

Method used

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  • 3, 3 ', 4, 4'-biphenyltetracarboxylic acid reaction crystallization method
  • 3, 3 ', 4, 4'-biphenyltetracarboxylic acid reaction crystallization method
  • 3, 3 ', 4, 4'-biphenyltetracarboxylic acid reaction crystallization method

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Add 300Kg of pure water and 40Kg of 30wt% industrial hydrochloric acid to the enamel reaction tank, heat up to 85°C, and dropwise add 70°C 3,3',4,4'-sodium biphenyltetracarboxylate reaction solution, 300L / h according to 568L / h h Add 40 ℃, 30wt% hydrochloric acid solution dropwise, and control the reaction temperature to 85 ℃, after 2 hours of dropwise addition, transfer the reaction solution to a cooling enamel reaction tank according to the starting 868L / h, cool down to 55 ℃, use a centrifuge for solidification The 3,3',4,4'-biphenyltetracarboxylic acid flake crystals obtained by liquid separation and centrifugation have a moisture content of 15 wt %, and the measured content after drying is 99.8 wt %.

Embodiment 2

[0052] Add 310Kg of pure water and 42Kg of 30wt% industrial hydrochloric acid to the enamel reaction tank, heat up to 80°C, and dropwise add 70°C 3,3',4,4'-sodium biphenyltetracarboxylate reaction solution, 290L / h according to 570L / h h Add 40 ℃, 30wt% hydrochloric acid solution dropwise, and control the reaction temperature to 80 ℃, after 2 hours of dropwise addition, transfer the reaction solution to a cooling enamel reaction tank according to the starting 860L / h, cool down to 50 ℃, use a centrifuge for solidification The 3,3',4,4'-biphenyltetracarboxylic acid flake crystals obtained by liquid separation and centrifugation have a moisture content of 17 wt %, and the measured content after drying is 99.7 wt %.

Embodiment 3

[0054] Add 290Kg of pure water and 35Kg of 30wt% industrial hydrochloric acid to the enamel reaction tank, heat up to 82°C, and dropwise add 70°C 3,3',4,4'-sodium biphenyltetracarboxylate reaction solution, 295L / h according to 565L / h h Add 40 ℃ 30wt% hydrochloric acid solution dropwise, and control the reaction temperature to 82 ℃, after 2 hours of dropwise addition, transfer the reaction solution to a cooling enamel reaction tank according to the starting 860L / h, cool down to 52 ℃, use a centrifuge to conduct solid-liquid separation and centrifugation to obtain 3,3',4,4'-biphenyltetracarboxylic acid flake crystals (crystal morphology such as figure 1 shown), the moisture content was 13 wt%, and the measured content after drying was 99.6 wt%.

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Abstract

The invention provides a 3, 3 ', 4, 4'-biphenyltetracarboxylic acid reaction crystallization method, and belongs to the field of chemical reaction. Mixing water with first hydrochloric acid, and preheating to obtain a preheated hydrochloric acid solution; a 3, 3 ', 4, 4'-biphenyl sodium tetraformate solution and second hydrochloric acid are dropwise added into the preheated hydrochloric acid solution at the same time, an obtained reaction solution is subjected to a double decomposition reaction, a double decomposition product is obtained, and the content of hydrochloric acid in the reaction solution is kept to be 1-10 wt% in the dropwise adding process; and continuously discharging the double decomposition product, and sequentially carrying out cooling and solid-liquid separation. According to the invention, the content of hydrochloric acid in the reaction liquid is ensured to be constant, and simultaneous dropwise addition of the 3, 3 ', 4, 4'-biphenyltetracarboxylic acid sodium solution and hydrochloric acid is limited, so that the crystalline state of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid is improved, crystalline particles of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid are more suitable for solid-liquid separation, and the quality level of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid is improved.

Description

technical field [0001] The invention relates to the technical field of chemical reactions, in particular to a method for crystallization of 3,3',4,4'-biphenyltetracarboxylic acid by reaction. Background technique [0002] 3,3',4,4'-biphenyl dianhydride is an important monomer for the synthesis of polyimide. The polyimide produced by using it has excellent high temperature resistance and high insulation properties, and is widely used in aviation , aerospace, electromechanical, and electronic fields, with the development of digitization, intelligence, and touch screen, polyimide is used as high-end electronic materials for display screens, 5G network equipment materials, and new energy vehicle materials, and its usage is growing rapidly. [0003] With the promotion of high-end applications of 3,3',4,4'-biphthalic anhydride, the demand for high-quality level 3,3',4,4'-biphthalic anhydride is increasing. From the pre-production process, 3 ,3',4,4'-biphenyltetracarboxylic acid i...

Claims

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Application Information

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IPC IPC(8): C07C51/02C07C51/43C07C51/42C07C63/331
CPCC07C51/02C07C51/43C07C51/42C07C63/331
Inventor 郭少康武帆朱玉梅李文革王晶晓李朋
Owner 河北海力香料股份有限公司
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