Method for preparing 4, 4'-diphenyl ether dicarboxylic acid
A technology of diphenyl ether dicarboxylic acid and dimethyl diphenyl ether, which is applied in the field of preparing 4,4'-diphenyl ether dicarboxylic acid, can solve the problems of long reaction time, cumbersome operation, high cost, etc., and achieve less catalyst consumption , post-processing is simple, the effect of cost reduction
Image
Examples
Embodiment 1）
[0024] This example is the preparation of 4,4'-diphenyl ether dicarboxylic acid by the normal pressure method (the reaction vessel is connected to the atmosphere during the reaction), which has the following steps:
[0025] ①Add 12g of the reactant 4,4'-dimethyldiphenyl ether, 1g of the catalyst cobalt acetate tetrahydrate, 0.75g of the catalyst manganese acetate, and 0.6g of the oxidation additive sodium bromide into a 100mL reaction flask, and then 50 g of organic acid propionic acid was added as a solvent.
[0026] ②By bubbling, quickly pass excess oxygen into the reaction device below the liquid level, and heat to 120°C to carry out the oxidation reaction of 4,4'-diphenyl ether dicarboxylic acid for 4 hours until a large amount of white solids are precipitated.
[0027] ③ Cool the material after the oxidation reaction to 20°C, then filter it with suction, then wash it twice with propionic acid, then wash it with water three times, and finally dry it in vacuum to obtain 14g...
Embodiment 2～ Embodiment 5）
[0029] The preparation method of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.
[0030]
[0031]
Embodiment 6）
[0033] This example is the preparation of 4,4'-diphenyl ether dicarboxylic acid by the high-pressure method (the reaction vessel is in a closed state during the reaction), which has the following steps:
[0034] ①Add 6g of the reactant 4,4'-dimethyldiphenyl ether, 0.17g of the catalyst cobalt acetate tetrahydrate, 0.11g of the catalyst manganese acetate, and 0.32g of the oxidation additive sodium bromide into a 100mL autoclave, Then 30 g of the organic acid glacial acetic acid was added as a solvent.
[0035] ②Introduce excess oxygen into the autoclave and pressurize to 1.0MPa to generate 4,4'-diphenyl ether dicarboxylic acid oxidation reaction, while stirring and heating to 135°C, the pressure in the autoclave immediately drops rapidly, when the pressure When it drops to 0.5MPa, re-introduce oxygen and pressurize to 1.0MPa, repeat this cycle 2 to 4 times until the pressure in the autoclave is maintained for 1 hour and no longer drops.
[0036] ③ Cool the material after the o...
PUM
Login to View More Abstract
Description
Claims
Application Information
- IPC
- C07C65/24; C07C51/265
- Inventors
- 胡国宜; 丁志伟