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A kind of preparation method of intumescent flame retardant of phosphorus, nitrogen and carbon trinity

An intumescent flame retardant and trinity technology, which is applied in the field of intumescent flame retardants with phosphorus, nitrogen and carbon trinity, can solve the problems of high reactivity of phosphorus oxychloride, high viscosity of esterification products, difficult operation, etc., and save raw materials. , Good compatibility and easy operation

Inactive Publication Date: 2011-12-21
HUAZHONG UNIV OF SCI & TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above-mentioned patents, due to the high reactivity of phosphorus oxychloride, a large excess of phosphorus oxychloride is required, and the excessive amount of phosphorus oxychloride needs to be evaporated during the preparation process, which consumes a lot of energy, and the esterification product has a high viscosity, which is difficult to operate and yield. low rate

Method used

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  • A kind of preparation method of intumescent flame retardant of phosphorus, nitrogen and carbon trinity
  • A kind of preparation method of intumescent flame retardant of phosphorus, nitrogen and carbon trinity
  • A kind of preparation method of intumescent flame retardant of phosphorus, nitrogen and carbon trinity

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Embodiment 1

[0037]Disperse 30g of hexamethylolmelamine in 50mL of chlorobenzene, slowly add 45g of phosphorus oxychloride dropwise at 60°C for esterification, and obtain an esterified product dispersed in chlorobenzene. 100 mL of water was added to the above organic solution, and stirred at room temperature for 2 hours. After the stirring was stopped, the organic phase and the aqueous phase were separated, and the hydrolyzate was dissolved in the aqueous phase. Add 40 g of melamine to the aqueous solution of the hydrolyzate, react in a water bath at 70° C. for 60 minutes, and a white precipitate is formed. The pH was adjusted to 7 with liquid caustic soda, cooled and placed, then dehydrated and dried to obtain the final product.

Embodiment 2

[0039] Disperse 55g of phosphorus pentachloride in 80ml of carbon tetrachloride, and slowly add 30g of hexamethylolmelamine at 80°C for esterification to obtain an esterified product dispersed in carbon tetrachloride. 120ml of water was added to the above organic solution, and stirred at room temperature for 2 hours. After the stirring was stopped, the obtained hydrolyzate was dissolved in the water phase, the organic phase and the water phase were separated, and carbon tetrachloride was recovered. Finally, 35 g of melamine was added to the aqueous solution of the hydrolyzate, reacted in a water bath at 90°C for 90 minutes, adjusted to pH 5 with soda ash, washed with water after cooling, dehydrated and dried to obtain the final product.

Embodiment 3

[0041] Disperse 30kg of hexamethylolmelamine in 50L of chlorobenzene in a reaction kettle, slowly add 45kg of phosphorus oxychloride dropwise at 60°C to undergo esterification reaction, and obtain an esterified product dispersed in chlorobenzene. 100 L of water was added to the above organic solution, and stirred at room temperature for 2 hours. After the stirring was stopped, the organic phase and the aqueous phase were separated, and the hydrolyzate was dissolved in the aqueous phase. Add 40 kg of melamine to the hydrolyzate aqueous solution, stir at 70° C. for 60 minutes, and a white precipitate is formed. The pH was adjusted to 6 with ammonia water, left to cool, and then centrifuged and dried to obtain the final product.

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Abstract

The invention provides a new method for preparing a phosphorus-nitrogen-carbon trinity intumescent flame retardant with hexamethylolmelamine, melamine and phosphorus halide as the main raw materials and an inert organic solvent as the reaction medium. The reaction of methylol melamine and phosphorus halide in an inert organic solvent to obtain an esterification product; then adding water to the esterification product for hydrolysis, after the organic phase and the aqueous phase are separated, the organic phase is separated to obtain a hydrolyzate solution; the hydrolyzate Melamine is added to the solution to form a salt, and a white precipitate is produced to obtain hexamethylol melamine phosphate melamine salt. The compound molecule contains three elements of phosphorus, nitrogen and carbon, that is, an intumescent flame retardant of the trinity of phosphorus, nitrogen and carbon. Since an inert organic solvent is used as the reaction medium, the preparation method is convenient to operate and is conducive to realizing industrial production. Excellent combustion performance.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and relates to a preparation method of a flame retardant, in particular to a trinity compound of phosphorus, nitrogen and carbon synthesized by using hexamethylol melamine, melamine and phosphorus halide as main raw materials and using an inert organic solvent as a reaction medium. A new approach to intumescent flame retardants. technical background [0002] Flame retardants are a class of functional additives that impart flame retardancy to flammable polymers. Among them, the most commonly used is the halogenated flame retardant, but it will release toxic gas when heated, which brings non-negligible harm to the environment and human health. Phosphorus-nitrogen flame retardants are a new generation of high-efficiency and environmentally friendly halogen-free flame retardants. This type of flame retardant does not release toxic gases when heated, and has good compatibility with o...

Claims

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Application Information

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IPC IPC(8): C07F9/6584C07D251/56C08K7/22C08K5/527C08L23/06C08L23/12C08L75/04
Inventor 陈芳寇江勇李琳
Owner HUAZHONG UNIV OF SCI & TECH
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