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Preparation method of superfine zsm-5 molecular sieve-red phosphorus synergistic flame retardant

A ZSM-5, synergistic flame retardant technology, applied in the field of flame retardants, can solve the problems of easy explosion, complex preparation process, restricted use, etc. Effect

Active Publication Date: 2018-07-17
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] 15g of ZSM-5 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 120min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was introduced at 450°C for 90min, phosphine was introduced at 440°C, and reacted for 10h. After cooling, the The sample was heated to 290°C in an air-isolated reaction vessel and held for 60 minutes to obtain a flame retardant loaded with red phosphorus in the pores of ZSM-5 molecular sieve with a red phosphorus content of 37%. The flame retardant prepared by mixing the flame retardant with polyethylene The oxygen index of the material was 33.6.

Embodiment 2

[0024] 15g of ZSM-5 molecular sieve with a median particle size of 500nm 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 20min, 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 the pores of ZSM-5 molecular sieve with a red phosphorus content of 5%. The flame retardant prepared by mixing the flame retardant with polyethylene The oxygen index of the material was 28.7.

Embodiment 3

[0026] 15g of ZSM-5 molecular sieve with a median particle size of 300nm and 500mL of 0.1mol / L NiCl 2The solutions were mixed, stirred at 60°C for 75min, filtered, washed and dried, placed in a quartz tube reactor, hydrogen gas was introduced at 425°C for 55min, 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 pores of ZSM-5 molecular sieve with a red phosphorus content of 16%. The flame retardant prepared by mixing the flame retardant with polyethylene The oxygen index of the material was 31.3.

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Abstract

The invention relates to a preparation method of an ultrafine ZSM-5 molecular sieve-red phosphorus synergistic flame retardant. In the method, ZSM-5 molecular sieve is mixed with a certain amount of 0.1mol / L NiCl2 solution, and ion exchange is performed at 60°C for 30- After 120 minutes, filter, wash, and dry, then place in a quartz tube reactor, pass hydrogen at 400-450°C for 20-90 minutes, then pass through phosphine at 410-440°C for 2-10 hours, and finally put the sample Heating and heat preservation at 260-290° C. for 10-60 minutes in an air-insulated reaction vessel to obtain a ZSM-5 molecular sieve-red phosphorus synergistic flame retardant loaded with 5-37% (mass ratio) red phosphorus in the channels. 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 an ultrafine ZSM-5 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/12C08K3/02C08K7/26C08L23/06
CPCC08K3/02C08K7/26C08K9/12C08K2003/026C08K2201/003C08K2201/011C08L2201/02C08L2201/08C08L23/06
Inventor 徐会君李伟志于华芹杜庆洋
Owner SHANDONG UNIV OF TECH