Cellulose-based nitrogen-phosphorus flame retardant and preparation method thereof

A nitrogen-phosphorus-based and cellulose-based technology is applied in the field of cellulose-based nitrogen-phosphorus flame retardants and their preparation, which can solve the problems of generating more smoke and corrosive gases, insufficient heat resistance, and high volatility. Achieve the effect of excellent flame retardant performance, high nitrogen and phosphorus content, and wide application prospects

Active Publication Date: 2017-01-11
珠海菲伯过滤材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The easiest and quickest method for flame retardant materials is to use flame retardant blending. At present, the total consumption of flame retardants in the world has reached 1.2 million tons per year, and it will continue to grow at an average annual rate of 4-5% in the next few years. However, the current The use of flame retardants in our country is still not popular. Domestic flame retardant plastics account for less than 2% of plastic products. Among them, halogen flame retardants are the main ones. A lot of smoke and corrosive gas, and troubled by the dioxin problem, the use of halogenated flame retardants has been more and more restricted. In the long run, the non-halogenated flame retardant is the ultimate goal of the development Target
Phosphorus and nitrogen flame retardants are only used as additive flame retardants, generally have high volatility and insufficient heat resistance. The phosphorus and nitrogen content of flame retardants is roughly proportional to the flame retardant effect. Solid phosphorus-nitrogen flame retardants with good compatibility and excellent flame retardant effect are the main direction of current research

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Under the condition of stirring at a speed of 200 rpm, 100 g of hydroxypropyl cellulose with a moisture content of less than 1 wt.% was dissolved in 500 g of dichloromethane, and 10 g of ethylenediamine was added as an acid-binding agent and nitrogen was introduced; the temperature was raised to After 80°C, add 80g of phosphorus oxychloride dropwise to the above solution and continue to stir for 6 hours; add a large amount of water to wash until there is no chloride ion (use 0.1mol / L silver nitrate aqueous solution for identification), and then add 500g of water as Solvent, after heating up to 65°C, add 20g of melamine and continue to stir for 6 hours; add ice cubes to cool down and filter to remove unreacted melamine, and distill the aqueous solution to remove water under reduced pressure, dry at 80°C to obtain a cellulose-based nitrogen-phosphorus flame retardant . The performance results of the prepared flame retardant are shown in the attached table.

Embodiment 2

[0035] Under the condition of stirring at a speed of 300 rpm, 100g of hydroxypropyl methylcellulose with a water content of less than 1wt.% was dissolved in 500g of chloroform, and 10g of pyridine was added as an acid-binding agent and nitrogen gas was introduced; the temperature was raised to After 80°C, add 200g of phosphorus oxychloride dropwise to the above mixture and continue to stir for 6 hours; add a large amount of water to rinse until no chloride ions exist (use 0.1mol / L silver nitrate aqueous solution for identification), and then add 1000g of water As a solvent, after heating up to 65°C, add 30g of melamine and continue to stir for 6 hours; add ice cubes to cool down and filter to remove unreacted melamine, then distill the water solution under reduced pressure to remove water, and dry at 90°C to obtain a cellulose-based nitrogen-phosphorus flame retardant agent. The performance results of the prepared flame retardant are shown in the attached table.

Embodiment 3

[0037]Dissolve 100g of methylcellulose with a moisture content of less than 1wt.% in 500g of acetonitrile under stirring at a speed of 500 rev / min, add 5g of 4-dimethylaminopyridine as an acid-binding agent and feed nitrogen; heat up to 80 After ℃, add 120g of phosphorus oxychloride dropwise to the above mixture and keep stirring for 6 hours; add a large amount of water to wash until no chloride ions exist (use 0.1mol / L silver nitrate aqueous solution for identification), and then add 500g of water as Solvent, after heating up to 65°C, add 10g of dicyandiamide and continue to stir for 6 hours; add ice cubes to cool down and filter to remove unreacted dicyandiamide, and distill the water solution under reduced pressure to remove water, dry at 100°C to obtain cellulose-based nitrogen phosphorus Department of flame retardants. The performance results of the prepared flame retardant are shown in the attached table.

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Abstract

The invention relates to a cellulose-based nitrogen-phosphorus flame retardant and a preparation method thereof. The preparation method comprises the following steps: dissolving a cellulose derivative into a solvent under the stirring condition that the speed is 100-1000 revolutions per minute so as to form uniform phases, adding micromolecule amine compounds as an acid-binding agent, and introducing nitrogen, wherein the water content of the cellulose derivative is less than 1%; dropwise adding phosphorus oxychloride into the solution, and continuously stirring for 1-10 hours while the reaction temperature is maintained at 25-100 DEG C; washing until no chloride ion exists, adding amino compounds into water which serves as a solvent according to the solid-to-liquid ratio of (1 to 1)-(1 to 50), and continuously stirring for 1-10 hours while the reaction temperature is maintained at 25-100 DEG C; filtering and drying to obtain the cellulose-based nitrogen-phosphorus flame retardant, wherein the drying temperature is 40-100 DEG C. The cellulose-based nitrogen-phosphorus flame retardant and the preparation method of the cellulose-based nitrogen-phosphorus flame retardant are environmentally friendly, and the preparation method is easy, convenient and feasible.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a cellulose-based nitrogen-phosphorus flame retardant and a preparation method thereof. Background technique [0002] China's major fires have continued in recent years, which is very important to the development and production of flame-retardant building materials. With the further improvement of energy-saving heat preservation and flame-retardant performance indicators of building materials in my country, the demand for flame-retardant and fire-resistant materials will further increase. The easiest and quickest method for flame retardant materials is to use flame retardant blending. At present, the total consumption of flame retardants in the world has reached 1.2 million tons per year, and it will continue to grow at an average annual rate of 4-5% in the next few years. However, the current The use of flame retardants in our country is still not popular. D...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/06C09K21/14
Inventor 陈日清南静娅刘娟李双王春鹏储富祥
Owner 珠海菲伯过滤材料有限公司
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