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Synthesis of novel flame-retarding polyester polyol, and application thereof in polyurethane

A flame-retardant polyester and polyol technology, which is applied in the field of preparation of new flame-retardant polyester polyols for polyurethane, can solve the problems of bromine content to be further improved, flame-retardant performance limited, etc. The effect of mild conditions and simple synthesis process

Inactive Publication Date: 2012-03-28
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent application No. 200510122057.X uses dibromoneopentyl glycol as a flame retardant and introduces it as a chain extender into the polyurethane material to obtain a self-flame retardant waterborne polyurethane. Due to the addition of the chain extender The amount is small, and the effect on improving the flame retardant performance is limited
The Chinese patent application number is 201010295881.6, a highly active flame-retardant polyether polyol is prepared through polyols, epoxides, halogenated epoxides and tribromophenol, and it is applied to rigid polyurethane foam, but Its bromine content needs to be further improved

Method used

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  • Synthesis of novel flame-retarding polyester polyol, and application thereof in polyurethane
  • Synthesis of novel flame-retarding polyester polyol, and application thereof in polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 87.30g of dibromoneopentyl glycol, 33.73g of triethylamine and 30g of N-methylpyrrolidone to the four-necked flask, and gradually raise the temperature to 80°C. 2 Add 32.50 g of phenylphosphoryl dichloride and 60 g of toluene dropwise under the atmosphere, and control the dropwise addition in about 2 hours. After the dropwise addition, continue the reaction at 80°C for 2h under the condition of condensation and reflux, and then raise the temperature to 100°C for 4h to obtain viscous THICK BROWN LIQUID. The resulting liquid was filtered under reduced pressure to remove triethylamine hydrochloride to obtain a clear liquid. The filtrate was successively washed with 0.1 mol / L hydrochloric acid solution, saturated sodium carbonate solution and deionized water, then the toluene was removed under reduced pressure, and finally the product was obtained by drying in a vacuum oven. The hydroxyl value of the product was determined to be 145 mgKOH / g, and the acid value was 1.8 ...

Embodiment 2

[0027] Add 87.31 g of dibromoneopentyl glycol, 38.00 g of potassium carbonate and 60 g of xylene in the four-necked flask, and gradually heat up to 80 ° C. 2 Add 52.80g of phenylphosphoryl dichloride and 100g of xylene dropwise under the atmosphere, and control the dropwise addition in about 2 hours. After the dropwise addition, continue to react at 80°C for 2h under condensing and reflux conditions, and then raise the temperature to 100°C for 4h to obtain Viscous brown liquid. The resulting liquid was filtered under reduced pressure to remove solid matter to obtain a clear liquid. The filtrate was successively passed through 0.1 mol / L hydrochloric acid solution, saturated sodium carbonate solution, and deionized water to wash, then remove the solvent on a rotary evaporator, and finally dry in a vacuum oven to obtain the product. The hydroxyl value of the product was determined to be 54 mgKOH / g.

[0028] Take 50g of the above-mentioned flame-retardant polyester, 50g of polye...

example 3

[0030] Add 181.30g of tetrabromobisphenol A, 33.73g of triethylamine and 160g of N-methylpyrrolidone (NMP) to the four-necked flask, and gradually raise the temperature to 80°C. 2 Under the atmosphere, 29.83g of phenyl phosphorus dichloride and 60g of NMP were added dropwise. After the dropwise addition, the reaction was continued at 80°C for 4h, and then the temperature was raised to 100°C for 10h to obtain a viscous brown liquid. The resulting liquid was filtered to remove triethylamine hydrochloride to obtain a clear liquid. The filtrate was sequentially washed with 0.1 mol / L hydrochloric acid, saturated sodium carbonate solution and deionized water, then the solvent was removed on a rotary evaporator, and finally dried in a vacuum oven to obtain the product. The hydroxyl value of the product was determined to be 94 mgKOH / g.

[0031] Take 30g of the above-mentioned polyester and 70g of polyether polyol NJ220 into a three-necked flask. After vacuum dehydration at 90°C for 3...

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Abstract

The invention relates to the synthesis of novel phosphorus-containing halogen-containing response-type flame-retarding polyester polyol, and an application of the flame-retarding polyester polyol in polyurethane. The flame-retarding polyester polyol is formed from halogen-containing polyhydric alcohol and phosphorus oxychloride through a condensation polymerization reaction. The hydroxyl value ofthe obtained flame-retarding polyester polyol is 50-500mgKOH / g. The flame-retarding polyester polyol has advantages such as good fluidity, high reaction activity, and good compatibility with other compounds such as polyether glycol and polyester polyol. When the flame-retarding polyester polyol is applied in rigid polyurethane foam, flexible polyurethane foam, polyurethane elastomer or other polyurethane materials, flame-retarding capacities of the materials can be greatly improved, and migration does not occur, such that a purpose of permanent flame-retardance is achieved.

Description

technical field [0001] The invention relates to the preparation of a novel flame-retardant polyester polyol for polyurethane. Background technique [0002] Polyurethane materials have various excellent properties such as shock absorption, heat insulation, sound absorption, and wear resistance, and are widely used in industrial production and daily life. However, like other polymers, polyurethane materials without flame retardant treatment are flammable materials, thus limiting the application of polyurethane materials. Therefore, improving the flame retardancy of polyurethane materials has become a hot spot in the field of polyurethane research. [0003] Compared with additive flame retardants, reactive flame retardants have the advantages of less addition, less impact on the mechanical properties of materials, and good flame retardancy durability, so they are widely used. The Chinese patent application No. 200510122057.X uses dibromoneopentyl glycol as a flame retardant a...

Claims

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Application Information

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IPC IPC(8): C08G79/04C08L75/04C08L85/02
Inventor 王贵友张伟丁学文晏义青
Owner EAST CHINA UNIV OF SCI & TECH
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