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Method for preparing 4, 4'-dihydroxyl diphenyl sulfone

A technology of dihydroxydiphenyl sulfone and phenol, applied in the field of organic intermediate preparation, can solve the problems of difficult preparation of catalyst isophthalic acid, high price, etc., and achieves favorable dehydration reaction, high reaction temperature and high yield. Effect

Active Publication Date: 2013-02-27
KEMAI CHEM
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0014] In order to overcome the problem that in the BPS production process obtained by the sulfonation of phenol and concentrated sulfuric acid and high-temperature dehydration, it is difficult to prepare and expensive using the catalyst m-benzenedisulfonic acid, the present invention uses a cheaper, easy-to-obtain, and easy-to-preserve catalyst

Method used

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  • Method for preparing 4, 4'-dihydroxyl diphenyl sulfone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The material ratio is as follows:

[0028] The mass ratio of phenol to concentrated sulfuric acid is 1.93:1

[0029] The mass ratio of solvent to concentrated sulfuric acid is 2.07:1;

[0030] The mass ratio of catalyst 2,6-naphthalene disulfonic acid to concentrated sulfuric acid is 0.098:1

[0031] Add 106g of mesitylene and durene mixed solvent (the mass ratio of mesitylene to durene is 3:1) and 98.5g of phenol And catalyst 2,6-naphthalene disulfonic acid 5g. Stir the materials, and slowly add 51.1 g of concentrated sulfuric acid (concentration 98%) dropwise to the four-necked bottle, and the temperature reaches 110°C at the same time as the concentrated sulfuric acid is added dropwise in 2 hours. After the concentrated sulfuric acid was added dropwise, continue to heat up to the reflux temperature of 174° C., and maintain the reflux reaction temperature. The duration of this process is 8 hours. The reaction was considered complete after anhydrous evolution. Coo...

Embodiment 2

[0033] The material ratio is as follows:

[0034] The mass ratio of phenol to concentrated sulfuric acid is 1.89:1

[0035] The mass ratio of solvent to concentrated sulfuric acid is 1.85:1;

[0036] The mass ratio of catalyst 2,6-naphthalene disulfonic acid to concentrated sulfuric acid is 0.03:1

[0037] Add 94.5 g of mesitylene and durene mixed solvent (the mass ratio of mesitylene to durene is 4:1), phenol 96.6 g and 1.53 g of catalyst 2,6-naphthalene disulfonic acid. Stir the materials, and slowly add 51.1 g of concentrated sulfuric acid (concentration 98%) dropwise to the four-necked bottle, and it takes 2 hours for the concentrated sulfuric acid to be added dropwise. While adding concentrated sulfuric acid dropwise, start heating to 110°C, which also takes 2 hours. After the concentrated sulfuric acid was added dropwise, continue to heat up to the reflux temperature (172°C), and maintain the reflux reaction temperature. The duration of this process is 10h. The reac...

Embodiment 3

[0039] The material ratio is as follows:

[0040] The mass ratio of phenol to concentrated sulfuric acid is 2.03:1

[0041] The mass ratio of solvent to concentrated sulfuric acid is 2.48:1;

[0042] The mass ratio of catalyst 2,6-naphthalene disulfonic acid to concentrated sulfuric acid is 0.15:1

[0043] Add 126.7 g of mesitylene and durene mixed solvent (the mass ratio of mesitylene to durene is 2.8:1), phenol 103.7 g in a 500 mL four-neck flask equipped with reflux separator, thermometer and stirrer. g and 7.67 g of catalyst 2,6-naphthalene disulfonic acid. Stir the materials, and slowly add 51.1 g of concentrated sulfuric acid (concentration 98%) dropwise to the four-necked bottle, and it takes 2 hours for the concentrated sulfuric acid to be added dropwise. While adding concentrated sulfuric acid dropwise, start heating to 110°C, which also takes 2 hours. After the concentrated sulfuric acid was added dropwise, continue to heat up to the reflux temperature (175°C), a...

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Abstract

The invention provides a method for preparing 4, 4'-dihydroxyl diphenyl sulfone. The method comprises the following steps: adding 2,6-naphthalene disulfonic acid in a mixed solvent of mesitylene and durene, and then preparing the 4, 4'-dihydroxyl diphenyl sulfone by sulfonation and dehydration reaction between phenol and concentrated sulfuric acid, wherein the 2,6-naphthalene disulfonic acid is a by-product separated from the production of 2,7-naphthalene disulfonic acid, low in price and rich in source; the mass ratio of the 2,6-naphthalene disulfonic acid to the concentrated sulfuric acid (density of 98%) is (0.03-0.15):1; the mass ratio of the solvent to the concentrated sulfuric acid is (1.85-2.48):1; the mass ratio of the phenol to the concentrated sulfuric acid is (1.89-2.03):1; in the solvent, the mass ratio of the mesitylene to durene is (2.8-4):1; and the time of reflux dehydration reaction is 6-10h. The material of the method is excellent in suspension, high in reaction temperature and beneficial to dehydration reaction and the yield of 4, 4'-dihydroxyl diphenyl sulfone is high.

Description

technical field [0001] The technology of the invention belongs to the field of preparation of organic intermediates, and particularly proposes a preparation method of 4,4'-dihydroxydiphenyl sulfone. Background technique [0002] 4,4'-dihydroxydiphenyl sulfone, also referred to as bisphenol S or BPS. Has excellent heat resistance, light resistance and oxidation resistance. Polyethersulfone, polysulfone ether ketone, etc. can be prepared by BPS reaction. BPS can also undergo bromination or sulfonation reactions, such as tetrabrominated bisphenol S, or octabromo-S ether, which is an excellent flame retardant. BPS is also mainly used as an intermediate of color developer for thermal pressure-sensitive recording paper. [0003] There are mainly the following methods for preparing BPS. [0004] Hydrolysis method: 4,4'-dichlorodiphenyl sulfone is hydrolyzed under the action of alkali, and then acidified to obtain BPS. Because 4,4'-dichlorodiphenyl sulfone is not easy to obtain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/22C07C315/00B01J31/02
Inventor 张天永李彬朱佳佑陈松王树华汤元睿
Owner KEMAI CHEM
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