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Triazine ring hexaphenyl phosphate-containing flame retardant and preparation method thereof

A hexaphenyl phosphate and flame retardant technology, which is applied in the field of triazine ring hexaphenyl phosphate flame retardant and its preparation, can solve the adverse effects of material mechanical properties, limit industrial production and application, matrix resin phase Poor compatibility and other problems, to achieve the effect of excellent P-N synergistic flame retardancy, excellent char formation ability, and good compatibility

Active Publication Date: 2014-07-16
CHANGZHOU XIAOGUO INFORMATION SERVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional intumescent flame retardants have disadvantages such as large addition, poor thermal stability, and poor compatibility with matrix resins, which have adverse effects on the processing and mechanical properties of materials, thus limiting their industrial production and application.

Method used

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  • Triazine ring hexaphenyl phosphate-containing flame retardant and preparation method thereof
  • Triazine ring hexaphenyl phosphate-containing flame retardant and preparation method thereof
  • Triazine ring hexaphenyl phosphate-containing flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 60ml toluene, 11.63mmol Saike, 0.2840g dimethylaminopyridine and 34.89mmol triethylamine in the 100mL dry four-neck flask equipped with constant pressure dropping funnel, thermometer, electric stirrer, then in ice-salt bath condition and At a stirring speed of 500r / min, add 34.89mmol of diphenyl chlorophosphate and 15ml of toluene dropwise for 2 hours. After the dropwise addition, move to room temperature at 20°C for 8 hours, then filter to obtain the filtrate, and evaporate it under reduced pressure. Organic solvent, then wash with distilled water to 3-5 times successively, the sodium carbonate solution that mass fraction is 5% washs 3-5 times, distilled water washes to neutrality, finally obtain light yellow viscous liquid in vacuum drying, yield is 94%. According to the analysis of the characteristic peaks of the group by infrared spectrum and hydrogen nuclear magnetic resonance spectrum, it has been confirmed that the obtained product is a new type of phosphorus...

Embodiment 2

[0026] Embodiment 2, the synthetic method of novel phosphorus-nitrogen synergistic flame retardant is carried out according to the following steps:

[0027] Add 90ml of toluene, 17.43mmol of Saike, 0.4260g of dimethylaminopyridine and 57.52mmol of triethylamine into a dry four-neck flask equipped with a constant pressure dropping funnel, a thermometer, and an electric stirrer with a capacity of 250ml, and then add Under the condition of bath and stirring speed of 500r / min, add 57.52mmol of diphenyl chlorophosphate and 23ml of toluene dropwise, add dropwise for 2h, move to room temperature 20°C for 8h after the dropwise addition, and then filter to obtain the filtrate , evaporate the organic solvent under reduced pressure, then wash with distilled water for 3-5 times, then wash with 5% sodium carbonate solution for 3-5 times, then wash with distilled water until neutral, and finally dry in vacuum to obtain light yellow viscous Liquid, 94% yield. According to the analysis of th...

Embodiment 3

[0028] Embodiment 3, the synthetic method of novel phosphorus-nitrogen synergistic flame retardant is carried out according to the following steps:

[0029] Add 120ml of toluene, 23.26mmol of Saike, 0.5680g of dimethylaminopyridine and 65.93mmol of triethylamine into a dry four-neck flask equipped with a constant pressure dropping funnel, a thermometer, and a stirrer with a capacity of 250ml, and then place the mixture in an ice-salt bath With a stirring speed of 500r / min, add 65.78mmol of diphenyl chlorophosphate and 30ml of toluene dropwise, dropwise for 2h, move to room temperature at 20°C for 8h after the dropwise addition, and then filter to obtain the filtrate. Evaporate the organic solvent under reduced pressure, then wash with distilled water for 3-5 times, then wash with 5% sodium carbonate solution for 3-5 times, wash with distilled water until neutral, and finally dry in vacuum to obtain a light yellow viscous liquid , and the yield was 94%. According to the analys...

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Abstract

The invention discloses a triazine ring hexaphenyl phosphate-containing flame retardant and a preparation method thereof, relating to the technical field of preparing halogen-free flame retardant. According to the method, the mole ratio of tri(2-hydroxylethyl)isocyanurate to diphenyl chlorophosphate is 1:(3-3.2) under the condition of an organic solvent, the preparation method comprises the following steps of: sequentially adding tri(2-hydroxylethyl)isocyanurate, solvent, acid-binding agent and a catalyst, dropwise adding diphenyl chlorophosphate solution at -10DEG C to 5DEG C, heating to 20DEG C-25DEG C after the dropwise addition is completed, preserving heat for 2h-8h, after the reaction is finished, decompression-steaming the solvent, then sequentially washing with water and 5wt% sodium carbonate solution, and finally performing vacuum drying. The triazine ring hexaphenyl phosphate-containing synthetic method provided by the invention is simple to operate, low in cost and less in energy consumption; the decomposition temperature of the prepared flame retardant is at 280DEG C-438DEG C, and the prepared flame retardant has better thermal stability and better carbon forming capability.

Description

technical field [0001] The invention relates to the technical field of preparation of a halogen-free flame retardant, in particular to a flame retardant containing triazine cyclohexaphenyl phosphate and a preparation method thereof. Background technique [0002] With the development of society and the advancement of science and technology, synthetic polymer materials have widely penetrated into various fields of people's lives. However, synthetic polymer materials are usually flammable or combustible materials due to their particular composition. Therefore, in order to meet the social requirements for materials, especially in terms of flame retardancy, they must be modified for flame retardancy. Usually, the easiest and most feasible way to modify the flame retardant of materials is to add flame retardants to the materials. Therefore, the development and research of flame retardants has gradually become a hot spot. [0003] At present, the flame retardants used in industry...

Claims

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Application Information

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IPC IPC(8): C08K5/523C07F9/6521
Inventor 宋艳蒋明访李锦春邹国享
Owner CHANGZHOU XIAOGUO INFORMATION SERVICES
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