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Preparation method of bisphenol P

A phenol-to-mass ratio technology, applied in the field of bisphenol P preparation, can solve the problems of increased cost, excessive sewage, unfavorable environmental protection, etc., and achieve the effect of cost saving and pollution reduction

Active Publication Date: 2015-01-21
SUZHOU WUGAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method is simple and easy to operate, not only does it need to use alkali for neutralization reaction in the process, which increases the cost; it also needs to be cleaned with a large amount of water, resulting in more sewage, which is not conducive to environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0015] The preparation method of bisphenol P of the present invention comprises the following steps successively: comprises the following steps successively:

[0016] (a) Put phenol, methyl butanone, and composite catalyst into the reaction vessel in sequence, wherein the mass ratio of phenol, methyl butanone and composite catalyst is 18~25:8~10:1 and the mass of phenol exceeds that of methylbutanone Twice the mass of ketone, which is conducive to the complete reaction of methyl butanone, mix well and react at 30~40°C for 8~15 hours (at this time, bisphenol P is solid); then heat up to 60~70°C and filter while hot , to obtain filtrate and filter residue; filter residue is a composite catalyst that can be recovered and used in the next reaction. At this temperature, bisphenol P is in a liquid state, so it is dissolved in the filtrate, and phenol, methyl butanone and Composite catalysts are beneficial to inhibit the progress of side reactions, thereby increasing the yield.

[0...

Embodiment 1

[0021] The embodiment of this city provides a kind of preparation method of bisphenol P, comprises the following steps successively:

[0022] (a) Put 1200kg of phenol, 420kg of methyl ethyl ketone, and 50kg of composite catalyst into the reaction vessel in sequence, mix them evenly and react at 30°C for 15 hours, then heat up to 65°C and filter while hot to obtain filtrate and filter residue, among which the filter residue is recovered use;

[0023] (b) Evaporating the filtrate at 200 Pa and 75°C to remove phenol to obtain a crude product, wherein the phenol is recycled;

[0024] (c) Dissolving the crude product in methanol for crystallization;

[0025] (d) Mixing the product obtained in step (c) with methanol at a mass ratio of 1:2, followed by two crystallizations;

[0026] Among them, 50kg of composite catalyst is composed of 20kg of main catalyst and 30kg of sub-catalyst, 20kg of main catalyst includes 5kg of ferric chloride, 7kg of copper chloride and 8kg of alumina, an...

Embodiment 2

[0028] The embodiment of this city provides a kind of preparation method of bisphenol P, comprises the following steps successively:

[0029] (a) Put 900kg of phenol, 400kg of methyl ethyl ketone, and 50kg of composite catalyst into the reaction vessel in turn, mix them evenly, and react at 40°C for 8 hours, then heat up to 60°C and filter while hot to obtain filtrate and filter residue, of which the filter residue is recovered use;

[0030] (b) Evaporating the filtrate at 700 Pa and 90°C to remove phenol to obtain a crude product, wherein the phenol is recycled;

[0031] (c) Dissolving the crude product in ethanol for crystallization.

[0032] (d) Mixing the product obtained in step (c) with ethanol at a mass ratio of 1:4, followed by five crystallizations;

[0033] Among them, 50kg of composite catalyst is composed of 20kg of main catalyst and 30kg of sub-catalyst, 20kg of main catalyst includes 3kg of ferric chloride, 5kg of copper chloride and 12kg of alumina, and the su...

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Abstract

The invention relates to a preparation method of phenol P. The preparation method comprises the following steps: (a) sequentially putting phenol, methyl butanone and a compound catalyst into a reaction container, uniformly mixing and carrying out reaction for 8-15 hours at 30-40 DEG C, then raising temperature to 60-70 DEG C and filtering when the mixture is hot to obtain a filtrate and filter residues; (b) evaporating the filtrate under the condition of 200-700Pa and 75-90 DEG C to remove phenol so as to obtain a coarse product; and (c) dissolving the coarse product in an alcohol solvent to crystallize, wherein the mass ratio of the phenol to the methyl butanone to compound catalyst is (18-25) to (8-10) to 1. According to the preparation method of the phenol P, which is provided by the invention, on the one hand, the phenol and the methyl butanone are catalyzed by using the compound catalyst, and after reaction, no alkali liquor is required to neutralize and the catalyst can be repeatedly used, so that the cost is lowered; on the other hand, the phenol is evaporated and removed directly and is then refined and the product is not washed by water, so that the environmental pollution is favorably reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of bisphenol P. Background technique [0002] Bisphenol P, also known as 2,2-bis(4-hydroxyphenyl)-4-methylpentane or 4,4'-(1,3-dimethylbutyl)diphenol, has a chemical structure of , are very important organic chemical raw materials, as intermediates of polymer materials, they are widely used in the fields of synthetic epoxy resin, cyanate ester, polycarbonate, polyarylate and phenolic resin; as antioxidant, optical Stabilizers, plasticizers, heat stabilizers, flame retardants and widely used in the manufacture of optical discs and high-performance coatings and other fields. Research and development of new bisphenol compounds is of great significance for the manufacture, application and development of new materials. At present, the preparation method of bisphenol P generally refers to the synthesis method of bisphenol B. For example, the Chinese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/16C07C37/20
CPCC07C37/20C07C37/685C07C37/70C07C37/84C07C39/16
Inventor 计建明李东钱晨朱凤林计雄荣
Owner SUZHOU WUGAN PHARMA
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