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Polyurethane foam composite flame retardant and preparation method thereof

A composite flame retardant and polyurethane foam technology, applied in the field of flame retardants, can solve the problems of reduced flame retardant performance and atomization performance, poor flame retardant effect, environmental pollution, etc., achieve low atomization value, save alkali Washable, excellent flame retardant effect

Active Publication Date: 2019-02-22
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method only adopts the addition of fuacid to solve the problem of reducing the content of low-toxic substances and does not reduce the content of n=0 in the mixture, the flame retardant effect is not good, and the viscosity is still very large
[0013] CN102277176A (the application number is 201110122334.2, the title of invention is a kind of chlorinated alkyl polyphosphate flame retardant and its synthesis process). Among the chlorinated alkyl polyphosphates synthesized by this patent, the n=1 compound is mainly synthesized, It is not a mixture, a severe excess of propylene oxide is capped, which is likely to cause environmental pollution
[0014] The inventor found in the research: the monochlorine content in the diethylene glycol chloropropyl phosphate oligomer DECPP (being structural formula II) is low namely: when n=0, its flame retardancy and atomization performance are very good, but High viscosity (2000-2500mpa.s), when n=1, the viscosity is 800-1200mpa.s, as the n value increases, the viscosity decreases, but the flame retardancy and atomization performance decrease, and when used alone, foaming There will be foam collapse in the process. In order to improve its viscosity and foaming problems, the inventor provides a preparation method that can reduce the content of monochlorine

Method used

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  • Polyurethane foam composite flame retardant and preparation method thereof
  • Polyurethane foam composite flame retardant and preparation method thereof
  • Polyurethane foam composite flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0062] Add phosphorus oxychloride (1500g, 9.78mol) and catalyzer magnesium chloride (1g, be equivalent to 0.067% of phosphorus oxychloride weight) in reactor, be heated to 55-60 ℃ under stirring, begin to feed propylene oxide ( 2000g, 34.44mol) (the molar ratio of phosphorus oxychloride to propylene oxide is 1:3.52), the balance of temperature and cooling rate is strictly controlled during the feeding process, until the rated amount of epoxy compound is passed through, and the Keep warm at 55-60°C for another 3 hours, and recover the epoxy compound by vacuum distillation after the reaction. During vacuum distillation, vacuumize for 0.5 hours, and control the vacuum degree at 50-60KPa. After distillation, keep the vacuum at 50-60°C Phosphorus oxychloride (2300g, 15mol) and diethylene glycol (1060g, 9.99mol) were added dropwise at the same time, the temperature was controlled at 55-60°C, and the dropping time was 3-5 hours. During the reaction, a large amount of acid was directly...

Embodiment 2

[0064] Add phosphorus oxychloride (3100g, 20.22mol) and catalyst titanium tetrachloride (3.g, equivalent to 0.097% of the weight of phosphorus oxychloride) in the reactor, heat to 55-60°C under stirring, and start continuous Enter propylene oxide (6500g, 111.91mol) (the mol ratio of phosphorus oxychloride and propylene oxide is 1:5.54), the balance of temperature and cooling rate is strictly controlled in the feeding process, until the epoxy compound of rated amount is passed through, After passing through the material, keep the temperature at 55-60°C for another 3 hours. After the reaction, the epoxy compound is recovered by vacuum distillation. During the vacuum distillation, vacuumize for 0.5 hours, and the vacuum degree is controlled at 45-55KPa. After the distillation, keep the vacuum , drop phosphorus oxychloride (4166g, 27.17mol) and diethylene glycol (2060g, 19.41mol) at 35-60°C, control the temperature at 40-45°C, drop time for 4-5 hours, during the reaction A large a...

Embodiment 3

[0066] Add phosphorus oxychloride (1500kg, 9.78kmol) and catalyzer magnesium chloride (1KG, be equivalent to 0.067% of the weight of phosphorus oxychloride) in reactor, be heated to 55-60 ℃ under stirring, start to feed propylene oxide ( 2000Kg, 34.44kmol) (the molar ratio of phosphorus oxychloride to propylene oxide is 1:3.52), the balance of temperature and cooling rate is strictly controlled during the feeding process, until the rated amount of epoxy compound is passed, and after the feeding is completed, the Keep warm at 55-60°C for another 5 hours, and recover the epoxy compound by vacuum distillation after the reaction. During vacuum distillation, vacuumize for 1 hour, and the vacuum degree is controlled at 40-50KPa. After distillation, keep the vacuum at 35-60°C Phosphorus oxychloride (2300kg, 15kmol) and diethylene glycol (1060kg, 9.99kmol) were added dropwise, the temperature was controlled at 45-50°C, and the addition time was 4-6 hours. After the addition, N-methylm...

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Abstract

The invention relates to a polyurethane foam composite flame retardant and a preparation method thereof. The composite flame retardant is composed of TCPP and a diethylene glycol chloropropyl phosphate oligomer which are in the weight ratio of (40-50):(60-50) measured by 100 parts, and the diethylene glycol chloropropyl phosphate oligomer is also known as a diethylene glycol bis(2-(chloroethyl)phosphate oligomer and is a compound or a mixture shown as a structural formula II. By using the composite flame retardant provided by the invention, defects existing in a using process of a single flameretardant are avoided, meanwhile, the problem of high atomization performance is solved, and the prepared polyurethane foam sponge is very low in atomization value and good in flame retardance.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a polyurethane foam composite flame retardant and a preparation method thereof. Background technique [0002] Rigid polyurethane foam, referred to as rigid polyurethane foam, is second only to soft polyurethane foam in the amount of polyurethane products. Polyurethane rigid foam mostly has a closed-cell structure, which has excellent properties such as good heat insulation effect, light weight, high specific strength, and is widely used in automotive materials. [0003] With the development of society, automobiles are becoming more and more popular, the automobile industry is advancing by leaps and bounds, and the demand for automobile materials is increasing. However, the rigid polyurethane foam of automobile materials is easy to burn, and flame retardants need to be added for flame retardant modification. [0004] The flame retardants added to automotive materials are...

Claims

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Application Information

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IPC IPC(8): C08K5/521C08G18/76C08G18/48C08J9/08C08G101/00
CPCC08G18/48C08G18/7671C08K5/521C08K2201/014C08G2110/005C08G2110/0083
Inventor 王秋伟牛丽丹金译平王咪咪
Owner ZHEJIANG WANSHENG
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