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Compound protonic acid promoted by Lewis acid and catalytic application of compound protonic acid

A protonic acid and catalyst technology, which is applied in the field of compound protonic acid and its catalytic application, can solve the problems of low selectivity of 4,4-dihydroxydiphenylmethane, low catalytic activity of bisphenol F, etc., and achieve effective synthesis effect , high selectivity and strong catalytic efficiency

Active Publication Date: 2021-07-13
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, there are still problems of low catalytic activity and low selectivity of bisphenol F and 4,4-dihydroxydiphenylmethane in the synthesis process of bisphenol F.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Catalyzing the reaction of phenol and formaldehyde to synthesize bisphenol F

[0030] First add 10g of phenol into a four-necked bottle, add 50mL of toluene as a solvent, heat until it is completely dissolved, and keep stirring at a constant speed, start to add 20mL of 85% phosphoric acid, 1.5g of lithium fluoride, 1mL of perchloric acid, 0.8g of Tris Potassium fluoromethanesulfonate was mixed together and stirred for 0.3h into the four-necked flask, and then 1.5g of formaldehyde was added dropwise into the four-necked flask. Keep the temperature of the reaction mixture at 55°C and react for 6 hours. After the reaction, add sodium bicarbonate until the pH of the reaction solution is 5-6, and collect the organic phase. Rotate the obtained crude product to recover the solvent, and distill under reduced pressure to recover the remaining unreacted For phenol, after the distillation, recrystallize the remaining product recovery solvent to obtain pure white leafy c...

Embodiment 2

[0032] Embodiment 2: Catalyzing the reaction of phenol and formaldehyde to synthesize bisphenol F

[0033] First add 10g of phenol into a four-neck flask, add 50mL of toluene as a solvent, heat until it is completely dissolved, and keep stirring at a constant speed, start adding 25mL of 85% phosphoric acid, 2g of lithium fluoride, 1mL of perchloric acid, 0.8g of trifluoro Potassium methanesulfonate was mixed together and stirred for 0.5h into the four-necked flask, and then 1.5g of formaldehyde was added dropwise into the four-necked flask. Keep the temperature of the reaction mixture at 60°C and react for 6 hours. After the reaction, add sodium bicarbonate until the pH of the reaction solution is 5-6, and collect the organic phase. Rotate the obtained crude product to recover the solvent, and distill under reduced pressure to recover the unreacted residue. For phenol, after the distillation, recrystallize the remaining product recovery solvent to obtain pure white leafy cryst...

Embodiment 3

[0035] Embodiment 3: catalytic phenol and formaldehyde reaction synthesis bisphenol F

[0036]First add 10g of phenol into a four-neck flask, add 50mL of toluene as a solvent, heat until it is completely dissolved, and keep stirring at a constant speed, start adding 30mL of 85% phosphoric acid, 2g of lithium fluoride, 1.5mL of perchloric acid, 1g of trifluoro Potassium methanesulfonate was mixed together and stirred for 0.5h into the four-necked flask, and then 1g of formaldehyde was added dropwise into the four-necked flask. Keep the temperature of the reaction mixture at 60°C and react for 6 hours. After the reaction, add sodium bicarbonate until the pH of the reaction solution is 5-6, and collect the organic phase. Rotate the obtained crude product to recover the solvent, and distill under reduced pressure to recover the unreacted residue. For phenol, after the distillation, recrystallize the remaining product recovery solvent to obtain pure white leafy crystals as bispheno...

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PUM

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Abstract

The invention discloses compound protonic acid promoted by Lewis acid and a catalytic application of the compound protonic acid, and belongs to the field of chemical materials and industry. Aiming at the defects of a traditional bisphenol F synthesis method, the invention provides the compound catalyst prepared from phosphoric acid, lithium fluoride, perchloric acid and potassium trifluoromethanesulfonate in a mass ratio of (30-60):(1-5):(1-3):1. According to the invention, the catalyst is used in the bisphenol F synthesis reaction, so that the good catalysis effect is achieved, the high conversion rate and the high selectivity are provided, and the selectivity on the 4,4-dihydroxydiphenylmethane is high. Meanwhile, the catalytic system can also be used for synthesis of bisphenol A, and has a particularly effective synthesis effect on an important industrial product n-butyl acetate in the industry.

Description

technical field [0001] The invention relates to a compound protonic acid promoted by Lewis acid and its catalytic application, which belongs to the field of chemical materials and industry. Background technique [0002] The chemical name of bisphenol F is dihydroxydiphenylmethane. At present, the industrial production of bisphenol F generally uses phenol and formaldehyde as raw materials, and is obtained through condensation reaction in the presence of an acidic catalyst. Mainly composed of three isomers of dihydroxydiphenylmethane, it is mainly used as low-viscosity epoxy resin, special polyester raw material and information recording paper additive. Among them, 4,4-dihydroxydiphenylmethane has the best performance, which can be used as a raw material for polycarbonate (PC) resin, but the process of synthesizing 4,4-dihydroxydiphenylmethane alone has not been studied so far. [0003] Catalyst selection is one of the important process conditions in the bisphenol F synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26B01J31/02B01J27/16B01J27/12C07C37/20C07C39/16C07C67/08C07C69/14
CPCB01J31/26B01J31/0225B01J27/16B01J27/12C07C37/20C07C67/08B01J2231/49C07C39/16C07C69/14Y02P20/584
Inventor 王大伟常绍泽李家豪胡昕宇
Owner JIANGNAN UNIV
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