Method for preparing 3,3',4,4'-benzophenone tetracarboxylic acid by liquid phase air oxidation process
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A technology of benzophenone tetracarboxylic acid and air oxidation, which is applied in 3 fields, can solve the problems of difficult feeding, low purity, and low yield, and achieve the effects of reducing reaction time, increasing reaction yield, and improving purity
Inactive Publication Date: 2009-12-09
HEILONGJIANG INST OF PETROCHEM
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[0004] The purpose of the present invention is to solve the problems of using a highly toxic purification solvent, difficulty in addition, low purity and low yield in the process of preparing 3,3',4,4'-benzophenone tetracarboxylic acid in the prior art, and provide A method for preparing 3,3',4,4'-benzophenone tetracarboxylic acid
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specific Embodiment approach 1
[0007] Specific embodiment one: the preparation of 3,3',4,4'-benzophenone tetracarboxylic acid by the liquid phase air oxidation method in this embodiment is carried out according to the following steps: 1. 1 mole of 3,3',4, 4'-Tetramethyldiphenylethane, 15-35 moles of glacial acetic acid, 0.01-0.05 moles of cobalt acetate tetrahydrate, 0.001-0.1 moles of manganese acetate tetrahydrate and 0.005-0.08 moles of tetrabromoethane are mixed, heated and dissolved to obtain Mixed solution; 2. Add the mixed solution obtained in step 1 to the reaction kettle, 3 Air flow rate per hour, pressurize to 1.5-2.0MPa, and stir at 150-180°C for 60-90min, then pressurize to 2.0-3.0MPa, continue stirring for 60-90min, then release the pressure, discharge and cool and centrifugation to obtain 3,3',4,4'-benzophenone tetracarboxylic acid.
specific Embodiment approach 2
[0008] Specific embodiment two: The difference between this embodiment and specific embodiment one is that in step one, 1 mole of 3,3',4,4'-tetramethyldiphenylethane, 25 moles of glacial acetic acid, 0.03 mole of tetramethyldiphenylethane Cobalt acetate water, 0.05 mole manganese acetate tetrahydrate and 0.04 mole tetrabromoethane were mixed. Other steps and parameters are the same as those in Embodiment 1.
specific Embodiment approach 3
[0009] Embodiment 3: The difference between this embodiment and Embodiment 1 is that the purity of 3,3',4,4'-tetramethyldiphenylethane in Step 1 is 99.0-99.8%. Other steps and parameters are the same as those in Embodiment 1.
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Abstract
A method for preparing 3,3',4,4'-benzophenone tetracarboxylic acid by liquid-phase air oxidation method, which relates to a preparation method of 3,3',4,4'-benzophenone tetracarboxylic acid . It solves the problems of using a highly toxic purification solvent, difficulty in adding materials, low purity and low yield in the process of preparing 3,3',4,4'-benzophenone tetracarboxylic acid in the prior art. The method step is to mix 3,3',4,4'-tetramethyldiphenylethane, glacial acetic acid, cobalt acetate tetrahydrate, manganese acetate tetrahydrate and tetrabromoethane in molar ratio, dissolve and add to the reaction In the kettle, react under the conditions of pressurization, heating and stirring, and then release the pressure, discharge, cool and centrifuge to obtain 3,3',4,4'-benzophenone tetracarboxylic acid. The preparation process of the invention is a weight gain reaction, the product yield is as high as 100-140%, and the product purity is 97.5-99.8%.
Description
technical field [0001] The invention relates to a preparation method of 3,3',4,4'-benzophenone tetracarboxylic acid. Background technique [0002] In the past ten years, due to the needs of science and technology and the development of the national economy, synthetic materials with various characteristics such as high temperature resistance, corrosion resistance, and good insulation performance are required, among which polyimide is the most important one in this material. , 3,3',4,4'-benzophenone tetracarboxylic acid is widely used in the field of polyimide, and can be used to prepare special synthetic materials. Polyimide prepared from 3,3',4,4'-benzophenone tetracarboxylic acid has good processability, it can be made into film, laminate, coating, adhesive, insulating material and Reinforcement materials, etc.; its products have excellent thermal stability, outstanding insulation and mechanical properties. [0003] At present, the preparation of 3,3',4,4'-benzophenone te...
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