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Method for preparing 3, 3 ', 4, 4'-biphenyltetracarboxylic dianhydride

A technology of biphenyltetracarboxylic dianhydride and biphenyltetracarboxylic acid, which is applied in the field of preparation of 3,3', can solve the problems of high production cost of biphenyltetracarboxylic acid, achieve the effects of eliminating residues, simple industrial production, and easy availability of raw materials

Active Publication Date: 2020-09-04
河北东丽新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the technical problem of high production cost of 3,3', 4,4'-biphenyltetracarboxylic acid and improve the product quality of 3,3', 4,4'-biphenyltetracarboxylic acid, the present invention is a dechlorination coupling catalyst Research was carried out, and a suitable reducing agent was selected, and a method for preparing 3,3', 4,4'-biphenyltetracarboxylic acid was obtained. The method obtained 3,3', 4,4'-biphenyltetracarboxylic acid Good quality, low production cost, simple process, easy to industrialize

Method used

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  • Method for preparing 3, 3 ', 4, 4'-biphenyltetracarboxylic dianhydride
  • Method for preparing 3, 3 ', 4, 4'-biphenyltetracarboxylic dianhydride
  • Method for preparing 3, 3 ', 4, 4'-biphenyltetracarboxylic dianhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of palladium-copper carbon-supported catalyst:

[0023] Weigh 0.42g solid CuCl 2 , dissolved in 100 ml of pure water, add 20 g of 5% palladium carbon catalyst into the solution, raise the temperature to 80°C, adjust the pH to 11 with aqueous sodium hydroxide solution, let it stand for 1 hour, stir and keep the temperature, add 10% aqueous sodium formate 8 g, keep warm for 8 hours, drop to room temperature, filter, wash with 260 ml of water, and drain to obtain a palladium-copper carbon-supported catalyst, which is set aside.

[0024] Preparation of 3,3',4,4'-biphenyltetracarboxylic dianhydride:

[0025] Put 336.2ml of pure water and 59.3g of sodium hydroxide into a 1000ml four-necked reaction flask equipped with a peristaltic pump, a thermometer and stirring, stir and dissolve, then add 110g of chlorophthalic acid monosodium salt mixture (4-chlorophthalic acid Diformic acid monosodium salt 75.1%, 4,5-dichlorophthalic acid monosodium salt 10.3%, 3-chloropht...

Embodiment 2

[0032] Preparation of palladium-copper carbon-supported catalyst:

[0033] Weigh 0.42g solid CuCl 2 , dissolved in 100 ml of pure water, 20 g of 5% palladium carbon catalyst was added into the solution, the temperature was raised to 80°C, and the pH was adjusted to 11 with aqueous sodium hydroxide solution, left to stand for 1.5 h, stirred and kept at temperature, and 10% sodium formate was added 8g of aqueous solution, continue to keep warm for 8h, cool down, filter, wash with 260ml of water, and drain to obtain a palladium-copper carbon-supported catalyst, which is set aside.

[0034] Preparation of 3,3',4,4'-biphenyltetracarboxylic dianhydride:

[0035]Put 336.2ml of pure water and 59.3g of sodium hydroxide into a 1000ml four-necked reaction flask equipped with a peristaltic pump, a thermometer and stirring, stir and dissolve, then add 110g of chlorophthalic acid monosodium salt mixture (4-chlorophthalic acid Diformic acid monosodium salt 79.6%, 4,5-dichlorophthalic acid ...

Embodiment 3

[0042] Preparation process of palladium-copper carbon-supported catalyst:

[0043] Weigh 0.42g solid CuCl 2 , dissolved in 100 ml of pure water, take 20 g of 5% palladium carbon catalyst and add it into the solution, raise the temperature to 100°C, adjust the pH to 11 with aqueous sodium hydroxide solution, let it stand for 1 hour, stir and keep the temperature, add 10% aqueous sodium formate 8g, continue to keep warm for 12h, cool down, filter, wash with 260 ml of water, and drain to obtain a palladium-copper carbon-supported catalyst, which is set aside.

[0044] Preparation of 3,3',4,4'-biphenyltetracarboxylic dianhydride:

[0045] Put 336.2ml of pure water and 59.3g of sodium hydroxide into a 1000ml four-necked reaction flask equipped with a peristaltic pump, a thermometer and stirring, stir and dissolve, then add 110g of chlorophthalic acid monosodium salt mixture (4-chlorophthalic acid Diformic acid monosodium salt 76.6%, 4,5-dichlorophthalic acid monosodium salt 13.9%...

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Abstract

The invention discloses a method for preparing 3, 3 ', 4, 4'-biphenyltetracarboxylic dianhydride. The method comprises the following steps: 1) coupling and acid precipitation: reducing a chlorinated phthalate monosodium salt mixture by a hydrazine reducing agent under the catalysis of a palladium-copper carbon supported catalyst by taking water as a solvent, carrying out a dechlorination couplingreaction to obtain 3, 3 ', 4, 4'-biphenyltetracarboxylic acid, adding filtrate after the catalyst is filtered into dilute sulfuric acid, and carrying out cooling crystallization to obtain a 3, 3 ', 4,4'-biphenyltetracarboxylic acid crude product; 2) refining: refining with a methanol aqueous solution to obtain a 3, 3 ', 4, 4'-biphenyltetracarboxylic acid refined product; and 3) anhydrous treatment: heating and dehydrating the 3, 3 ', 4, 4'-biphenyltetracarboxylic acid fine product to obtain the 3, 3 ', 4, 4'-biphenyltetracarboxylic dianhydride. The raw materials are easy to obtain, the palladium-copper carbon supported catalyst is adopted, and a proper dechlorination coupling reducing agent hydrazine sulfate is preferably selected, so that the conversion rate of the chlorinated sodium phthalate mixture reaches 100%; a proper solvent system is selected, a product is finally obtained, the content is larger than 99.7%, the yield is 81%-87%, and metal ions are smaller than 2 ppM.

Description

technical field [0001] The invention relates to a method for preparing fine chemical organic materials, in particular to a method for preparing 3,3',4,4'-biphenyltetracarboxylic dianhydride. Background technique [0002] 3,3',4,4'-biphenyltetracarboxylic acid can be dehydrated to obtain 3,3',4,4'-biphenyltetracarboxylic dianhydride, which is an important monomer of polyimide and can be used with A variety of amines are polymerized to form polyimides. Due to the rigid structure of 3,3',4,4'-biphenyltetracarboxylic dianhydride, the polyimide synthesized from it is the super heat-resistant resin with the highest heat-resistant temperature so far. Imide film and copper foil have almost the same thermal expansion coefficient, and can be well laminated with copper foil under long-term high and low temperature conditions without peeling off. It is widely used in flexible circuit boards and ultra-high-power 5G signal transmitters. Polymerized with specific amines, it can be made i...

Claims

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Application Information

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IPC IPC(8): C07C51/353C07C51/42C07C51/43C07C63/331B01J23/89C07D307/89
CPCC07C51/353C07C51/42C07C51/43B01J23/8926C07D307/89C07C63/331
Inventor 吴晓霞
Owner 河北东丽新材料有限公司
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