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Preparation method of 4,4'-diamido-2,2'-dicarboxylbiphenyl

A technology of dicarboxybiphenyl and diamino, which is applied in the field of preparation of 4,4'-diamino-2,2'-dicarboxybiphenyl, can solve problems such as being unsuitable for industrial production, and achieves good product color and environmental protection. The effect of low pollution and high yield

Active Publication Date: 2014-01-22
天津众泰材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This condition is not suitable for industrial production

Method used

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  • Preparation method of 4,4'-diamido-2,2'-dicarboxylbiphenyl
  • Preparation method of 4,4'-diamido-2,2'-dicarboxylbiphenyl

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preparation example Construction

[0016] Preparation method of the present invention specifically comprises the following contents:

[0017] In step (1): 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl reacts with concentrated sulfuric acid under heating conditions to obtain 4,4'-diamino-2,2'-bis Crude carboxybiphenyl. After the reaction was complete, the reaction solution was poured into ice water, and after cooling down, sodium hydroxide was added to adjust the pH to 3-4, stirred, and then filtered to obtain the crude product. The molar ratio is 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl:concentrated sulfuric acid=1:(5.2~9.2), the preferred ratio is: 4,4'-diamino-2,2 '-bistrifluoromethylbiphenyl:concentrated sulfuric acid=1:7.2. The reaction temperature ranges from 110°C to 130°C, preferably 120°C.

[0018] In the step (2): 4,4'-diamino-2,2'-dicarboxybiphenyl is obtained by recrystallization in a polar solvent under reflux conditions. The polar solvent is methanol or ethanol; the molar ratio is: 4,4'-diam...

Embodiment 1

[0021] Add 1.35 kg of concentrated sulfuric acid to the reaction flask, and add 0.6 kg of 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl in batches (the molar ratio is: 4,4'-diamino-2, 2'-bistrifluoromethylbiphenyl:concentrated sulfuric acid=1:7.2), after the addition, the temperature was raised to 110°C for 7 hours, and after the reaction was completed, it was cooled to room temperature. Pour the reaction solution into 3 kg of ice water, lower the temperature to below 10°C, add sodium hydroxide to adjust the pH to 3-4, stir for 1 hour and filter to obtain 4,4'-diamino-2,2'-dicarboxy The crude product of biphenyl is 0.36 kg, gray solid, and the crude product yield is 70.5%. The reaction structure is as follows:

[0022]

Embodiment 2

[0024] Add 1.13 kg of concentrated sulfuric acid to the reaction flask, and add 0.6 kg of 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl in batches (the molar ratio is: 4,4'-diamino-2, 2'-bistrifluoromethylbiphenyl:concentrated sulfuric acid=1:6.2), after the addition, the temperature was raised to 120°C for 7 hours, and after the reaction was completed, it was cooled to room temperature. Pour the reaction solution into 2.5 kg of ice water, lower the temperature to below 10°C, add sodium hydroxide to adjust the pH to 3-4, stir for 1 hour and filter to obtain 4,4'-diamino-2,2'-dicarboxy The crude product of biphenyl was 0.38 kg, gray solid, and the crude product yield was 74.5%.

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Abstract

The invention relates to a preparation method of 4,4'-diamido-2,2'-dicarboxylbiphenyl, which comprises the following steps: reacting 4,4'-diamido-2,2'-bis-trifluoromethylbiphenyl used as a raw material with concentrated sulfuric acid under heating conditions to obtain a crude product; and recrystallizing under the polar solvent reflux conditions to obtain the 4,4'-diamido-2,2'-dicarboxylbiphenyl pure product. The method has the advantages of high yield, simple technological operation, favorable product color, small environmental pollution, accessible reactor and the like.

Description

technical field [0001] The present invention relates to a preparation method of 4,4'-diamino-2,2'-dicarboxybiphenyl which can be used as an important monomer raw material for synthesizing polyimide, 4,4'-diamino-2, 2'-Dicarboxybiphenyl can also be used as an intermediate of pesticides and medicines. Background technique [0002] 4,4'-diamino-2,2'-dicarboxybiphenyl is an important monomer raw material for the synthesis of polyimide, and it can also be used to synthesize polyimide containing heterocyclic groups such as imidazole and having good solubility Amines, this type of polyimide has good heat resistance, and can prepare excellent polyimide films. 4,4'-diamino-2,2'-dicarboxybiphenyl is widely used in liquid crystal displays, heat-resistant resins, engineering plastics, light-emitting devices, pesticides, pharmaceutical intermediates, etc. [0003] The preparation method of 4,4'-diamino-2,2'-dicarboxybiphenyl is currently: (1) Using 2,2'-dicarboxybiphenyl as raw materia...

Claims

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Application Information

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IPC IPC(8): C07C227/02C07C229/60
Inventor 尚振华栗晓东
Owner 天津众泰材料科技有限公司
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