Synthetic method of fire-retardant N,N'-ethylene bis-tetrabromo phthalimide and screw thrust tubular reactor

A technology of tetrabromophthalimide and tubular reactor, which is applied in the field of flame retardant N, can solve the problems of insufficient fineness, excessive bromine content, long reaction time, etc., and achieve stable product quality , low residual bromine content and high bromination degree

A technology of tetrabromophthalimide and tubular reactor, which is applied in the field of flame retardant N, can solve the problems of insufficient fineness, excessive bromine content, long reaction time, etc., and achieve stable product quality , low residual bromine content and high bromination degree

CN1821225AInactive Publication Date: 2006-08-23蔡晨波

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  • Synthetic method of fire-retardant N,N'-ethylene bis-tetrabromo phthalimide and screw thrust tubular reactor
  • Synthetic method of fire-retardant N,N'-ethylene bis-tetrabromo phthalimide and screw thrust tubular reactor

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Experimental program
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Embodiment Construction

[0024] 200Kg of phthalic anhydride and 43.5Kg of ethylenediamine are simultaneously injected into the screw-propelled tubular reactor, and the temperature is gradually raised to react at 60-100°C for 4 hours, 100-160°C for 4 hours, and 240-260°C for 2 hours , In N, N'-ethylene bisphthalimide. After the reaction, the collected reaction solution was cooled to room temperature and sectioned.

[0025] Gained chip load is dropped in the reactor again, add 4.2Kg heterogeneous aluminum vanadium iron catalyst and 2500Kg 60% fuming sulfuric acid, drop the bromine of 600Kg, reaction temperature is controlled at 50~100 ℃ and reacts 14 hours, 125~ React at 135°C for 4 hours. After the reaction, cool, wash and filter (pressure) to obtain light yellow N, N'-ethylene bis-tetrabromophthalimide. The filtrate is recycled to the next use.

[0026] Add N, N`-ethylene bis-tetrabromophthalimide into 5000Kg water, use wet sanding method, sanding for 5-20 hours, check the fineness and whiteness, s...

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Abstract

The present invention discloses the synthesis process of fire retardant Nú¼Níõ-ethylene bis-tetrabromo phthalimide and its screw thrust tubular reactor. Inside the screw thrust tubular reactor, phthalic anhydride and ethylene diamine are first condensated under no water condition to synthesize Nú¼Níõ-ethylene bis-phthalimide, and bromine is then dropped to produce bromination in fuming sulfuric acid as solvent and in the presence of multiple phase catalyst so as to produce Nú¼Níõ-ethylene bis-tetrabromo phthalimide. The process may include post-treatment steps of water washing, sand grinding, pressure filtering, stoving, etc. to obtain the target product fine white Nú¼Níõ-ethylene bis-tetrabromo phthalimide powder. It has no color change in high temperature roasting, and may be used in product with high color requirement.

Description

technical field [0001] The invention belongs to a production method of a flame retardant, in particular to an industrial synthesis method of a flame retardant N, N'-ethylene bistetrabromophthalimide. Background technique [0002] N,N'-Ethylene bis-tetrabromophthalimide, molecular formula structure: [0003] [0004] The pure product is white powder, melting point is 450°C, decomposition temperature is above 450°C, density is 2660 kg / m3, solubility (g / 100g, temperature 25°C), in acetone, benzene, o-dichlorobenzene and dimethyl Formamide is less than 0.5, 0.015 in cottonseed oil, and 0.002 in water. It is an efficient additive flame retardant. [0005] Looking at the production and research and development status at home and abroad, the synthesis route of N,N′-ethylene bis-tetrabromophthalimide flame retardant from phthalic anhydride is as follows: [0006] ①First bromination and then organic solvent condensation process [0007] Typical synthesis method of tetrabromopht...

Claims

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Application Information

Patent Timeline
23 Aug 2006
Publication
CN1821225A
IPC
C07D209/48; C09K21/10
Inventors
徐保明; 蔡晨波