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A kind of preparation method of flame retardant polyol with high phosphorus content and multifunctionality

A flame retardant polyol and multi-functionality technology, which is applied in the field of flame retardant materials, can solve the problems of high flame retardant effect, low phosphorus content and insufficient hydroxyl functionality, and achieves good flame retardant effect.

Active Publication Date: 2022-03-15
浙理(浙江)检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the mass fraction of phosphorus in the existing phosphorus-carbon structure phosphorus-containing polyether polyol products is generally lower than 8%, and the phosphorus content is not high, so the flame-retardant effect cannot meet some high flame-retardant requirements, or the flame-retardant effect cannot be satisfied when the amount is too large. The combustion effect is achieved but the overall performance is insufficient
At the same time, the hydroxyl functionality in the existing phosphorus-containing polyether polyol molecular structure is not high enough, resulting in insufficient modulus, strength and mechanical properties of the prepared bulk flame-retardant adhesive after bonding, and the bulk flame-retardant foam is soft and brittle, and the foam is soft and hard. Poor degree adjustability, resulting in limited application fields of flame retardant foam

Method used

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  • A kind of preparation method of flame retardant polyol with high phosphorus content and multifunctionality
  • A kind of preparation method of flame retardant polyol with high phosphorus content and multifunctionality

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preparation example Construction

[0028] A preparation method of a highly phosphorus-containing and multifunctional flame-retardant polyol, comprising the following steps:

[0029] 1) Mix the pentaerythritol phosphate and the Lewis acid catalyst evenly, heat up to 55-65°C, then pass in the small molecule alkylene oxide compound, keep the pressure at 95-105°C for 0.5-3h, then vacuumize for 0.5-2h, and react Intermediate A is obtained. In terms of molar parts, the pentaerythritol phosphate is 45-55 parts, the small molecule alkylene oxide is 150-450 parts, and the Lewis acid catalyst is 1-3 parts.

[0030] 2) Mix the intermediate product A, trimethylolphosphine oxide and catalyst evenly, heat up to 55-65°C, react at 60-180°C for 4-8h, and vacuumize for 0.5-2h to obtain the intermediate product B. In molar fractions, the intermediate product A is 45-55 parts, the trishydroxymethyl phosphorus oxide is 100-400 parts, and the catalyst is 1-3 parts.

[0031] 3) Heat the intermediate product B, low molecular weight ...

Embodiment 1

[0036] (1) Pentaerythritol phosphate and Lewis acid catalyst (AlCl 3 and TiCl 4 ) mix evenly, heat up to 60°C, then feed 1,4-epoxybutane, keep the pressure at about 100°C for 1h, and then vacuumize for 2h, and react to obtain intermediate product A; in molar fraction, pentaerythritol phosphate : 50 parts, alkylene oxide: 400 parts, catalyst: 1 part.

[0037] (2) Mix intermediate product A, trihydroxymethylphosphine oxide and potassium hydroxide catalyst evenly, heat up to 60°C, react at 100°C for 6 hours, and vacuumize for 1 hour to obtain intermediate product B. In terms of molar parts, intermediate product A: 50 parts, trishydroxymethylphosphine oxide: 300 parts, catalyst: 1 part.

[0038] (3) Heat the intermediate product B, low molecular weight polyether polyols (PPG and PEG) and potassium hydroxide catalyst to react at 80°C for 6h, and vacuumize at 100°C for 1h to obtain a highly phosphorus-containing multifunctional flame retardant Polyol. In terms of molar parts, inte...

Embodiment 2

[0041] (1) Pentaerythritol phosphate and Lewis acid catalyst (AlCl 3 and TiCl 4 ) mix evenly, heat up to 60°C, then feed 1,4-epoxybutane, keep the pressure at about 100°C for 1h, and then vacuumize for 2h, and react to obtain intermediate product A; in molar fraction, pentaerythritol phosphate : 50 parts, alkylene oxide: 400 parts, catalyst: 1 part.

[0042] (2) Mix intermediate product A, trimethylolphosphine oxide and monobutyltin oxide catalyst evenly, heat up to 60°C, react at 100°C for 6 hours, and vacuumize for 1 hour to obtain intermediate product B. In terms of molar parts, intermediate product A: 50 parts, trishydroxymethylphosphine oxide: 300 parts, catalyst: 1 part.

[0043] (3) Heat the intermediate product B, low-molecular-weight polyether polyol and monobutyltin oxide catalyst to react at 80°C for 6h, and vacuumize at 100°C for 1h to obtain a highly phosphorus-containing multifunctional flame-retardant polyol. In terms of molar parts, intermediate product B: 5...

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Abstract

The invention relates to the field of flame retardant materials, and discloses a method for preparing a highly phosphorus-containing and multifunctional flame retardant polyol, comprising: 1) reacting pentaerythritol phosphate, a small molecule epoxy compound and a catalyst to obtain an intermediate product A; 2) ) Mix the intermediate product A, trihydroxymethyl phosphorus oxide and the catalyst to obtain the intermediate product B; 3) heat and mix the intermediate product B, the low-molecular-weight polyether polyol and the catalyst to obtain a flame-retardant polyol with high phosphorus-containing multifunctionality . The high-phosphorus-containing multi-functionality flame-retardant polyol of the present invention has the advantages of high and adjustable phosphorus content, high and adjustable functionality, and a wide range of applications. Adhesives and various foams prepared with it as raw materials have permanent flame-retardant functions , and environmental protection non-toxic exudation and other properties.

Description

technical field [0001] The invention relates to the field of flame retardant materials, in particular to a method for preparing a high phosphorus-containing and multifunctional flame retardant polyol. Background technique [0002] At present, flame-retardant polyols are basically halogenated polyether polyols, which contain high content of bromine or / and chlorine, and have good compatibility with polyether and polyester polyols. However, halogenated flame retardants lack anti-ultraviolet stability and are easy to bloom on the surface. When they are flame-retardant to polymers, they are easy to emit toxic smoke and gas, which is harmful to the environment and human health. Therefore, the development direction of flame retardants should be To the direction of halogen-free development. [0003] Phosphorus-containing polyether polyols are a kind of flame-retardant polyether polyols commonly used in rigid foam materials. They are generally made of phosphoric acid esters. The foa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08G18/50C08G81/00C09J175/08C08G101/00
CPCC08G65/2639C08G81/00C08G18/5084C08G18/5078C09J175/08C08G2101/00
Inventor 万军民
Owner 浙理(浙江)检测技术有限公司