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Halogen-free phosphorus-nitrogen additive-type flame retardant and preparation method thereof

A halogen-free phosphorus-nitrogen, additive-type technology, applied in the field of halogen-free flame retardants, can solve the problems of poor thermal stability, difficult processing, easy exudation, etc., and achieves the effects of high synthesis efficiency, low yield and difficult hydrolysis.

Inactive Publication Date: 2020-02-21
珠海格力绿色再生资源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although organophosphorus flame retardants have the advantages of good compatibility, flame retardancy, plasticization, and phosphorus-nitrogen synergy, they also have problems such as low efficiency, poor thermal stability, easy hydrolysis, easy oozing, and difficult processing.

Method used

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  • Halogen-free phosphorus-nitrogen additive-type flame retardant and preparation method thereof
  • Halogen-free phosphorus-nitrogen additive-type flame retardant and preparation method thereof
  • Halogen-free phosphorus-nitrogen additive-type flame retardant and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] This embodiment provides a preparation method of a halogen-free phosphorus-nitrogen additive flame retardant, the steps comprising:

[0032] (1) Preparation of intermediate piperazine diphosphate

[0033] A nitrogen-passing device, a mechanical stirrer, a spherical condenser, a thermometer and a constant-pressure dropping funnel were installed on a 500 mL five-necked round-bottomed flask (all glass instruments were thoroughly washed and dried with deionized water before use). Under the condition of nitrogen, pour 115.3 g of phosphoric acid solution with a concentration of 98% into the reaction device, and then put 43.1 g of anhydrous piperazine into a 250 mL beaker, stir with an appropriate amount of deionized water until completely dissolved, pour into constant In the dropping funnel, slowly dropwise into the phosphoric acid solution in the reaction vessel. After the dropwise addition of the anhydrous piperazine solution, the reaction temperature of the system was rais...

Embodiment 2

[0039] This embodiment provides a preparation method of a halogen-free phosphorus-nitrogen additive flame retardant, the steps comprising:

[0040] (1) Preparation of intermediate piperazine diphosphate

[0041] A nitrogen-passing device, a mechanical stirrer, a spherical condenser, a thermometer and a constant-pressure dropping funnel were installed on a 500 mL five-necked round-bottomed flask (all glass instruments were thoroughly washed and dried with deionized water before use). Under the condition of nitrogen, pour 98 g of phosphoric acid solution with a concentration of 85% into the reaction device, and then put 34.4 g of anhydrous piperazine into a 250 mL beaker, stir with an appropriate amount of deionized water until it is completely dissolved, pour it into a constant pressure In the dropping funnel, slowly added dropwise to the phosphoric acid solution in the reaction vessel. After the dropwise addition of the anhydrous piperazine solution, the reaction temperature o...

Embodiment 3

[0045] This embodiment provides a preparation method of a halogen-free phosphorus-nitrogen additive flame retardant, the steps comprising:

[0046] (1) Preparation of intermediate piperazine diphosphate

[0047] A nitrogen-passing device, a mechanical stirrer, a spherical condenser, a thermometer and a constant-pressure dropping funnel were installed on a 500 mL five-necked round-bottomed flask (all glass instruments were thoroughly washed and dried with deionized water before use). Under the condition of nitrogen, 98g phosphoric acid solution with a concentration of 98% was poured into the reaction device, and then 43.5g anhydrous piperazine was put into a 250mL beaker, stirred with an appropriate amount of deionized water until completely dissolved, poured into a constant pressure In the dropping funnel, slowly added dropwise to the phosphoric acid solution in the reaction vessel. After the dropwise addition of the anhydrous piperazine solution, the reaction temperature of t...

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Abstract

The invention relates to a halogen-free phosphorus-nitrogen additive-type flame retardant and a preparation method thereof. The preparation method comprises the following steps: dissolving anhydrous piperazine with deionized water; adding a phosphoric acid solution, reacting under inert conditions to obtain intermediate piperazine diphosphate, and carrying out dehydration polycondensation reactionon the intermediate piperazine diphosphate to obtain polypiperazine phosphate which is the halogen-free phosphorus-nitrogen additive-type flame retardant. The halogen-free phosphorus-nitrogen additive-type flame retardant is not easily hydrolyzed, has favorable charring performance and heat stability; reaction conditions are mild, operation is safer, synthesis efficiency is higher. According to the preparation method of the halogen-free phosphorus-nitrogen additive-type flame retardant, a phosphoric acid structure and a piperazine structure are introduced into a same flame retardant moleculestructure, so that better intermolecular synergistic effect is achieved; it is shown by thermogravimetric analysis results that at 800 DEG C, the polypiperazine phosphate carbon yield is 16.4wt%, thepiperazine diphosphate carbon yield is 14.1wt%, and the polypiperazine phosphate carbon yield is 16.3% higher than that of the piperazine diphosphate, it indicates that the flame retardant polypiperazine phosphate has good char forming performance and thermal stability.

Description

technical field [0001] The invention belongs to the technical field of halogen-free flame retardants, in particular to a halogen-free phosphorus-nitrogen additive type flame retardant and a preparation method thereof. Background technique [0002] With the vigorous development of polymer materials such as plastics, rubber, synthetic fibers and their products, they are rapidly replacing traditional steel, metal products, cement and natural polymers such as wood and fibers, and are widely used in industry, agriculture, military industry, construction and other industrial sectors. The large-scale use of polymer materials not only promotes technological progress and brings huge economic benefits to the society, but also has serious safety and environmental problems, among which fire is the most serious safety problem. With the increase in the application of polymer materials in various fields, the economic losses and casualties caused by fires caused by polymer materials are al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/32C08K5/3462C07D295/023C07D295/027
CPCC07D295/023C07D295/027C08K3/32C08K5/3462C08K2003/329
Inventor 夏思禹彭楚堂李勉陈龙王琳
Owner 珠海格力绿色再生资源有限公司
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