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Method for preparing phosphorus-containing flame-retardant polyether polyol

A technology for flame retardant polyether and polyol, which is applied in the field of preparation of phosphorus-containing flame retardant polyether polyol, can solve the problems of flame retardant performance and mechanical performance defects, application limitations and the like, achieves good mechanical performance, simple preparation method, The effect of high flame retardant properties

Inactive Publication Date: 2018-03-30
SHAANXI JUJIEHAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame retardant materials in the prior art are still limited in their application due to the defects of flame retardancy and mechanical properties.

Method used

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  • Method for preparing phosphorus-containing flame-retardant polyether polyol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation method of phosphorus-containing flame-retardant polyether polyol comprises the following steps:

[0021] (1) Add trihydroxymethyl phosphine and KOH into the stainless steel reactor at a mass ratio of 6:1, replace the air in the reactor with nitrogen for 3 times, then raise the temperature to 80°C and keep it warm for 0.5h;

[0022] (2) Add propylene oxide to the product of step (1), then raise the temperature to 110°C, and keep the pressure at 0.2-0.6Mpa, wherein the mass ratio of the product of step (1) to propylene oxide is 10:1.5;

[0023] (3) Release the pressure of the reactor, add phosphoric acid and N,N-dimethylcyclohexylamine to the product of step (2) in sequence, then vacuum dehydrate for 2 hours, filter, and use the filter residue for later use; among them, the product of step (2), The mass ratio of phosphoric acid and N,N-dimethylcyclohexylamine is 10:0.8:1;

[0024] (4) Disperse the obtained filter residue in water, and disperse it ultrason...

Embodiment 2

[0029] The preparation method of phosphorus-containing flame-retardant polyether polyol comprises the following steps:

[0030] (1) Add trihydroxymethyl phosphine and KOH into the stainless steel reactor at a mass ratio of 8:1, replace the air in the reactor with nitrogen for 3 times, then raise the temperature to 80°C and keep it warm for 1.5h;

[0031] (2) Add propylene oxide to the product of step (1), then raise the temperature to 110°C, and keep the pressure at 0.2-0.6Mpa, wherein the mass ratio of the product of step (1) to propylene oxide is 10:1.5;

[0032] (3) Release the pressure of the reactor, add phosphoric acid and N,N-dimethylcyclohexylamine to the product of step (2) in sequence, then vacuum dehydrate for 2 hours, filter, and use the filter residue for later use; among them, the product of step (2), The mass ratio of phosphoric acid and N,N-dimethylcyclohexylamine is 10:0.8:1;

[0033] (4) Disperse the obtained filter residue in water, and disperse it ultrason...

Embodiment 3

[0036] The preparation method of phosphorus-containing flame-retardant polyether polyol comprises the following steps:

[0037] (1) Add trihydroxymethylphosphine and KOH into a stainless steel reactor at a mass ratio of 6:1, replace the air in the reactor with nitrogen for 3 times, then raise the temperature to 80°C and keep it warm for 1 hour;

[0038] (2) Add propylene oxide to the product of step (1), then raise the temperature to 110°C, and keep the pressure at 0.2-0.6Mpa, wherein the mass ratio of the product of step (1) to propylene oxide is 10:1.5;

[0039] (3) Release the pressure of the reactor, add phosphoric acid and N,N-dimethylcyclohexylamine to the product of step (2) in sequence, then vacuum dehydrate for 2 hours, filter, and use the filter residue for later use; among them, the product of step (2), The mass ratio of phosphoric acid and N,N-dimethylcyclohexylamine is 10:0.8:1;

[0040] (4) Disperse the obtained filter residue in water, and disperse it ultrasoni...

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Abstract

The invention discloses a preparation method of phosphorus-containing flame-retardant polyether polyol, which comprises the following steps: (1) adding trimethylol phosphine and KOH into a stainless steel reaction kettle, and replacing the air in the reaction kettle with inert gas for 3 times , then raise the temperature to 80°C and keep it warm for 0.5‑1.5h; (2) Add propylene oxide to the product of step (1), then raise the temperature to 110°C and keep the pressure at 0.2‑0.6Mpa; (3) Release the pressure of the reactor , add phosphoric acid and N,N-dimethylcyclohexylamine to the product of step (2) in sequence, then vacuum dehydrate for 2 hours, filter, and filter the residue for later use; (4) disperse the obtained filter residue in water, and ultrasonically disperse it; (5 ) The product of step (4) was subjected to microwave reaction, and then suction filtered. According to the method provided by the invention, the obtained phosphorus-containing flame-retardant polyether polyol has high flame-retardant performance, the oxygen index can reach about 25%, and the mechanical performance is good.

Description

technical field [0001] The invention belongs to the field of preparation of organic materials, and in particular relates to a preparation method of phosphorus-containing flame-retardant polyether polyol. Background technique [0002] Rigid polyurethane foam plastics have excellent properties such as unique thermal insulation properties, light weight, high specific strength, and simple construction. At the same time, they also have the characteristics of sound insulation, cold resistance, heat resistance, and corrosion resistance. An insulation material with the lowest thermal conductivity. Therefore, it is widely used as thermal insulation material for building exterior walls, cold storage, pipelines, refrigerator freezers, etc. The oxygen index of polyurethane rigid foam without flame retardant treatment is about 19%, and its flame retardant problem is particularly prominent. [0003] At present, the flame retardant of polyurethane materials is mainly divided into two typ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/327C08G65/28
CPCC08G65/327C08G65/2639
Inventor 李长英
Owner SHAANXI JUJIEHAN CHEM CO LTD
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