Check patentability & draft patents in minutes with Patsnap Eureka AI!

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
View PDF3 Cites 11 Cited by
  • 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 and high purity. There are three kinds of isomers in the product obtained by the preparation method, which require cumbersome separation and purification

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing 4,4'-dihydroxydiphenylmethane
  • Method for preparing 4,4'-dihydroxydiphenylmethane
  • Method for preparing 4,4'-dihydroxydiphenylmethane

Examples

Experimental program
Comparison scheme
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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com