Tetrabromo-benzene anhydride diol synthesis method

A technology of tetrabromophthalic anhydride diol and a synthesis method, applied in directions such as organic chemistry, can solve problems such as the synthesis method of tetrabromophthalic anhydride diol, etc., and achieve high product yield, good product quality and good thermal stability Effect

Active Publication Date: 2013-08-07
SHANDONG RUNKE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prior art all does not relate to the synthetic method of tetrabromophthalic anhydride diol of the present invention

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Tetrabromophthalic anhydride and diethylene glycol are added to the reactor, the molar ratio of tetrabromophthalic anhydride and diethylene glycol is 1:1, under stirring state, add catalyst p-toluenesulfonic acid, the addition amount of catalyst The molar ratio of tetrabromophthalic anhydride is 0.1%. Under the protection of the protective gas nitrogen, the reaction is carried out after the first temperature rise to the reaction temperature, and the time required for the first temperature rise is 5h; the reaction temperature of the first temperature rise is 150°C; The time is 10h, after the reaction finishes, add organic solvent dichloromethane and stir to dissolve the above-mentioned reaction materials, the addition of organic solvent is 1 times of tetrabromophthalic anhydride quality; The molar ratio of propylene oxide is 1:1; the temperature for adding propylene oxide is 40°C; the temperature is raised for the second time for heat preservation reaction, and the react...

Embodiment 2

[0019] Tetrabromophthalic anhydride and diethylene glycol are added into the reactor, the molar ratio of tetrabromophthalic anhydride and diethylene glycol is 1:1.5, under stirring state, add catalyst sodium acetate, the addition amount of catalyst accounts for 4 The molar ratio of bromophthalic anhydride is 5%. Under the protection of the protective gas argon, the reaction is carried out after the first temperature rise to the reaction temperature, and the time required for the first temperature rise is 3 hours; the reaction temperature of the first temperature rise is 125°C; the reaction is carried out after the first temperature rise to the reaction temperature The time is 15h, after the reaction finishes, add organic solvent dichloroethane and stir to dissolve the above-mentioned reaction material, the add-on of organic solvent is 5 times of tetrabromophthalic anhydride quality; Add propylene oxide after cooling, propylene oxide add-on and tetrabromophthalic anhydride quali...

Embodiment 3

[0021] Tetrabromophthalic anhydride and diethylene glycol are added into the reactor, the molar ratio of tetrabromophthalic anhydride and diethylene glycol is 1:2, under stirring state, add catalyst triethylamine, the addition amount of catalyst accounts for The molar ratio of tetrabromophthalic anhydride is 10%. Under the protection of the protective gas carbon dioxide, the reaction is carried out after the first temperature rise to the reaction temperature, and the time required for the first temperature rise is 1h; The time is 20h, after the reaction finishes, add organic solvent chloroform and stir to dissolve the above-mentioned reaction materials, the addition of organic solvent is 10 times of tetrabromophthalic anhydride quality; The ratio is 3:1; the temperature for adding propylene oxide is 50°C; the second temperature rise is for the heat preservation reaction, and the reaction temperature for the second heat rise is 80°C; the time for the second temperature rise to ...

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PUM

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Abstract

The invention discloses a tetrabromo-benzene anhydride diol synthesis method comprising the steps that: tetrabromo-benzene anhydride and diethylene glycol are uniformly stirred; a catalyst is added; under the protection of a protective gas, fist heating is carried out, and a reaction is carried out when a reaction temperature is reached; when the reaction is finished, an organic solvent is added for dissolving the reaction material; the temperature is reduced, and epoxypropane is added; secondary heating is carried out, and a maintained-temperature reaction is carried out; after the reaction, hot filtering is carried out; and distillation is carried out for removing the organic solvent, such that the product is obtained. The solvent adopted in the invention can be recovered by distillation and can be recycled, the process is simple, reaction temperature is low, reaction conditions are mild, the reactions are easy to control, production energy consumption is low, no harsh reaction condition is in the steps, industrial production can be easily carried out, product yield is high, product thermal stability is high, product content is high, product quality is good, no three-waste production is caused, and no environment-pollution problem is caused.

Description

technical field [0001] The invention relates to the field of flame retardant synthesis, in particular to a synthesis method of tetrabromophthalic anhydride diol. Background technique [0002] Tetrabromophthalic anhydride diol is a reactive flame retardant intermediate mainly used in rigid polyurethane foam. It has a light brown viscous liquid appearance and has good compatibility with most polyols and fluorocarbons. Tetrabromophthalic anhydride diol contains 46% bonded aromatic bromine and is extremely stable in mixed resins. [0003] Tetrabromophthalic anhydride diol is a reactive flame retardant, mainly used for flame retardancy of hard polyurethane foam, adhesives and coatings. [0004] Tetrabromophthalic anhydride diol is mainly used as a reactive flame retardant for the production of Class I and Class II polyurethane rigid foam (PUR). Foams containing tetrabromophthalic anhydride (even in strips as thin as 4″) have very low smoke generation and flame spread. Excellent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/48C08K5/3417
Inventor 宗先庆
Owner SHANDONG RUNKE CHEM
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