Method for preparing 4,4'-dihydroxydiphenylmethane

A technology of dihydroxydiphenylmethane and organic solvents, which is applied in the field of preparation of 4,4'-dihydroxydiphenylmethane, can solve the problems of cumbersome separation and purification, and achieve low production cost, cost reduction and simple purification process Effect

Inactive Publication Date: 2011-09-28
HEBEI JIANXIN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for preparing 4,4'-dihydroxydiphenylmethane with simple operation

Method used

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  • Method for preparing 4,4'-dihydroxydiphenylmethane
  • Method for preparing 4,4'-dihydroxydiphenylmethane
  • Method for preparing 4,4'-dihydroxydiphenylmethane

Examples

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Effect test

Embodiment 1

[0028] ①Add 140g of water and 180g of concentrated sulfuric acid (mass concentration 98%) into a 500mL reaction bottle to make a sulfuric acid solution with a mass concentration of 56%, then add 39.6g of MDA, and raise the temperature to 50°C to dissolve all MDA solids. Then cool to 5°C and continue to stir for 0.5h, then slowly add 29.0 g of sodium nitrite, and keep it warm at 5°C until the starch-potassium iodide test paper just turns blue as the end point of the reaction, and a light yellow hydrogen sulfate diazonium salt solution is obtained.

[0029] ②Add 120g of toluene and 20g of copper nitrate into a 1000mL reaction flask, stir and heat to about 70°C, then add dropwise the hydrogen sulfate diazonium salt solution obtained in step ① into the 1000mL reaction flask, and keep the temperature of the solution in the reaction flask during the dropping process At 70~80°C, continue to react for 2 hours after the dropwise addition is completed. The water phase was separated, and...

Embodiment 2

[0039]① Add 100g of water and 180g of concentrated sulfuric acid (mass concentration 98%) to a 500mL reaction bottle to prepare a sulfuric acid solution, then add 39.6g of MDA, heat up to 55°C to dissolve all the solids; then cool to -10°C, and continue to stir for 0.5 h, then slowly add 29.0 g of sodium nitrite, and keep warm at -10°C until the starch-potassium iodide test paper just turns blue as the end point of the reaction to obtain a light yellow hydrogen sulfate diazonium salt solution.

[0040] ② Add 100g of water and 20g of zinc sulfate to a 1000mL reaction bottle, stir and heat to about 90°C, then add the above-mentioned hydrogen sulfate diazonium salt solution dropwise, keep the temperature of the aqueous solution in the reaction bottle at 85~95°C during the dropwise addition, add dropwise After completion, continue to react for 2 hours; then extract twice with 150g chloroform, separate the water phase, wash the organic phase with water to weak acidity (pH=5~7), then...

Embodiment 3

[0044] ① Add 150g of water and 100g of concentrated sulfuric acid (mass concentration 98%) to a 500mL reaction bottle to make a sulfuric acid solution, then add 39.6g of MDA, heat up to 60°C to dissolve all the solids; then cool to 10°C, continue stirring for 0.5h, Then slowly add 29.0 grams of sodium nitrite, keep warm and react until the starch-potassium iodide test paper just turns blue as the reaction end point to obtain light yellow hydrogen sulfate diazonium salt solution.

[0045] ②Add 120g of 2-pentanone and 30g of alumina into a 1000mL reaction flask, stir and heat to about 50°C, add dropwise the hydrogen sulfate diazonium salt solution obtained in step ①, and keep the temperature of the solution in the reaction flask at 40~ 50°C, after the dropwise addition was completed, the reaction was continued for 2h. Separate the water phase, wash the oil phase with water to weak acidity (pH=6~7), and recover 2-pentanone by distillation under reduced pressure. The residue is cr...

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Abstract

The invention discloses a method for preparing 4,4'-dihydroxydiphenylmethane (BPF), which comprises the following steps of: diazotizing 4,4'-diaminodiphenyl-methane (MDA) and sodium nitrite serving as raw materials, hydrolyzing, refining and the like to synthesize the 4,4'-dihydroxydiphenylmethane with the purity of over 98.5 percent. The raw materials are low-cost, the operation process is simple, and industrial production is easy to realize; and a mixture of three isomers of dihydroxydiphenylmethane does not exist in the product, the product is easy to purify, and cost for complicated separation and purification is reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of 4,4'-dihydroxydiphenylmethane. Background technique [0002] 4,4'-Dihydroxydiphenylmethane (BPF), also known as bisphenol F, is mainly used in electronic-grade epoxy resins, high-performance polyester resins and polycarbonate products, and PC made from bisphenol F The resin is easily soluble in low-boiling organic solvents, with low softening point and good processability, and its heat resistance and mechanical properties are significantly improved compared with bisphenol A PC resin. For example, the melting temperature of bisphenol F PC resin is 300°C , 70°C higher than bisphenol-A PC resin, and it has stretchability when subjected to very large damage. Therefore, it has better overall performance than bisphenol A PC resin, and is suitable for manufacturing molding materials or films. [0003] The traditional preparation method of 4,4...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/045
Inventor 姚建文郭永利于德乾李宝森朱守琛
Owner HEBEI JIANXIN CHEM IND CO LTD
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