Method for preparing biphenyltetracarboxylic dianhydride (BPDA)

A technology of biphenyl dianhydride and tetramethylbiphenyl, which is applied in the field of biphenyl dianhydride preparation and can solve problems such as high cost and environmental pollution

Inactive Publication Date: 2012-01-25
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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Problems solved by technology

[0004] Yet the preparation method of biphenyl dianhydride of above-mentioned report all uses potassium permanganate or

Method used

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  • Method for preparing biphenyltetracarboxylic dianhydride (BPDA)
  • Method for preparing biphenyltetracarboxylic dianhydride (BPDA)
  • Method for preparing biphenyltetracarboxylic dianhydride (BPDA)

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[0023] The invention discloses a preparation method of biphenyl dianhydride, comprising the following steps:

[0024] Using acetic acid as a solvent, a cobalt source compound as a catalyst, and a bromine source compound as a cocatalyst, reacting tetramethylbiphenyl with a gas containing molecular oxygen to obtain biphenyltetracarboxylic acid;

[0025] The biphenyl tetracarboxylic acid is dehydrated to obtain biphenyl dianhydride.

[0026] In the present invention, the cobalt source compound is preferably cobalt acetate and its hydrate, cobalt naphthenate and its hydrate, cobalt sulfate and its hydrate, cobalt acetylacetonate and its hydrate, cobalt benzoylacetonate and its hydrate Cobalt bromide and its hydrate, cobalt carbonate and its hydrate, cobalt chloride and its hydrate, cobalt fluoride and its hydrate, cobalt nitrate and its hydrate, cobalt stearate and its hydrate One or more, more preferably cobalt acetate. The bromine source compound is preferably bromine, hydroge...

Embodiment 1

[0054] At room temperature, add 0.5mol 4-chloro-o-xylene (70.3g), 0.025mol nickel bromide (5.46g), 0.05mol triphenylphosphine (13.1g), 0.6mol zinc powder (39.2 g), 0.025mol 2,2'-bipyridine (3.90g) and 150ml dimethylacetamide were reacted at 70° C. for 6 hours, then added toluene, filtered to remove solid residue, and after the toluene layer was washed twice, Concentrate to remove the solvent, slowly add methanol to the solvent-removed substance, and let it stand for 24 hours to obtain a white solid; filter the white solid and dry it in vacuo to obtain 44.6 g of 3,4,3',4'-tetramethyl Base biphenyl, the yield is 85%.

[0055] Add 0.1mol 3,4,3',4'-tetramethylbiphenyl (21.03g), 0.001mol cobalt acetate (0.177g), 0.0005mol sodium bromide (0.051g) and 100g acetic acid, in described reaction vessel, feed air, make pressure in the vessel remain on 0.5MPa;

[0056] Heat the reaction vessel so that the temperature in the reaction vessel reaches 100°C, and continue the reaction for 6 ho...

Embodiment 2

[0059] At room temperature, add 0.25mol 3-chloro-o-xylene (35.15g), 0.25mol 4-chloro-o-xylene (35.15g), 0.025mol nickel bromide (5.46g), 0.05mol tris Phenylphosphine (13.1g), 0.6mol zinc powder (39.2g), 0.025mol 2,2'-bipyridine (3.90g) and 150ml dimethylacetamide were reacted at 70°C for 6 hours, then added toluene, filtered Remove the solid residue, wash the toluene layer twice with water, concentrate to remove the solvent, slowly add methanol to the solvent-removed substance, and let it stand for 24 hours to obtain a white solid; filter the white solid and recrystallize it with methanol 30.55 g of 2,3,3',4'-tetramethylbiphenyl was obtained with a yield of 58.2%.

[0060] Add 0.1mol 2,3,3',4'-tetramethylbiphenyl (21.03g), 0.001mol cobalt acetate (0.177g), 0.0005mol sodium bromide (0.051g) and 100g Acetic acid, feeds air into described reaction vessel, makes pressure in the vessel remain on 0.5MPa;

[0061] The reaction vessel was heated so that the temperature in the reacti...

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Abstract

The invention discloses a method for preparing biphenyltetracarboxylic dianhydride (BPDA). The method comprises the following steps: carrying out a reaction on tetramethyl biphenyls and gases containing molecular oxygen to obtain biphenyltetracarboxylic acid by taking acetic acid as a solvent, cobalt source compounds as catalysts and a bromine source compound as a promoter; and then carrying out dehydration on biphenyltetracarboxylic acid to obtain BPDA. Under the catalytic actions of the cobalt source compounds and the bromine source compound, the gases containing molecular oxygen are used as oxidants, tetramethyl biphenyls and the gases containing molecular oxygen are subjected to an oxidation reaction and BPDA is obtained after dehydration. Compared with the prior art, the method has the following beneficial effects: the gases containing molecular oxygen are used as oxidants; the oxidants have low cost and are environmentally-friendly; therefore the environment is protected while the cost is lowered; and the experimental results show that BPDA is obtained by the preparation method.

Description

technical field [0001] The invention relates to the technical field of biphenyl dianhydride, more specifically, to a preparation method of biphenyl dianhydride. Background technique [0002] Biphenyl dianhydride (BPDA), also known as biphenyl dianhydride, has three isomers, namely 3, 4, 3', 4'-biphenyl dianhydride (s-BPDA), 2, 3, 2',3'-biphenyltetraacid dianhydride (i-BPDA) and 2,3,3',4'-biphenyltetraacid dianhydride (a-BPDA). Biphenyldianhydride (BPDA) is an important monomer for the synthesis of polyimide, a heat-resistant polymer material, and can be polymerized with various substances to prepare polyimide. Polyimide has superior comprehensive performance in the polymer materials that have been industrialized at present. Has been widely used. Therefore, as an important monomer of high-performance polyimide, biphenyl dianhydride has attracted extensive attention at home and abroad for its synthesis and application. [0003] Biphenyldianhydride is generally obtained by ...

Claims

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Application Information

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IPC IPC(8): C07D307/89B01J27/128
Inventor 郭海泉姚海波邱雪鹏高连勋杜志军高鑫康传清
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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