A kind of synthetic method of bisphenols

A synthesis method and phenol technology, applied in the field of organic synthesis, can solve the problems of reduced service life, complex process and high cost of heat transfer oil, and achieve the effects of improving purity and yield, simplifying operation process and reducing reaction cost

Active Publication Date: 2021-07-09
SHANDONG DOCRIS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction requires the heat transfer oil to be at a high temperature of 230°C for a long time. Generally, the best use temperature of the heat transfer oil is below 200°C. Long-term high temperature may reduce the service life of the heat transfer oil, and the use of the heat transfer oil in the open air during the small test may cause fire hazards.
[0005] 2. The reaction will evaporate the solvent, which needs to be condensed immediately, and has higher requirements for the condensing device
[0006] 3. High temperature reaction, more trihydroxytriphenyldisulfone may appear in the reaction process
[0008] Therefore, the current bisphenol S synthesis method has many problems such as complex process, high cost, low product yield and harsh equipment requirements, which restricts the industrial production of bisphenol S

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] While stirring, 284g (3.0mol) of phenol and 0.5g of benzenesulfonic acid were heated to 130°C under nitrogen protection, and 100g (1.0mol) of 98% sulfuric acid was added dropwise therein, and the dropwise reaction time was 3h . The sulfonated reaction solution is kept warm in an oil bath and dehydrated with a slight negative pressure of -0.005MPa. After dripping the sulfuric acid, keep it warm for 2.5 hours, then raise the temperature to 175°C, and keep it warm for 5.5 hours until the system becomes molten. Samples are taken and analyzed by HPLC. The results showed that the composition (weight ratio) of 4,4'-dihydroxydiphenylsulfone / 2,4'-dihydroxydiphenylsulfone / trihydroxytriphenyldisulfone=92.5 / 7.0 / 0.5. All the excess phenol has been distilled off, and there is no residue in the system, and the crude product of 4,4'-dihydroxydiphenyl sulfone is obtained. The steamed phenol is used for the next application.

[0025] Dissolve the crude product in dilute lye, adjust th...

Embodiment 2

[0027] While stirring, 284g (3.0mol) of phenol and 0.45g of benzenesulfonic acid were heated up to 135°C under nitrogen protection, and 100g (1.0mol) of 98% sulfuric acid was added dropwise thereto, and the dropwise reaction time was 2.8 h. The sulfonated reaction solution is kept warm in an oil bath and dehydrated with a slight negative pressure of -0.006MPa. After dripping the sulfuric acid, keep it warm for 3 hours, then raise the temperature to 180°C, and keep it warm for 5 hours until the system becomes molten. Samples are taken and analyzed by HPLC. The results showed that the composition (weight ratio) of 4,4'-dihydroxydiphenylsulfone / 2,4'-dihydroxydiphenylsulfone / trihydroxytriphenyldisulfone=92.4 / 7.0 / 0.6. All the excess phenol has been distilled off, and there is no residue in the system, and the crude product of 4,4'-dihydroxydiphenyl sulfone is obtained. The steamed phenol is used for the next application.

[0028] Dissolve the crude product in dilute lye, adjust ...

Embodiment 3

[0030] While stirring, 237g of phenol and 0.4g of benzenesulfonic acid were heated up to 122°C under nitrogen protection, and 100g of 98% sulfuric acid was added dropwise thereto, and the dropwise reaction time was 3.5h. The sulfonated reaction solution is kept warm in an oil bath and dehydrated with a slight negative pressure of -0.005MPa. After dripping the sulfuric acid, keep it warm for 2.5 hours, then raise the temperature to 170°C, and keep it warm for 5.8 hours until the system becomes molten. Samples are taken and analyzed by HPLC. The results showed that the composition (weight ratio) of 4,4'-dihydroxydiphenylsulfone / 2,4'-dihydroxydiphenylsulfone / trihydroxytriphenyldisulfone=92.3 / 7.1 / 0.6. All the excess phenol has been distilled off, and there is no residue in the system, and the crude product of 4,4'-dihydroxydiphenyl sulfone is obtained. The steamed phenol is used for the next application.

[0031] Dissolve the crude product in dilute lye, adjust the pH to 9.0, ob...

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PUM

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Abstract

The invention discloses a method for synthesizing bisphenol S, which comprises the following steps: (1) while stirring, under nitrogen protection, phenol and a catalyst are heated to 120-140° C., and 98wt% concentrated sulfuric acid is added dropwise thereto. , the dropwise addition time is 2.5-3.5h; continue to keep the reaction for 2-3h, heat up to 160-190°C, and keep the temperature for 5-6h until the system becomes molten to obtain the crude product. (2) dissolving the obtained crude product in dilute alkali solution, adjusting pH to be 8.5~9.5, obtaining mother liquor after decolorization heat filtration, adjusting the pH of the mother liquor to 5~6 with dilute hydrochloric acid, dissolving the separated monosodium salt in water, continue The pH is adjusted to 2-3, the product is precipitated in solid form, and 4,4'-dihydroxydiphenyl sulfone is obtained after filtration and drying. The invention reduces the reaction temperature, improves the reaction safety, simplifies the operation process, reduces the reaction cost, and increases the content of 4,4'-dihydroxydiphenyl sulfone in the fine product.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis technology of bisphenol S. Background technique [0002] Bisphenol S, the Chinese name is 4,4'-dihydroxydiphenyl sulfone; 4,4'-dihydroxydiphenyl sulfone; 4,4'-sulfonyl diphenol; bisphenol S; 4,4'-dihydroxy Diphenylsulfone; 4-hydroxyphenylsulfone; p,p-dihydroxydiphenylsulfone; 4,4'-sulfonyldiphenol; bis(4-hydroxyphenyl)sulfone. It is mainly used as a monomer for the synthesis of polysulfone resin, and can also be directly used in coatings, leather modifiers, dye intermediates, metal plating brighteners, etc. The molecule contains two hydroxyl groups and a strong electron-withdrawing sulfone group, so the acidity is stronger than other phenols. It has heat resistance, oxidation resistance and light stability. [0003] At present, the synthesis technology of bisphenol S in the prior art is to synthesize bisphenol S at a high temperature of 230°C by using phe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C315/00C07C317/22C07C303/06C07C309/42
CPCC07C303/06C07C315/00C07C317/22C07C309/42
Inventor 于文智刘凯卢凤阳李强宫雪红马淑敏段升芹黄进强张鹏
Owner SHANDONG DOCRIS CHEM
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