A kind of preparation method of modified phosphorus nitrogen type flame retardant

A flame retardant and modification technology, which is applied in the field of preparation of modified phosphorus-nitrogen flame retardants, can solve the problem of unsatisfactory improvement of polycarbonate flame retardancy, achieve a significant increase in LOI, and improve flame retardancy Effect

Active Publication Date: 2019-01-04
HUAIAN SHUANGYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The improvement of the flame retardancy of polycarbonate by the phosphorus-nitrogen flame retardant in the prior art is still not ideal, and it is necessary to develop a new flame retardant production process for improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Synthesis reaction:

[0020] In a 1000L reactor, add 100Kg phosphoric acid, 50Kg ethylene glycol, 110Kg melamine, 3Kg methyl isobutyl carbinol; esterify at 120°C for 3 hours, and react at 110°C for 1 hour, then cool and wash , to get intermediate products.

[0021] (2) Modification treatment

[0022] In the 5000L reactor, add 100Kg intermediate product, 15Kg vinyl acetate, 0.5Kg dimethylsilyl (cyclopentadiene) (9-fluorenyl) zirconium dichloride, 0.5Kg dicyclopentadiene, 2000Kg toluene, 3Kg hydroxymethylcellulose, 1Kg azobisisoheptanonitrile, react at 85°C for 8h to obtain the product. Product number M-1.

Embodiment 2

[0024] (1) Synthesis reaction:

[0025] In a 1000L reactor, add 100Kg of phosphoric acid, 30Kg of ethylene glycol, 70Kg of melamine, and 1Kg of methyl isobutyl carbinol; at 100°C for 1 hour of esterification, at 100°C for 0.5 hour of salt formation, and then cool. Washing yields an intermediate product.

[0026] (2) Modification treatment

[0027] In the 5000L reactor, add 100Kg intermediate product, 5Kg vinyl acetate, 0.1Kg dimethylsilyl (cyclopentadiene) (9-fluorenyl) zirconium dichloride, 0.1Kg dicyclopentadiene, 1000Kg toluene, 1Kg hydroxymethylcellulose, 0.5Kg azobisisoheptanonitrile, react at 80°C for 5h to obtain the product. Product number M-2.

Embodiment 3

[0029] (1) Synthesis reaction:

[0030] In a 1000L reactor, add 100Kg phosphoric acid, 70Kg ethylene glycol, 110Kg melamine, 5Kg methyl isobutyl carbinol; esterify at 130°C for 4 hours, and react at 120°C for 2 hours, then cool and wash get intermediate products.

[0031] (2) Modification treatment

[0032] In a 5000L reactor, add 100Kg intermediate product, 20Kg vinyl acetate, 1Kg dimethylsilyl (cyclopentadiene) (9-fluorenyl) zirconium dichloride, 1Kg dicyclopentadiene, 3000Kg toluene, 4Kg hydroxyl Methyl cellulose and 2Kg azobisisoheptanonitrile were reacted at 95°C for 12 hours to obtain the product. Product number M-3.

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PUM

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Abstract

The invention provides a method for preparing a modified phosphorus-nitrogen flame-retardant agent. In a reaction kettle, phosphoric acid, ethylene glycol, melamine and methyl isobutyl carbinol are added by weight, an esterification reaction and a salt forming reaction are conducted to obtain an intermediate product, and then a modification reaction is conducted to obtain the product.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant, in particular to a method for preparing a modified phosphorus-nitrogen type flame retardant. Background technique [0002] Flame retardant, a functional additive that imparts flame retardancy to flammable polymers, is mainly designed for the flame retardant of polymer materials; there are many types of flame retardants, which are divided into additive flame retardants and reaction type flame retardant. Additive flame retardants are added to polymers by mechanical mixing to make polymers flame retardant. At present, additive flame retardants mainly include organic flame retardants and inorganic flame retardants. Halogenated flame retardants (organic flame retardants) chlorides and organic bromides) and non-halogenated. Organic is some flame retardants represented by bromine, phosphorus nitrogen, nitrogen and red phosphorus and compounds, and inorganic is mainly antimony trioxide, magne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L31/04C08L1/28C08L69/00C08K5/3492C08K5/54C08F218/08C08F232/08
CPCC08F218/08C08L31/04C08L69/00C08L2201/02C08L2205/03C08L1/284C08K5/34928C08K5/5406C08F232/08
Inventor 王荣军吴健泳
Owner HUAIAN SHUANGYANG CHEM
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