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A kind of preparation method of cancryptite-red phosphorus synergistic flame retardant

A synergistic flame retardant and cancryptite technology, applied in the field of flame retardants, can solve the problems of restricted use, easy explosion, complicated preparation process, etc., and achieve improved compatibility, improved mechanical properties and thermal stability, and simple preparation process Effect

Active Publication Date: 2018-07-06
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when red phosphorus is used, there are the following problems: flammable, explosive, and long-term contact with air will release highly toxic pH 3 Gas; itself is red, easy to color the product; easy to absorb water, poor compatibility with polymers
Although the flame retardant effect of red phosphorus microcapsules is good, its preparation process is relatively complicated, and the particle size of the flame retardant is not easy to control, which limits its wide use.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Mix 20g of cancryptite with a median particle size of 0.5μm and 500mL of 0.1mol / L NiCl 2 The solutions were mixed, stirred at 60°C for 180min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was introduced at 450°C for 120min, phosphine was passed at 440°C, and reacted for 10h. After cooling, the The sample was heated to 290°C in an air-isolated reaction vessel and kept for 60 minutes to obtain a flame retardant loaded with red phosphorus in the channels of cancryptite with a red phosphorus content of 33%. The flame retardant material was prepared by mixing the flame retardant with polyethylene The oxygen index is 33.2.

Embodiment 2

[0024] Mix 20g of cancryptite with a median particle size of 1 μm and 500mL of 0.1mol / L NiCl 2 The solutions were mixed, stirred at 60°C for 30min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was introduced at 400°C for 30min, phosphine was passed at 410°C, reacted for 2h, and after cooling, the The sample was heated to 260°C in an air-isolated reaction vessel and kept for 10 minutes to obtain a flame retardant loaded with red phosphorus in cancryptite channels with a red phosphorus content of 4%. The flame retardant material was prepared by mixing the flame retardant with polyethylene The oxygen index is 28.1.

Embodiment 3

[0026] Mix 20g of cancryptite with a median particle size of 0.75μm and 500mL of 0.1mol / L NiCl 2 The solutions were mixed, stirred at 60°C for 105min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was introduced at 425°C for 75min, phosphine was passed at 425°C, reacted for 6h, and after cooling, the The sample was heated to 275°C in an air-isolated reaction vessel and kept for 35 minutes to obtain a flame retardant loaded with red phosphorus in the channels of cancryptite with a red phosphorus content of 17%. The flame retardant material was prepared by mixing the flame retardant with polyethylene The oxygen index is 31.4.

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PUM

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Abstract

The invention relates to a preparation method of a cannesite-red phosphorus synergistic flame retardant. The method comprises the steps of mixing cannonite and a certain amount of 0.1 mol / L NiCl2 solution, ion-exchanging at 60° C. for 30-180 min, and filtering , washed, dried, then placed in a quartz tube reactor, passed hydrogen at 400-450°C for 30-120min, then passed phosphine at 410-440°C for 2-10h, and finally put the sample in an air-isolated environment. The reaction vessel is heated and kept at 260-290° C. for 10-60 minutes to obtain a cannesite-red phosphorus synergistic flame retardant with 4-33% (mass ratio) of red phosphorus loaded in the pores. The preparation process of the invention is relatively simple, the deficiency of using the red phosphorus flame retardant alone is solved, and the prepared flame retardant has good flame retardant performance.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a preparation method of a cancryptite molecular sieve-red phosphorus synergistic flame retardant. Background technique [0002] With the enhancement of people's awareness of health and environmental protection, it has become an inevitable trend in the flame retardant industry to seek environmentally friendly, low-toxicity, high-efficiency, and multi-functional flame retardants. New flame retardant technologies such as ultra-fine technology, microencapsulation technology, compounding technology, and cross-linking technology are constantly developing. [0003] In modern flame retardant technology, the compounding of flame retardant is an extremely important aspect. Compounding is to use the interaction between flame retardants to improve the flame retardant performance, that is, the synergistic effect of flame retardants. The flame retardant system with syner...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/12C08K3/02C08L23/06
CPCC08K3/02C08K9/12C08K2003/026C08L2201/02C08L2201/08C08L23/06
Inventor 杜庆洋于华芹李伟志徐会君
Owner SHANDONG UNIV OF TECH
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