Method for increasing yield and polymerization degree of polymeric phosphorus-nitrogen intumescent flame retardant

A technology of intumescent flame retardant and degree of polymerization, which is applied in the field of preparation of polymeric flame retardants, can solve the problems of complex purification process of synthetic products, structural characterization of synthetic products, failure to achieve the use effect, etc., and achieve simplified post-processing procedures, excellent Mechanical properties, beneficial to the effect of industrial production

Active Publication Date: 2017-02-15
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the degree of polymerization of the synthesized compound is low, and the expected use effect cannot be achieved. In addition, the yield is very low
A large amount of organic solvents are used in the synthesis process, so that the purity of the obtained product is low, and the purification process of the synthetic product is too complicated
Because the amount of phosphorus oxychloride used is too large, it will seriously corrode the synthesis equipment, even endanger human health and pollute the environment
In addition, the above-mentioned patents did not carry out structural characterization of the synthetic product, which is not convincing

Method used

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  • Method for increasing yield and polymerization degree of polymeric phosphorus-nitrogen intumescent flame retardant
  • Method for increasing yield and polymerization degree of polymeric phosphorus-nitrogen intumescent flame retardant
  • Method for increasing yield and polymerization degree of polymeric phosphorus-nitrogen intumescent flame retardant

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Experimental program
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Effect test

Embodiment 1

[0039] Step 1: Under the protection of nitrogen, add 6.8g (0.05mol) of just ground pentaerythritol (PER), 23.1g (0.15mol) of just distilled phosphorus oxychloride (POCl) to a 500ml container 3 ) and 0.72g aluminum trichloride (AlCl 3 ). Connect the above-mentioned reaction vessel with a thermometer, a mechanical stirrer, a reflux condenser and a tail gas absorption device. Mix at room temperature first, and the rotation speed of the stirring blade is 230r / min. After the system is uniformly mixed, slowly raise the temperature to 80°C until the reaction is complete, that is, no hydrogen chloride gas appears. After the reaction, the excess phosphorus oxychloride solvent was recovered by distillation with a rotary evaporator, and the obtained residue was washed with dichloromethane, filtered, and recrystallized in glacial acetic acid after repeated several times. Dry at 120°C to constant weight to obtain 13.5 g of white intermediate pentaerythritol diphosphate diphosphoryl chlor...

Embodiment 2

[0047] Step 1: Under the protection of nitrogen, add 6.8g (0.05mol) of freshly ground PER, 30.6g (0.20mol) of freshly distilled POCl into a 500ml container 3 and 0.74g AlCl 3 , connect the above-mentioned reaction vessel with a thermometer, a mechanical stirrer, a reflux condenser and an exhaust gas absorption device. Mix at room temperature first, and the rotation speed of the stirring blade is 230r / min. After the system is uniformly mixed, slowly raise the temperature to 75°C until the reaction is complete, that is, no hydrogen chloride gas appears. After the reaction, the excess POCl was recovered by distillation with a rotary evaporator 3 Solvent, the obtained residue was washed with dichloromethane, filtered, and after repeated several times, recrystallized in glacial acetic acid, and the recrystallized product was dried in a blast oven at 120°C to constant weight to obtain a white intermediate SPDPC 13.7 g, the yield is 92.3%, and the purity is 98.6%;

[0048] Step 2:...

Embodiment 3

[0050] Step 1: Under the protection of nitrogen, add 6.8g (0.05mol) of freshly ground PER, 30.6g (0.20mol) of freshly distilled POCl into a 500ml container 3 and 0.74g AlCl 3 . Connect the above-mentioned reaction vessel with a thermometer, a mechanical stirrer, a reflux condenser and a tail gas absorption device. Mix at room temperature first, and the rotation speed of the stirring blade is 230r / min. After the system is uniformly mixed, slowly raise the temperature to 60°C until the reaction is complete, that is, no hydrogen chloride gas appears. After the reaction, the excess POCl was recovered by distillation with a rotary evaporator 3 Solvent, the obtained residue was washed with dichloromethane, filtered, and after repeated several times, recrystallized in glacial acetic acid, and the recrystallized product was dried in a blast oven at 120°C to constant weight to obtain a white intermediate SPDPC 13.6 g, the yield is 91.6%, and the purity is 98.3%;

[0051] Step 2: Un...

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Abstract

The invention relates to a method for increasing the yield and the polymerization degree of a polymeric phosphorus-nitrogen intumescent flame retardant, and belongs to the technical field of preparation of polymeric flame retardants. Phosphorus oxychloride, pentaerythritol and a catalyst AlCl3 are uniformly mixed at normal temperature, and a crude intermediate pentaerythritol diphosphate diphosphoryl chloride (SPDPC) is obtained; high-purity SPDPC obtained in the step 1, 4,4-diamino diphenyl sulfone and an acid binding agent are added into an organic solvent, after the materials are stirred and mixed to be uniform, a temperature increasing reaction is conducted in two stages, and the polymeric phosphorus-nitrogen intumescent flame retardant is obtained. In the synthetic process of the method, the reactants serve as a reaction solvent, therefore, the using amount of the solvent is decreased, and the aftertreatment procedure is greatly simplified; meanwhile, reverse precipitation operation and recrystallization operation are conducted on the product, and therefore the purity of the obtained product is high.

Description

technical field [0001] The invention relates to a method for increasing the yield and degree of polymerization of a polymeric phosphorus-nitrogen expansion flame retardant, and belongs to the technical field of preparation of polymeric flame retardants. Background technique [0002] Since the 1980s, with the demand for safe application of polymer materials, flame retardants have become one of the important additives for flame retardant modification of polymer materials. Among the existing flame retardants, although the traditional halogenated flame retardants have high flame retardant efficiency and have little influence on the inherent properties of the matrix material, they will produce a lot of smoke, corrosive gases and some toxic gases during thermal decomposition and combustion. Substances have a serious impact on human health and at the same time cause certain environmental pollution. Therefore, the replacement of halogen-based flame retardants by halogen-free green ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C08L85/02
Inventor 王银杰苏岩刘吉平
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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