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A preparation method of phosphorus, nitrogen and boron multi-element synergistic wood flame retardant

A synergistic flame retardant, multi-element technology, applied in the field of wood flame retardants, can solve the problem of not fully meeting the needs of the market, and achieve the effect of improving the utilization rate of chemical atoms, strong penetration, and easy availability of raw materials

Active Publication Date: 2017-03-29
河南森远科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as the current flame retardants for wood and fiber are concerned, due to the limitations of factors such as process, cost and effect, they cannot fully meet the needs of the market.

Method used

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  • A preparation method of phosphorus, nitrogen and boron multi-element synergistic wood flame retardant
  • A preparation method of phosphorus, nitrogen and boron multi-element synergistic wood flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for preparing a phosphorus, nitrogen and boron multi-element synergistic wood flame retardant, comprising the following steps:

[0030] (1) Preparation of reaction equipment: install conventional stirrer, thermometer and fractionation device in a 250ml three-necked flask;

[0031] (2) Take 12.1g of trimethylolmethylamine, 14.01g of trimethyl phosphate and 60ml of dioxane in step (1) in a 250ml three-neck flask, heat to reflux, the reflux temperature is 102°C, and the reflux time is 12h. And control the temperature of the top of the column to not be higher than 65° C. through the fractionation device, continuously fractionate the methanol generated by the reaction until the fractionated methanol reaches the theoretical amount, and obtain the reaction solution a;

[0032] (3) Cool the reaction solution a obtained in step (2) to below 40°C, add dropwise 5.76g of phosphoric acid with a concentration of 85% by mass, stir for 1h, filter, and vacuum-dry the filter cak...

Embodiment 2

[0035] A method for preparing a phosphorus, nitrogen and boron multi-element synergistic wood flame retardant, comprising the following steps:

[0036] (1) Preparation of reaction equipment: install conventional stirrer, thermometer and fractionation device in a 250ml three-necked flask;

[0037] (2) Take 12.1g of trimethylolmethylamine, 18.21g of triethyl phosphate and 80ml of diethylene glycol dimethyl ether in step (1) 250ml three-neck flask, heat to reflux, the reflux temperature is 110°C, reflux The time is 11 hours, and the temperature of the column top is controlled by the fractionation device to be not higher than 78.5°C, and the ethanol generated by the reaction is continuously fractionated until the ethanol fractionated reaches the theoretical amount, and the reaction solution a is obtained;

[0038] (3) Cool the reaction solution a obtained in step (2) to below 40°C, add dropwise 5.76g of phosphoric acid with a concentration of 85% by mass, stir for 1h, filter, and ...

Embodiment 3

[0041] A method for preparing a phosphorus, nitrogen and boron multi-element synergistic wood flame retardant, comprising the following steps:

[0042] (1) Preparation of reaction equipment: install conventional stirrer, thermometer and fractionation device in a 250ml three-necked flask;

[0043] (2) Take 12.1g of trimethylolmethylamine, 22.42g of tri-n-propyl phosphate and 80ml of dimethyl sulfoxide, put them in a 250ml three-neck flask in step (1), heat to reflux, the reflux temperature is 130°C, and the reflux time is 9h , and the temperature of the column top is controlled by a fractionation device to be no higher than 97.7° C., and the n-propanol generated by the reaction is continuously fractionated until the fractionated n-propanol reaches the theoretical amount, and the reaction solution a is obtained;

[0044] (3) Cool the reaction solution a obtained in step (2) to below 40°C, add dropwise 5.76g of phosphoric acid with a concentration of 85% by mass, stir for 1h, fil...

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Abstract

The invention relates to a preparation method of a wood fire retardant with synergized multiple elements of phosphorus, nitrogen and boron. The preparation method comprises the following steps that firstly, a conventional stirrer, a thermometer and a fractionating device are arranged in a reactor; secondly, trihydroxymethyl aminomethane, phosphotriester and an organic solvent are weighed, placed in the reactor and heated till backflow, the temperature of the top of a column of the fractionating device is controlled to be the boiling temperature of fractionated alcohol, and the alcohol generated in a reaction is fractionated continuously until the fractionated alcohol reaches a theoretical quantity; thirdly, the temperature is lowered to below 40 DEG C, phosphoric acid with the mass percent concentration being 85% is added dropwise, stirring, filtering and vacuum drying of a filter cake are conducted, and caged phosphoric acid ester amine hydrogen phosphate is obtained; and finally, the caged phosphoric acid ester amine hydrogen phosphate is dissolved in water, boric acid is added for dissolution, then tetrakis(hydroxymethy) phosphate and tri(hydroxymethyl) alkyl phosphonium bromide are added in sequence and evenly stirred, the pH of the flame retarding liquid is adjusted with ammonium hydroxide or phosphoric acid to range from 6.5 to 8.5, and then the wood fire retardant is obtained. The preparation method is simple and free of pollution, the fire retarding efficiency is high, and large-scale production is easy.

Description

technical field [0001] The invention belongs to the technical field of wood flame retardants, which are widely used in wood, fiber, paper, paint, etc., and specifically relates to a preparation method of a phosphorus, nitrogen and boron multi-element synergistic wood flame retardant. Background technique [0002] In recent years, the rapid development of science and technology has greatly improved people's living standards. There are more and more wood and fibers for home furniture, floors, walls and other decorations. Due to their flammability, the ensuing fire More and more, it has greatly promoted the improvement of people's fire safety awareness, especially the fire protection and safety protection of antique buildings, wooden structure houses and high-rise buildings of ethnic minorities in my country is more urgent. As far as the current fire retardants for wood and fiber are concerned, due to the limitations of factors such as process, cost and effect, they cannot fully...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6581C09K21/12B27K3/52
CPCB27K3/52B27K2240/30
Inventor 王令端沈敏杰徐元清王彦林
Owner 河南森远科技有限公司
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