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Method of preparing bromobisphenol S diene propyl ether

A technology of bisallyl ether and tetrabromobisphenol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large solvent loss, difficult application, large energy consumption, etc., and achieves manufacturing cost The effect of reducing and saving production costs and improving economic benefits

Inactive Publication Date: 2009-01-14
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process needs to distill the solvent every time to obtain the product, which has high energy consumption, large solvent loss, and serious pollution. In today's energy shortage and emphasis on green production, this process is difficult to apply

Method used

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  • Method of preparing bromobisphenol S diene propyl ether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 30g of tetrabromobisphenol S, 40ml of isopropanol, 60ml of water, 5ml of chlorobenzene, 4.5g of sodium hydroxide, and 0.5g of tetraethylammonium bromide into a 500ml four-necked bottle equipped with a stirrer, a thermometer, and a condenser. , put 9g of allyl chloride into the pear-shaped addition funnel, heat the solution to 80°C, add allyl chloride dropwise, and keep the reaction solution alkaline during the reaction. If the pH value is less than 8, NaOH can be added appropriately and kept warm After reacting for 10 hours and cooling, white crystals were obtained, which were centrifuged and dried to obtain the product tetrabromobisphenol S diallyl ether with a melting point of 183° C. and a yield of 95%.

Embodiment 2

[0020] Add 60ml of isopropanol, 30g of tetrabromobisphenol S, 40ml of water, and 4.5g of NaOH into a 250ml three-necked flask equipped with a stirrer, a thermometer, and a condenser, stir to dissolve, and then add 0.5g of tetraethylammonium bromide , 20ml of chlorobenzene, 9g of chloropropene, heated to 65°C, kept warm for 9 hours, cooled to obtain white crystals, centrifuged, and dried to obtain the product tetrabromobisphenol S diallyl ether with a melting point of 184°C. The rate is 92%.

Embodiment 3

[0022] Add 30g of tetrabromobisphenol S, 25ml of isopropanol, 30ml of water, 4ml of chlorobenzene, 5g of sodium hydroxide, and 1g of tetraethylammonium bromide in a 500ml four-necked bottle equipped with a stirrer, a thermometer, and a condenser tube. Put 10g of allyl chloride into the pear-shaped addition funnel, heat the solution to 70°C, add allyl chloride dropwise, and keep the reaction solution alkaline during the reaction. If the pH value is less than 8, NaOH can be added appropriately, and the reaction time is 8 After cooling for one hour, white crystals were obtained, which were centrifuged and dried to obtain the product tetrabromobisphenol S diallyl ether with a melting point of 184° C. and a yield of 94%.

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Abstract

The invention discloses a preparation method of tetrabromobisphenol S diallyl oxide, which is characterized in that: tetrabromobisphenol S is reacted with chloropropene at a temperature of between 40 and 100 DEG C to generate the tetrabromobisphenol S diallyl oxide in an isopropyl alcohol-water-chlorobenzene mixed solvent in the presence of sodium hydroxide and tetraethyl ammonium bromide, wherein, the function of sodium hydroxide is to transform tetrabromobisphenol S into sodium salt, and the tetraethyl ammonium bromide is a catalyst. After the complete reaction, the tetrabromobisphenol S diallyl oxide is obtained through centrifugal separation, and the mother liquor can be used repeatedly. The method has advantages of good purity of prepared products, low energy consumption and high production efficiency.

Description

Technical field: [0001] The invention relates to a method for producing a combustion aid, in particular to a method for producing tetrabromobisphenol S diallyl ether. Background technique: [0002] Tetrabromobisphenol S diallyl ether is a new type of flame retardant and also a key raw material for the synthesis of tetrabromobisphenol S bis(2,3-dibromopropyl ether). Tetrabromobisphenol S bis(2,3-dibromopropyl ether) is an excellent additive flame retardant with excellent heat resistance, light resistance and oxidation resistance. Widely used in polypropylene, ABS and polystyrene plastics. [0003] The synthesis of tetrabromobisphenol S diallyl ether is based on tetrabromobisphenol S as a raw material. In the presence of sodium hydroxide, tetrabromobisphenol S and 3-chloropropene undergo a substitution reaction to generate tetrabromobisphenol S bis Allyl ether. [0004] [0005] The synthesis of tetrabromobisphenol S diallyl ether usually uses isopropanol aqueous solutio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/22C07C315/04
Inventor 孔庆池尚智勇董青
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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