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

A technology of hexaphenylphosphate melamine salt and melamine, which is applied in the field of hexaphenylphosphate melamine salt flame retardant and its preparation, can solve the problems of releasing toxic gas, producing corrosive substances, generating smoke, etc., to prevent dripping Falling phenomenon, good heat insulation, and the effect of preventing the spread and spread of flames

Inactive Publication Date: 2012-11-21
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 0.1mol of phosphorus oxychloride and 0.002mol of anhydrous magnesium chloride into a 250ml three-necked flask equipped with a constant pressure dropping funnel, agitator and reflux device, stir mechanically and heat, and add phenol in batches at 110°C within 3h 0.2mol, keep warm and mechanically stir and reflux for 36h, and then distill under reduced pressure to obtain a light yellow liquid, which is diphenylphosphoryl chloride (DPCP).

[0022] 0.03mol of the product diphenylphosphoryl chloride of the previous step is placed in a 500ml three-necked flask equipped with a stirrer and a reflux device, and 100ml of distilled water and 100ml of N,N-dimethylformamide (DMF) are mixed and then added to In the three-necked flask, when the temperature was raised to 90°C, 0.01 mol of melamine was slowly added, kept at reflux for 9 hours, then cooled in an ice bath, filtered with suction, washed with water, and dried to constant weight to obtain a white solid, namely hexaphenylp...

Embodiment 2

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

[0025] The product diphenylphosphoryl chloride 0.102mol of the previous step is placed in a 500ml three-necked flask equipped with a stirrer and a reflux device, and the distilled water of 150ml and the N,N-dimethylformamide (DMF) of 150ml are mixed and then added to In the three-necked flask, when the temperature was raised to 90°C, 0.03 mol of melamine was slowly added, kept at reflux for 9 hours, then cooled in an ice bath, filtered with suction, washed with water, and dried to constant weight to obt...

Embodiment 3

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

[0028] 0.18mol of the product diphenylphosphoryl chloride of the last step is placed in a 500ml three-necked flask equipped with a stirrer and a reflux device, and 200ml of distilled water and 200ml of N,N-dimethylformamide (DMF) are mixed and then added to In the three-necked flask, when the temperature was raised to 90°C, 0.05 mol of melamine was slowly added, kept at reflux for 9 hours, then cooled in an ice bath, filtered with suction, washed with water, and dried to constant weight to obtain a white solid, nam...

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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 leadsthe 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 hexaphenylphosphate melamine salt flame retardant and a preparation method thereof. Background technique [0002] With the development of modern science and technology, human production and living standards 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 ensure the safety of synthetic materials, the most effective method is to add flame retardants to convert combustible materials into flame retardant materials according to the combustion characteristics, reduce the bu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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