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Hexaphenyl phosphate ester melamine salt fire retardant and method for preparing same

The technology of hexaphenyl phosphate melamine salt and melamine is applied in the field of hexaphenyl phosphate melamine salt flame retardant and its preparation, which can solve the problems of releasing toxic gas, generating corrosive substances, generating smoke, etc., and preventing dripping Falling phenomenon, good thermal insulation, the effect of preventing the spread and spread of flames

Inactive Publication Date: 2011-09-21
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the flame retardant improves the flame retardant performance of the polymer, it also has some disadvantages, mainly in: emitting toxic gas, generating smoke; generating corrosive substances; adding a large amount, affecting mechanical properties; having certain pollution to the environment and many more

Method used

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  • Hexaphenyl phosphate ester melamine salt fire retardant and method for preparing same
  • Hexaphenyl phosphate ester melamine salt fire retardant and method for preparing same
  • Hexaphenyl phosphate ester melamine salt fire retardant and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 0.1 mol of phosphorus oxychloride and 0.002 mol of anhydrous magnesium chloride to a 250ml three-necked flask equipped with a constant pressure dropping funnel, agitator and reflux device, stir and heat mechanically, add phenol in batches at 110°C and within 3 hours 0.2mol, heat preservation, mechanical stirring and reflux reaction for 36 hours, and then under reduced pressure distillation to obtain a pale yellow liquid, namely diphenylphosphoryl chloride (DPCP).

[0022] Put 0.03 mol of diphenylphosphoryl chloride from the previous step in a 500ml three-necked flask equipped with a stirrer and reflux device, mix 100ml of distilled water and 100ml of N,N-dimethylformamide (DMF) and add to In a three-necked flask, when the temperature is raised to 90°C, slowly add 0.01 mol of melamine, keep refluxing for 9 hours, then cool in an ice bath, filter with suction, wash with water, and dry to constant weight to obtain a white solid, which is hexaphenyl phosphate melamine salt....

Embodiment 2

[0024] Add 0.35mol of phosphorus oxychloride and 0.007mol of anhydrous magnesium chloride into a 500ml three-necked flask equipped with a constant pressure dropping funnel, stirrer and reflux device, stir and heat mechanically, and add phenol in batches at 110°C and within 3h 0.81mol, heat preservation, mechanical stirring and reflux reaction for 36h, and then under reduced pressure distillation to obtain a pale yellow liquid, namely diphenylphosphoryl chloride (DPCP).

[0025] Put 0.102 mol of diphenylphosphoryl chloride from the previous step in a 500ml three-necked flask equipped with a stirrer and reflux device, mix 150ml of distilled water and 150ml of N,N-dimethylformamide (DMF) and add to In a three-necked flask, when the temperature is raised to 90°C, slowly add 0.03 mol of melamine, keep refluxing for 9 hours, then cool in an ice bath, filter with suction, wash with water, and dry to constant weight to obtain a white solid, which is hexaphenyl phosphate melamine salt.

Embodiment 3

[0027] Add 1.15 mol of phosphorus oxychloride and 0.0115 mol of anhydrous magnesium chloride into a 500ml three-necked flask equipped with a constant pressure dropping funnel, agitator and reflux device, stir and heat mechanically, add phenol in batches at 110°C and within 3h 2.76mol, heat preservation, mechanical stirring, reflux reaction for 36h, and then under reduced pressure distillation to obtain a light yellow liquid, namely diphenylphosphoryl chloride (DPCP).

[0028] Put 0.18 mol of diphenylphosphoryl chloride from the previous step in a 500ml three-necked flask equipped with a stirrer and reflux device. Mix 200ml of distilled water and 200ml of N,N-dimethylformamide (DMF) and add to In a three-necked flask, when the temperature is raised to 90°C, slowly add 0.05 mol of melamine, keep refluxing for 9 hours, then cool in an ice bath, filter with suction, wash with water, and dry to constant weight to obtain a white solid, which is hexaphenyl phosphate melamine salt.

[0029...

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Abstract

The invention relates to a hexaphenyl phosphate ester melamine salt fire retardant and a method for preparing the same. Based on the molar ratio, the reaction ratio of diphenyl phosphorus oxychloride to melamine is (3.0-3.6):1.0, and the diphenyl phosphorus oxychloride comprises components of phenol, phosphorus oxychloride and anhydrous magnesium chloride in a ratio of (2.0-2.5):(1.0-1.4):(0.01-0.03). The preparation method comprises the following steps of: adding phosphorus oxychloride, anhydrous magnesium chloride and phenol respectively, performing continuous stirring reflux during reaction, and performing vacuum distillation after the reaction to obtain diphenyl phosphorus oxychloride; and adding the diphenyl phosphorus oxychloride and melamine, performing stirring reflux, and after the reaction, cooling the obtained product in an ice bath, and performing suction filtration, water washing and drying on the product to obtain the hexaphenyl phosphate ester melamine salt. The hexaphenyl phosphate ester melamine salt fire retardant prepared by the method has the advantages of low toxicity, less smoke, harmlessness, high efficiency, environmental friendliness and the like and leads the development trend of intumescent fire retardants in the future.

Description

Technical field [0001] The invention relates to a phosphorus-nitrogen series intumescent flame retardant, in particular to a hexaphenyl phosphate melamine salt flame retardant and a preparation method thereof. Background technique [0002] With the development of modern science and technology, the production and living standards of human beings continue to improve. Synthetic fibers, plastics, rubber and other polymer synthetic materials are more and more widely used in various fields, playing a huge role in national economic construction and people’s lives. effect. However, polymer materials are generally flammable or combustible, which can easily cause fire accidents. [0003] In order to solve the problems of flame resistance and smoke suppression of synthetic materials, and to ensure the safety of synthetic materials, the most effective method is to add flame retardants to convert flammable materials into flame retardant materials according to the combustion characteristics, re...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C07F9/6521
Inventor 潘志权吴风磊黄齐茂陈云峰周红
Owner WUHAN INSTITUTE OF TECHNOLOGY
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