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High-efficiency polyphosphate ester fire retardant and preparation method thereof

A technology of polyphosphate ester and flame retardant, which is applied in the field of polyphosphate ester and its preparation, can solve the problems of material mechanical properties and processing performance damage, low decomposition temperature, and low flame retardant efficiency, and achieve easy processing and recycling, and easy preparation The method is simple and the effect of high decomposition temperature

Inactive Publication Date: 2016-08-10
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the halogen-based flame retardant system has a good flame retardant effect, it releases toxic and corrosive gases during combustion, which poses great hidden dangers to humans and the environment, and its use has been gradually restricted or banned
Compared with halogen-based flame retardants, inorganic flame retardants, phosphorus-based and phosphorus-nitrogen-based flame retardants are currently recognized as environmentally friendly "green" flame retardants by the scientific and industrial circles, but such flame retardants are often A higher amount of addition (inorganic type is usually not less than 40wt%, and phosphorus-containing type is not less than 30wt%) can make the material achieve the expected flame retardant effect, and the flame retardant efficiency is low; and the above-mentioned such a large amount of addition leads to The mechanical properties and processing properties of the material are greatly damaged. At the same time, the poor thermal stability and low decomposition temperature cause difficulties in the processing and recycling of flame-retardant polymers.

Method used

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  • High-efficiency polyphosphate ester fire retardant and preparation method thereof
  • High-efficiency polyphosphate ester fire retardant and preparation method thereof
  • High-efficiency polyphosphate ester fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 28.6 g of bisphenolic acid (DPA; 4,4-bis(4-hydroxyphenyl)pentanoic acid, CAS No. 126-00-1) and 1-oxyphospha-4-hydroxymethyl into a 250 mL three-necked flask -18.0g of 2,6,7-trioxabicyclo[2.2.2]octane (PEPA), 1.92g of p-toluenesulfonic acid, 100ml of anhydrous acetonitrile, nitrogen protection, reflux reaction under mechanical stirring for 20 hours. During this period, part of the azeotrope of acetonitrile and water was evaporated three times, and then a corresponding volume of acetonitrile was added to obtain a purple transparent solution. The solvent was removed by rotary evaporation (rotary evaporation) to give the crude product.

[0032] The crude product was added into deionized water at 70°C for purification. Use thin-layer chromatography to track until there is no bisphenolic acid in the upper layer of water, then filter the product while it is hot, and dry it in vacuum at 80° C. for 10 hours. Monomer (II) is obtained. (That 1 H NMR and 13 C NMR spectrum ...

Embodiment 2

[0038] Add 28.6g of bisphenolic acid, 21.6g of 1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane (PEPA) and 1.92 g of phenylbenzenesulfonic acid, 100 ml of anhydrous acetonitrile, protected by nitrogen gas, and reflux reaction for 18 hours under mechanical stirring. During this period, part of the azeotrope of acetonitrile and water was evaporated three times, and then a corresponding volume of acetonitrile was added to obtain a purple transparent solution. The solvent was removed by rotary evaporation to obtain a crude product.

[0039] The crude product was added into deionized water at 80°C for purification. TLC was used to track until there was no bisphenolic acid in the upper layer of water, and then the product was filtered and vacuum-dried at 80° C. for 10 hours. Monomer (II) is obtained.

[0040] Synthesis of polyphosphate (IV): Add 22.4 g of monomer (II) and 120 mL of acetonitrile into a 250 ml three-necked flask, and flush with nitrogen gas for 10 minu...

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Abstract

The invention provides a high-efficiency polyphosphate ester fire retardant. The fire retardant is characterized by having a structure general formula (I) defined in the description, wherein n is 2-20, and R group is phenyl group or phenoxy group. The prepared phosphate ester has high phosphorus content by means of molecular structure design, and the additive amount of the phosphate ester is less than 10 wt% to reach a quite good flame retardant efficiency, which is much less than the additive amount of the traditional phosphorus based flame retardant. The phosphate ester is a high-efficiency green and environmentally-friendly fire retardant. The high-efficiency phosphate ester fire retardant overcomes the disadvantages of the traditional fire retardant such as deliquescence and migration, and has advantages such as strong water resistence, and good compatibility with the matrix, and is halogen-free and difficult to migrate.

Description

technical field [0001] The invention relates to a polyphosphate and a preparation method thereof. This kind of polyphosphate can be used as a high-efficiency (the addition amount is less than 10wt% can achieve a better flame-retardant effect, and the UL94 level can reach V0) flame-retardant in the field of flame-retardant. Background technique [0002] At present, the basic research and application development of flame retardant materials at home and abroad are very active. Although the halogen-based flame retardant system has a good flame retardant effect, it releases toxic and corrosive gases during combustion, which poses great hidden dangers to humans and the environment, and its use has been gradually restricted or banned. Compared with halogen-based flame retardants, inorganic flame retardants, phosphorus-based and phosphorus-nitrogen-based flame retardants are currently recognized as environmentally friendly "green" flame retardants by the scientific and industrial c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/12C09K21/14C07F9/6571C08G79/04
CPCC09K21/12C07F9/6571C08G79/04C09K21/14
Inventor 井健张艳方征平
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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