Preparation method of tetrabromobisphenol S bis(2,3-dibromopropyl ether) flame retardant

A technology of flame retardant and liquid bromine, which is applied in the field of preparation of octabromosulfide flame retardant, can solve the problems of low purity of octabromosulfide, long reaction route, high production cost, etc., achieve high yield and purity, and produce The effect of low cost and reduced production of three wastes

Active Publication Date: 2020-04-10
山东旭锐新材股份有限公司
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned preparation method uses liquid bromine twice as the bromination agent to brominate the benzene ring and the olefin respectively, the reaction route is long, the safety is low, the production cost is high, and the three wastes produced are many, and the obtained octabromo-S ether has low purity

Method used

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  • Preparation method of tetrabromobisphenol S bis(2,3-dibromopropyl ether) flame retardant
  • Preparation method of tetrabromobisphenol S bis(2,3-dibromopropyl ether) flame retardant

Examples

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Embodiment 1

[0036] A kind of preparation method of bisphenol S diallyl ether intermediate comprises steps as follows:

[0037] Add 200g of methanol, 50g of bisphenol S, 5g of sodium iodide, and 50g of water into a four-necked flask with stirring, and add 21g of sodium hydroxide under stirring. When the temperature of the solution reaches 35°C, start to add 45.5g of chloropropene dropwise under stirring. , the temperature of the system during the addition of allyl chloride is not higher than 60°C. After the addition of allyl chloride, the temperature is raised to 65°C, and the temperature is kept for 5 hours. The pH of the system is kept between 8 and 11 during the whole heat preservation reaction. At 8:00, solid sodium hydroxide was added to keep the pH of the system between 8 and 11. After the reaction, cool the reaction liquid to 15°C, filter it with suction, wash the solid obtained by suction filtration three times with water, and then dry the obtained solid at 75°C for 5 hours to obta...

Embodiment 2

[0040] A kind of preparation method of bisphenol S diallyl ether intermediate comprises steps as follows:

[0041] Add 220g of the mother liquor recovered in Example 1, 50g of bisphenol S, 5g of potassium iodide, and 30g of methanol into a four-neck flask with stirring, add 21g of sodium hydroxide under stirring, and when the temperature of the solution rises to 35°C, add 45.5g of it dropwise under stirring Allyl chloride, the temperature of the system during the addition of allyl chloride is not higher than 60°C. After the addition of allyl chloride, the temperature is raised to 65°C, and the reaction is kept for 5 hours. The pH of the system is kept between 8 and 11 during the whole heat preservation reaction process. When it is lower than 8, add solid sodium hydroxide to keep the pH of the system between 8 and 11. After the reaction, the resulting reaction solution was cooled to 15°C, filtered with suction, and the solid obtained by suction filtration was washed with water ...

Embodiment 3

[0046] A kind of preparation method of bisphenol S diallyl ether intermediate comprises steps as follows:

[0047] Add 200g of n-propanol, 50g of bisphenol S, 5g of sodium bromide, and 50g of water into a four-necked flask with stirring, and add 21g of sodium hydroxide under stirring. When the temperature of the solution reaches 35°C, add 45.5g of it dropwise under stirring Allyl chloride, the temperature of the system during the addition of allyl chloride is not higher than 60°C. After the addition of allyl chloride, the temperature is raised to 65°C, and the reaction is kept for 5 hours. The pH of the system is kept between 8 and 11 during the whole heat preservation reaction process. When it is lower than 8, add 30% sodium hydroxide solution to keep the pH of the system between 8 and 11. After the reaction, cool the reaction liquid to 15°C, filter it with suction, wash the solid obtained by suction filtration three times with water, and then dry the solid at 75°C for 6 hours ...

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Abstract

The invention provides a preparation method of a tetrabromobisphenol S bis(2,3-dibromopropyl ether) flame retardant. Bisphenol S used as a raw material and chloropropene undergo a substitution reaction to obtain a bisphenol S diallyl ether intermediate, and the bisphenol S diallyl ether and liquid bromine undergo addition and substitution reactions to obtain tetrabromobisphenol S bis(2,3-dibromopropyl ether). One-time bromination is adopted to introduce all eight bromine atoms into an aromatic ring and a side chain at the same time, so that the process route is shortened, the operation is simple, the safety is high, and the production cost is low. A solvent can be recycled in the process of preparing the bisphenol S diallyl ether intermediate, and the output of three wastes is greatly reduced, so the pollution to the environment is reduced, and the production cost is saved. The tetrabromobisphenol S bis(2,3-dibromopropyl ether) flame retardant prepared in the invention has high productpurity and improved application quality.

Description

technical field [0001] The invention relates to a method for preparing an octabromo-S ether flame retardant, and belongs to the technical field of flame retardant preparation. Background technique [0002] Octabromo-S ether, also known as tetrabromobisphenol S bis(2,3-dibromopropyl) ether, the chemical name is bis[3,5-dibromo-4-(2,3-dibromopropoxy) ]Phenylsulfone is a high-efficiency flame retardant, mainly used for flame retardancy of PE, PP, HIPS, etc., and has the structure shown in the following formula: [0003] [0004] At present, the preparation method of octabromobisphenol generally includes a three-step synthesis reaction: first, bisphenol S is brominated to synthesize tetrabromobisphenol S; in the second step, tetrabromobisphenol S is reacted with allyl halide to form tetrabromobisphenol S Bromobisphenol S diallyl ether, referred to as tetrabromo-S ether intermediate; finally, the tetrabromo-S ether intermediate is added with bromine to obtain octabromo-S ethe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C317/22
CPCC07C315/04C07C317/22
Inventor 杨振振王强张荣华杨清波李金忠杨凯李洪瑞
Owner 山东旭锐新材股份有限公司
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