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Method for preparing phosphorous-nitrogen synergistic wood fire retardant

A flame retardant and wood technology, applied in the field of flame retardants, can solve the problems that cannot fully meet the needs of the market, and achieve the effects of improving chemical atom utilization, high flame retardant efficiency, and reducing side effects such as salting out and hygroscopicity Effect

Active Publication Date: 2016-05-04
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

The current wood flame retardants cannot fully meet the needs of the market due to the limitations of factors such as process, cost and effect.

Method used

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  • Method for preparing phosphorous-nitrogen synergistic wood fire retardant
  • Method for preparing phosphorous-nitrogen synergistic wood fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for preparing a phosphorus-nitrogen synergistic wood flame retardant, characterized in that the method comprises the following steps:

[0029] (1) Preparation of reaction equipment: Install a stirrer, a high-efficiency reflux condenser in a 250ml reactor, and install a drying tube and an HCL absorption device on the top of the condenser;

[0030] (2) Take 15.75g (0.1mol) of trimethylolmethylamine hydrochloride and 80ml of dioxane and place them in the reactor of step (1), drive out the air in the reactor with nitrogen, and lower the temperature of the reaction system Cool down to below 10°C, drop 15.35g (0.1mol) phosphorus oxychloride into the reactor, control the reaction temperature not higher than 20°C during the dropping process, and raise the temperature to 85°C within 1 hour after the dropping, Insulation reaction at this temperature for 5 hours, after the generated HCL is exhausted, the reaction solution a is obtained;

[0031] Lower the temperature of ...

Embodiment 2

[0034] A method for preparing a phosphorus-nitrogen synergistic wood flame retardant, characterized in that the method comprises the following steps:

[0035] (1) Preparation of reaction equipment: Install a stirrer, a high-efficiency reflux condenser in a 250ml reactor, and install a drying tube and an HCL absorption device on the top of the condenser;

[0036] (2) Take 15.75g (0.1mol) of trimethylolmethylamine hydrochloride and 100ml of diethylene glycol dimethyl ether and place them in the reactor of step (1), drive out the air in the reactor with nitrogen, and put Cool the temperature of the reaction system to below 10°C, add 15.35g (0.1mol) phosphorus oxychloride dropwise into the reactor, control the reaction temperature not higher than 20°C during the dropping process, and raise the temperature to 100°C within 1 hour after the dropwise addition °C, keep the reaction at this temperature for 4 hours, and after the generated HCL is exhausted, the reaction solution a is obt...

Embodiment 3

[0040] A method for preparing a phosphorus-nitrogen synergistic wood flame retardant, characterized in that the method comprises the following steps:

[0041] (1) Preparation of reaction equipment: Install a stirrer, a high-efficiency reflux condenser in a 250ml reactor, and install a drying tube and an HCL absorption device on the top of the condenser;

[0042] (2) Take 15.75g (0.1mol) of trimethylolmethylamine hydrochloride and 110ml of tetrahydrofuran and place them in the reactor of step (1), drive out the air in the reactor with nitrogen, and cool the temperature of the reaction system to 10 Below ℃, drop 15.35g (0.1mol) phosphorus oxychloride into the reactor, control the reaction temperature not higher than 20℃ during the dropping process, and raise the temperature to 65℃ within 1 hour after the dropping, at this temperature Insulation reaction for 6 hours, after the generated HCL is exhausted, the reaction solution a is obtained;

[0043]Lower the temperature of the r...

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Abstract

The invention discloses a method for preparing a phosphorous-nitrogen synergistic wood fire retardant. The method includes the steps that trihydroxymethylaminomethane hydrochloride and phosphorus oxychloride are mixed in organic solvent at the temperature of 20 DEG C; the temperature is increased to 65-100 DEG C for heat preservation reaction for four to six hours, then the temperature is decreased, and an acid-binding agent of the equal mole is added; cooling and filtering are conducted, phosphoric acid is added into filtrate, filtering is conducted again, and vacuum drying is performed on a filter cake to obtain solid caged white amine phosphate hydrophosphate; and then water is added, tetrakis hydroxymethyl phosphonium phosphate and dodecy dimethyl benzyl ammonium bromide are added separately, and the pH of fire retardant liquid is adjusted to be 5 to 7.5 through ammonium hydroxide or phosphoric acid to obtain the product of the phosphorous-nitrogen synergistic wood fire retardant. The preparation method is simple, low in cost and free of pollution, the product is high in penetrability, good in durability and corrosion prevention function, high in fire-retarding effectiveness and convenient to apply, and large-scale production is easy.

Description

technical field [0001] The patent of the invention relates to the technical field of flame retardants such as wood, fiber, paper, coatings, etc., and specifically relates to a preparation method of a phosphorus-nitrogen synergistic wood flame retardant. Background technique [0002] With the advancement of science and technology and the improvement of people's living standards, the degree of lignification of home furniture, floors and other decorations is getting higher and higher, and the fire hazards and threats that follow are getting bigger and bigger, which greatly promotes the improvement of people's awareness of fire safety. , especially the fire protection and safety protection of antique buildings and wooden structure houses of ethnic minorities in my country is more urgent. Due to the limitations of factors such as process, cost and effect, the current wood flame retardants cannot fully meet the needs of the market. Contents of the invention [0003] Aiming at th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B27K3/52
CPCB27K3/52
Inventor 王彦林沈敏杰陈秀丽韩虹
Owner 河南森远科技有限公司
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