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Macromolecular intumescent flame retardant with phosphorus and nitrogen and synthesis method thereof

An intumescent flame retardant and a synthesis method technology, applied in the field of intumescent halogen-free flame retardants, can solve the problems of large molecular weight, etc., and achieve the effects of no halogen, good compatibility, and high carbon-forming properties

Active Publication Date: 2011-06-15
ANHUI ZHONGDING SEALING PARTS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of phosphorus and nitrogen macromolecular expansion type flame retardant, its molecular weight is big, can reach about 2000g / mol, and the compatibility with matrix is ​​better, and char formation is higher, basically can solve Problems such as migration, precipitation or volatilization during the processing and molding of flame retardants and polymers overcome the shortcomings of existing intumescent flame retardants, and are halogen-free and environmentally friendly

Method used

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  • Macromolecular intumescent flame retardant with phosphorus and nitrogen and synthesis method thereof
  • Macromolecular intumescent flame retardant with phosphorus and nitrogen and synthesis method thereof
  • Macromolecular intumescent flame retardant with phosphorus and nitrogen and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] (1) Add 59.4g of chlorinated spirocyclic phosphate and 100mL of acetonitrile into a 250mL reactor equipped with a nitrogen protection and stirring device, heat to 50°C to 60°C and keep stirring to completely dissolve the chlorinated spirocyclic phosphate in Acetonitrile solvent;

[0023] (2) Get 19g of 2,6-diaminopyridine and dissolve it in 60mL of acetonitrile solvent to make a concentration of 2.9mol / L containing 2,6-diaminopyridine in acetonitrile solution, which contains 2,6-diaminopyridine The acetonitrile solution is added dropwise in the solution of step (1) gained;

[0024] (3) Add 15 mL of catalyst pyridine dropwise into the solution obtained in step (2), raise the temperature to 80° C. and react for 4 hours, during which light yellow powder is continuously formed;

[0025] (4) Cool to room temperature, filter the reaction product, and wash the filter cake repeatedly with ethanol for 3 to 5 times to purify the product;

[0026] (5) Vacuum drying at 80°C for 1...

Embodiment 2

[0028] (1) Add 59.4g of chlorinated spirocyclic phosphate and 120mL of acetonitrile into a 250mL reactor equipped with a nitrogen protection and stirring device, heat to 50°C to 60°C and keep stirring to completely dissolve the chlorinated spirocyclic phosphate in Acetonitrile solvent;

[0029] (2) Get 21g of 2,6-diaminopyridine and dissolve it in 40mL of acetonitrile solvent to make a concentration of 4.9mol / L containing 2,6-diaminopyridine in acetonitrile solution, which contains 2,6-diaminopyridine The acetonitrile solution is added dropwise in the solution of step (1) gained;

[0030] (3) Add 20 mL of catalyst triethylamine dropwise into the solution obtained in step (2), raise the temperature to 80° C. and react for 6 hours, during which light yellow powder is continuously formed;

[0031] (4) Cool to room temperature, filter the reaction product, and wash the filter cake repeatedly with water for 3 to 5 times to purify the product;

[0032] (5) Vacuum drying at 80°C fo...

Embodiment 3

[0034] (1) Add 29.7g of chlorinated spirocyclic phosphate and 80mL of acetonitrile into a 250mL reactor equipped with a nitrogen protection and stirring device, heat to 50°C to 60°C and keep stirring to completely dissolve the chlorinated spirocyclic phosphate in Acetonitrile solvent;

[0035] (2) Get 9.5g of 2,6-diaminopyridine and dissolve it in 80mL of acetonitrile solvent to make a concentration of 1.1mol / L containing 2,6-diaminopyridine in acetonitrile solution, which contains 2,6-diaminopyridine The acetonitrile solution of pyridine is added dropwise in the solution obtained in step (1);

[0036] (3) Add 10 mL of catalyst pyridine dropwise into the solution obtained in step (2), raise the temperature to 80° C. and react for 3 hours, during which light yellow powder is continuously formed;

[0037] (4) Cool to room temperature, filter the reaction product, and wash the filter cake repeatedly with ethanol for 3 to 5 times to purify the product;

[0038] (5) Vacuum drying...

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Abstract

The invention discloses a macromolecular intumescent flame retardant with phosphorus and nitrogen and a synthesis method thereof. The synthesis method comprises the following steps: using acetonitrile as solvent and 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro-3,9-dioxa[5.5]undecane and 2,6-diaminopyridine as raw materials to react under the action of catalyst, and purifying the product to obtain poly(3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro-3,9-dioxa[5.5]undecane)-2,6-diaminopyridine. The method of the invention is simple and is easy to control; the synthetized macromolecular intumescent flame retardant with phosphorus and nitrogen has better compatibility with the matrix and higher char forming characteristic; by adopting the method, the problem of migration, precipitationor volatilization in the machinings of the flame retardant and the polymer matrix can be solved basically; and the flame retardant does not contain halogen, thus the flame retardant is environmentally friendly and has good application prospect.

Description

technical field [0001] The invention relates to an intumescent non-halogen flame retardant, in particular to a phosphorus- and nitrogen-containing macromolecule intumescent flame retardant and a synthesis method thereof. Background technique [0002] With the development of my country's synthetic material industry and the continuous expansion of its application fields, flame retardants are increasingly showing a broad market in various fields such as chemical building materials, electronic appliances, transportation, aerospace, daily furniture, interior decoration, basic necessities of life, etc. Prospects, flame retardants have developed into the second largest polymer material modification additive after plasticizers in my country. Halogenated flame retardants have been the most widely used type of flame retardants for a long time because of their incomparable high-efficiency flame retardant performance and price advantages, but they have harmful effects on the environment ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04
Inventor 徐国永张海潮朱宝宁章于川田友峰
Owner ANHUI ZHONGDING SEALING PARTS
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