Synthetic method for N,N-Ethylene-Bis(bromophthalimide)

The technology of a kind of bromophthalimide and synthesis method is applied in the field of synthesis of ethylene bisbromophthalimide, which can solve the problems of unfavorable industrialized production, complex production process and complicated condensation process, etc., and achieve Improve the synthesis reaction yield, good product quality, and improve the effect of bromination reaction yield

Inactive Publication Date: 2013-02-13
SHANDONG RUNKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The condensation process of this patent is complicated, a large amount of organic solvent is used, and the loss is large, and the production cost is high
[0010] Several synthetic methods in the prior art all have the defects of low product quality, low yield, complex production process, large production pollution or high production cost, which are unfavorable for industrialized production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put the catalyst of phthalic anhydride and metal chloride into oleum, add bromine dropwise at 22°C for bromination reaction to obtain crude tetrabromophthalic anhydride, the reaction molar ratio of phthalic anhydride and bromine is 1 : 4.0, the yield is 95.7%.

[0037] The crude tetrabromophthalic anhydride is firstly acid-washed, then complexed with a metal ion complexing agent, then neutralized and washed with water again to obtain tetrabromophthalic anhydride.

[0038] Put tetrabromophthalic anhydride into an organic solvent, add ethylenediamine dropwise according to the molar ratio of tetrabromophthalic anhydride and ethylenediamine 1:2.0, and condense at 100°C to obtain crude product ethylenedibromophthalimide. The yield 96.2%.

[0039] The crude ethylene bisbromophthalimide was washed with water, and dehydrated at 150°C to obtain the product ethylene bisbromophthalimide with a total yield of 90.1%.

Embodiment 2

[0041] Put phthalic anhydride and catalyst iron powder into fuming sulfuric acid, add bromine dropwise according to the molar ratio of 1:4.1 at 20°C, keep warm for 3 hours after the dropwise addition, then raise the temperature to 40°C for reflux reaction for 8 hours, then The temperature was raised to 140° C. for aging reaction for 2 hours to obtain crude tetrabromophthalic anhydride with a yield of 96.5%.

[0042] The crude tetrabromophthalic anhydride was first acid-washed, then reacted with a metal ion complexing agent at 55° C. for 0.5 hour, then neutralized and washed with water again to obtain tetrabromophthalic anhydride.

[0043] Put tetrabromophthalic anhydride into an organic solvent, add dropwise a mixed solution of ethylenediamine and an organic solvent at 110°C, the molar ratio of tetrabromophthalic anhydride to ethylenediamine is 1:2.1, and after the addition is completed, keep warm for 6 hours and undergo a condensation reaction to obtain The yield of crude pro...

Embodiment 3

[0046] Put phthalic anhydride and catalyst aluminum powder into 60% oleum, the amount of oleum used is 3 times by weight of phthalic anhydride, stir and heat up to 25°C, and drop Add bromine, add dropwise within 1.5 hours, keep warm for 2 hours, then raise the temperature to 90°C for reflux reaction for 6 hours, evaporate excess bromine and sulfur trioxide, then raise the temperature to 150°C for aging reaction for 1 hour, and obtain the crude product four Bromophthalic anhydride, the yield is 97.2%.

[0047] The crude tetrabromophthalic anhydride was first acid-washed with 10% hydrochloric acid solution at 55°C for 0.5 hours, then complexed with EDTA at 55°C for 1 hour, then neutralized with sodium carbonate solution to a pH value of 7, and washed with water again Tetrabromophthalic anhydride was obtained.

[0048] Tetrabromophthalic anhydride is dropped into DMF, and a mixed solution of ethylenediamine and DMF is added dropwise at 120° C. The molar ratio of tetrabromophthal...

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PUM

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Abstract

The invention discloses a synthetic method for N,N-Ethylene-Bis(bromophthalimide). The synthetic method includes the following steps: (1) throwing phthalic anhydride and catalyst into fuming sulphuric acid, dripping bromine in the fuming sulphuric acid at normal temperature to carry out brominating reaction to obtain crude product tetrabromophthalic anhydride, a reaction molar ratio between the phthalic anhydride and the bromine is 1:3.8-4.1; (2) subjecting the crude product tetrabromophthalic anhydride to scouring and complexation, second neutralization and then second water scrubbing to obtain tetrabromophthalic anhydride; (3) Throwing the tetrabromophthalic anhydride into organic solution, dropwise adding ethanediamine diamine on the basis that the molar ratio between the tetrabromophthalic anhydride and the ethidene diamine is 1:1.9-2.1; and obtaining the crude product of N,N-Ethylene-Bis(bromophthalimide) after condensation reaction at the temperature of 50 DEG C to 150 DEGC. (4) Water scrubbing crude product ethylene double bromine phthalates formyl imine to obtain the ethylene double bromine phthalates formyl imine after high-temperature dewatering. The synthetic method is low in temperature of bromination reaction, temperate in reaction condition, easy to control, low in production energy consumption, high in product yield rate, and good in product quality.

Description

technical field [0001] The invention relates to the field of flame retardant synthesis, in particular to a synthesis method of ethylene bisbromophthalimide. Background technique [0002] Ethylene bisbromophthalimide is an important class of plastic flame retardants. It has excellent flame retardant effect and low toxicity. It is used in plastic products without frosting, does not affect the electrical and mechanical properties of products and has outstanding It is an excellent flame retardant for various engineering plastics and thermoplastics due to its thermal stability and UV resistance. [0003] Looking at the research and development status of production institutions at home and abroad, the synthesis routes of ethylene bisbromophthalimide flame retardants produced from phthalic anhydride are as follows: [0004] 1. Bromination process after organic solvent condensation [0005] Patent [US 5049601] introduces the synthetic method of ethylene dibromophthalimide, using p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/48
Inventor 宗先庆崔明亮吴多坤
Owner SHANDONG RUNKE CHEM
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