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Phosphorus-nitrogen synergistic flame-retardant polyalcohol and preparation method thereof

A synergistic flame retardant and polyol technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Inexpensive, practical and easy to operate

Inactive Publication Date: 2014-08-13
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problems in the prior art that a single flame retardant element cannot meet the performance requirements in many cases with the improvement of flame retardant requirements, and utilize the synergistic effect between different types of flame retardant elements to provide a phosphorus Nitrogen synergistic flame retardant polyol and preparation method thereof

Method used

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  • Phosphorus-nitrogen synergistic flame-retardant polyalcohol and preparation method thereof
  • Phosphorus-nitrogen synergistic flame-retardant polyalcohol and preparation method thereof
  • Phosphorus-nitrogen synergistic flame-retardant polyalcohol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of trihydroxymethylphosphine oxide (THPO)

[0032] In a 1L three-necked flask equipped with a stirrer, a constant pressure dropping funnel, and a condenser, add 40.0 g (1 mol) of NaOH and 400 mL of distilled water, and stir to completely dissolve the alkali. After it was cooled to room temperature, 190.1 g (1 mol) of tetrakishydroxymethylphosphonium chloride solution was added dropwise through a constant pressure funnel. Dropping time 1h, 50 ℃ reaction 5h. After the reaction, slowly add HCl solution dropwise to the solution, after adjusting the pH to neutral, add 19mL HCl solution 2 o 2 After reacting for 2 hours, use a rotary evaporator to evaporate most of the water, then pour it into a 1L beaker containing 400mL of ethanol, and let it stand overnight until the salt is fully separated, then filter it with suction. The solvent is spin-dried to obtain the product THPO. And carried out infrared characterization, such as figure 1 shown.

[0033] (2) ...

Embodiment 2

[0036] (1) Preparation of trihydroxymethylphosphine oxide

[0037] Add 85.5g (0.5mol) Ba(OH) 2 , and add 300mL of distilled water, stir to dissolve the base completely. After it was cooled to room temperature, 190.1 g (1 mol) of tetrakishydroxymethylphosphonium chloride solution was added dropwise through a constant pressure funnel. Dropping time 1h, 70 ℃ reaction 4h. After the reaction was completed, HCl solution was slowly added dropwise to the solution to adjust the pH to neutral. Add 19mLH 2 o 2 After reacting for 2 hours, use a rotary evaporator to evaporate most of the water, then pour it into a 1L beaker containing 300mL of ethanol, and let it stand overnight until the salt is fully separated, then filter it with suction. The solvent is spin-dried to obtain the product.

[0038] (2) Preparation of Phosphorus Nitrogen Synergistic Flame Retardant Polyols

[0039] Experimental procedure 2 is the same as embodiment 1.

Embodiment 3

[0041] (1) Preparation of trihydroxymethylphosphine oxide

[0042]In a 1L three-necked flask equipped with a stirrer, a constant pressure dropping funnel, and a condenser, add 40.0 g (1 mol) of NaOH and 400 mL of distilled water, and stir to completely dissolve the alkali. After it was cooled to room temperature, 190.1 g (1 mol) of tetrakishydroxymethylphosphonium chloride solution was added dropwise through a constant pressure funnel. Dropping time 1h, 60 ℃ reaction 5h. After the reaction was completed, HCl solution was slowly added dropwise to the solution to adjust the pH to neutral. Add 19mLH 2 o 2 After reacting for 2 hours, use a rotary evaporator to evaporate most of the water, then pour it into a 1L beaker containing 400mL of ethanol, and let it stand overnight until the salt is fully separated, then filter it with suction. The solvent was spin-dried to obtain the product.

[0043] (2) Preparation of Phosphorus Nitrogen Synergistic Flame Retardant Polyols

[0044...

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Abstract

The invention discloses phosphorus-nitrogen synergistic flame-retardant polyalcohol and a preparation method thereof, relating to the synthesis of flame-retardant polyalcohol. The preparation method of the phosphorus-nitrogen synergistic flame-retardant polyalcohol comprises the following steps: 1) with quaternary phosphorus salt as a raw material, adding alkali and stirring for reacting, filtering and separating the salt generated by reacting, then oxidizing with a hydrogen peroxide solution, and performing reduced-pressure distillation for removing moisture to obtain tris(hydroxymethyl)phosphine oxide; 2) performing an ether exchange reaction between hexakis(methoxymethyl)melamine and the tris(hydroxymethyl)phosphine oxide obtained in the step 1) at 50-100 DEG C in the presence of an acid catalyst, and reducing pressure for removing small-molecular methanol to obtain the phosphorus-nitrogen synergistic flame-retardant polyalcohol. The prepared phosphorus-nitrogen synergistic flame-retardant polyalcohol is formed by connecting phosphorus elements through phosphorus-carbon bonds, and the weakness that the phosphorus-carbon bonds (phosphorus-ester bonds) are hydrolyzed easily is avoided, thus the phosphorus-nitrogen synergistic flame-retardant polyalcohol has the characteristic of relatively high hydrolysis resistance.

Description

technical field [0001] The invention relates to the synthesis of a flame-retardant polyol, in particular to a reactive phosphorus-nitrogen synergistic flame-retardant polyol and a preparation method thereof. Background technique [0002] Polyurethane material is one of the most widely used polymer materials in the world, and the global annual consumption is estimated to be more than 3.5 million tons. The preparation of polyurethane materials is known for its low energy consumption. It has the advantages of good heat insulation, oil resistance, cold resistance, moisture resistance and dimensional stability. It has become an indispensable material for shock resistance, liners and heat preservation. It is widely used in the automobile industry and home appliances. industry etc. However, polyurethane materials are flammable in the air, and the oxygen index of flexible foam plastics is only 17% to 18%, and a large amount of smoke and dust are generated when burning, which greatl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6521C08G18/32
Inventor 戴李宗刘诚陈国荣袁丛辉许一婷罗伟昂曾碧榕常迎毛杰
Owner XIAMEN UNIV
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