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Preparation method of nano-β molecular sieve-red phosphorus synergistic flame retardant

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

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 10g of β molecular sieve with a median particle size of 80nm and 500mL of 0.1mol / L NiCl 2 The solution was mixed, stirred at 60°C for 90min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was introduced at 450°C for 90min, phosphine was passed at 440°C, reacted for 10h, and after cooling, the The sample is 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 pores of a β molecular sieve with a red phosphorus content of 37%. The flame retardant is prepared by mixing the flame retardant with polyethylene. The oxygen index is 33.8.

Embodiment 2

[0024] Mix 10g of β molecular sieve with a median particle size of 100nm and 500mL of 0.1mol / L NiCl 2 The solutions were mixed, stirred at 60°C for 20min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was passed through at 400°C for 10min, phosphine was passed through 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 the pores of a β molecular sieve with a red phosphorus content of 7%. The flame retardant material prepared by mixing the flame retardant with polyethylene The oxygen index is 28.2.

Embodiment 3

[0026] Mix 10g of β molecular sieve with a median particle size of 90nm and 500mL of 0.1mol / L NiCl 2 The solutions were mixed, stirred at 60°C for 55min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was introduced at 425°C for 50min, phosphine was passed at 425°C, reacted for 6h, and after cooling, the The sample is 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 pores of a β molecular sieve with a red phosphorus content of 22%. The flame retardant is prepared by mixing the flame retardant with polyethylene. The oxygen index is 32.7.

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Abstract

The present invention relates to a preparation method of nano-β molecular sieve-red phosphorus synergistic flame retardant. In the method, β-molecular sieve is mixed with a certain amount of 0.1mol / L NiCl2 solution, ion-exchanged at 60°C for 20-90min, filtered, Wash and dry, then put in a quartz tube reactor, feed hydrogen at 400-450°C for 10-90min, then feed phosphine at 410-440°C for 2-10h, and finally put the sample in the air-isolated reaction The container is heated and kept at 260-290° C. for 10-60 minutes to obtain a β molecular sieve-red phosphorus synergistic flame retardant loaded with 7-37% (mass ratio) red phosphorus in the channel. The preparation process of the invention is relatively simple, which solves the shortcomings of using the red phosphorus flame retardant alone, 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 nano-beta 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 synergi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/12C08K3/02C08K7/26C08L23/06
CPCC08K3/02C08K7/26C08K9/12C08K2003/026C08L2201/02C08L2201/08C08L23/06
Inventor 徐会君王清涛李伟志杜庆洋
Owner SHANDONG UNIV OF TECH
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