Method for preparing 3,3',4,4'-benzophenone tetra carboxylic 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: 2008-05-14
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, pressurize to 1.5-2.0MPa with an air flow rate of 0.5-1.0m3 / h, and stir at 150-180°C for 60-90min, then Pressurize to 2.0-3.0 MPa, continue to stir for 60-90 minutes, then release the pressure, discharge, cool and centrifuge 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
The invention relates to a liquidoid air oxidation method for preparing 3, 3', 4, 4'-benzophenone tetrabasic carboxylic acid and a preparation method for 3, 3', 4, 4'-benzophenone tetrabasic carboxylic acid. The invention can solve the problems of the prior art such as adoption of toxic purification solvent, difficulty in feeding, low purity and low yield during the process of preparing 3, 3', 4, 4'-benzophenone tetrabasic carboxylic acid. The procedures are as follows: the 3, 3', 4, 4'-tetramethyl hexichol ethane, glacial acetic acid, tetrahydrate cobalt acetate, tetrahydrate manganese acetate and tetrabromoethane are mixed and dissolved according to the mol ratio, and then is arranged into a reaction kettle so as to react under the conditions of pressurizing, heating and stirring, and then the 3, 3', 4, 4'-benzophenone tetrabasic carboxylic acid is obtained through pressure relief, discharge, cooling and centrifugation. The invention has the advantages that: the preparation process of the invention is a weight increment reaction, thereby the yield of the product reaches 100 percent to 140 percent, and the purity of the product can reach 97.5 percent to 99.8 percent.
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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