High-selectivity catalytic synthesis method for 4, 4'-bisphenol F

A high-selectivity, catalyst technology, used in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc. To achieve the effect of improving acidity and steric hindrance, good stability and good catalytic activity

Inactive Publication Date: 2015-11-04
XIANGTAN UNIV
View PDF9 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalytic yield of inorganic acid is high, but it is severely corrosive to equipment and has many side reactions; the catalytic reaction condition of organic acid is mild, and it is less corrosive to equipment, but it has many side reactions, high phenolic ratio and low yield
Patent JP11269113 and patent CN101987812A respectively reported the method of catalyzing the synthesis of bisphenol F by zeolite molecular sieve and mesoporous molecular sieve. This kind of method is convenient for catalyst separation and recovery, but the phenol-formaldehyde ratio and reaction temperature are high, and the catalyst is easy to block pores and deactivate

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
  • High-selectivity catalytic synthesis method for 4, 4'-bisphenol F
  • High-selectivity catalytic synthesis method for 4, 4'-bisphenol F
  • High-selectivity catalytic synthesis method for 4, 4'-bisphenol F

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation of ionic liquid catalyst N,N-bis(4-mercapto)butyl-N,N,N,N-tetramethyl-1,3-propanediammonium dihydrogensulfate

[0020] The first step: 86.4 grams of 1,4 dibromobutane and 40 grams of tetrahydrofuran are mixed and dissolved to form solution A, and 13 grams of N,N,N,N-tetramethyl-1,3-propanediamine and 50 grams of methanol Mix and dissolve to form solution B. Slowly add solution B to solution A under stirring, react at 0°C for 3 hours, then raise the temperature to 25°C and continue to react for 24 hours. After the reaction, tetrahydrofuran and methanol are evaporated by fractional distillation, and extracted with water , the water phase is evaporated to obtain the first step reaction product, and the organic phase is excess 1,4-dibromobutane, which is directly recycled and used;

[0021] The second step: mix and dissolve 15.3 grams of thiourea and 75 grams of ethanol to form solution C, mix and dissolve 51 grams of the reaction product of the first step a...

Embodiment 2

[0030] Similar to Example 1, the difference is only that the mol ratio of phenol to ionic liquid to formaldehyde is 10:1:1 in the process of synthesizing bisphenol F, and all the other processes are the same, and the yield of bisphenol F obtained is 80%, 4 , 4'-bisphenol F selectivity was 62%.

Embodiment 3

[0032] Similar to Example 1, the difference is only that the molar ratio of phenol to ionic liquid to formaldehyde is 4:1:1 in the process of synthesizing bisphenol F, and all the other processes are the same, and the yield of bisphenol F obtained is 51%, 4, 4'-Bisphenol F selectivity was 58%.

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 high-selectivity catalytic synthesis method for 4, 4'-bisphenol F. Ionic liquid N, N-bi(4-sulfydryl) butyl-N, N, N, N-tetramethyl-1, 3-propane diammonium sulfate hydrogen sesquisulfate is used as a catalyst; phenol and formaldehyde are used as raw materials; the 4, 4'-bisphenol F is obtained through high-selectivity catalytic synthesis via condensation reaction. The adopted ion liquid catalyst of N, N-bi(4- sulfydryl) butyl-N, N, N, N- tetramethyl-1, 3-propane diammonium sulfate hydrogen sesquisulfate uses N, N, N, N-tetramethyl-1, 3- propane diamine, 1, 4- dibromobutane and thiourea as raw materials; firstly, butyl bromide is introduced onto diamine through nucleophilic substitution reaction; then, isothiuronium salts are generated through the reaction between thiourea and butyl bromide; sodium hydroxide is used for hydrolyzing the isothiuronium salts to obtain hydrosulfuryl salts; dilute hydrochloric acid acidification is carried out to obtain hydrosulphonyl; finally, concentrated sulfuric acid is used for replacing negative ions into bisulfate ions. When the catalyst is used for bisphenol F catalytic synthesis, the selectivity of the 4, 4'-bisphenol F is greatly improved.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing 4,4'-bisphenol F with high selectivity. Background technique [0002] Bisphenol F is a bisphenol compound produced by the condensation reaction of phenol and formaldehyde under the action of a catalyst. Its chemical name is dihydroxydiphenylmethane, and it has 4,4'-, 2,4'-, 2 , 2′-three isomers, wherein the isomer with the best performance is the para-position 4,4′-bisphenol F, and the chemical structural formulas of their three isomers are as follows: [0003] [0004] Bisphenol F is an important chemical intermediate. When synthesizing epoxy resin, polyester resin, polycarbon resin and phenolic resin, the heat and humidity resistance, insulation and processing injection molding performance of the obtained product are better than those of the previous products. Similar products made of bisphenol A as raw material have great development and application space. [0005] The catalysts f...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/16C07C37/20B01J31/02
CPCY02P20/52
Inventor 刘跃进王庆吴志民李勇飞何志成王丹凤
Owner XIANGTAN UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products