Preparation method of P-type molecular sieve-red phosphorus synergistic flame retardant

A technology of synergistic flame retardant and molecular sieve, 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: 2017-01-11
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] 20g of P-type molecular sieve with a median particle size of 200nm 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 100min, phosphine was passed at 440°C, reacted for 10h, and 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 a P-type molecular sieve with a red phosphorus content of 33%. The flame retardant was mixed with polyethylene to prepare a flame retardant material. The oxygen index is 32.8.

Embodiment 2

[0024] Mix 20g of P-type molecular sieve with a median particle size of 600nm 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 passed through at 400°C for 10min, phosphine was passed through at 410°C, reacted for 2h, and after cooling, the The sample is 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 P-type molecular sieve with a red phosphorus content of 5%. The flame retardant is prepared by mixing the flame retardant with polyethylene. The oxygen index is 27.5.

Embodiment 3

[0026] Mix 20g of P-type molecular sieve with a median particle size of 400nm and 500mL of 0.1mol / L NiCl 2 The 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 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 P-type molecular sieve with a red phosphorus content of 17%. The flame retardant is prepared by mixing the flame retardant with polyethylene. The oxygen index is 30.8.

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Abstract

The invention relates to a preparation method of a P-type molecular sieve-red phosphorus synergistic flame retardant. The preparation method includes: mixing a P-type molecular sieve with a certain amount of NiCl2 solution of 0.1mol / L; performing ion exchange at 60 DEG C for 30-120min; filtering, washing, and drying; putting in a quartz tube reactor, and feeding hydrogen at 400-450 DEG C for 10-100min; feeding hydrogen phosphide at 410-440 DEG C for 2-10h; heating a sample in a reaction container isolated from air at 260-290 DEG C, and holding the temperature for 10-60min to obtain the P-type molecular sieve-red phosphorus synergistic flame retardant with red phosphorus of 5-33% (mass ratio) loaded in pores. The preparation method is simple, the defect when a red phosphorus flame retardant is used solely is overcome, and the P-type molecular sieve-red phosphorus synergistic 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 P-type 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 synergisti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/12C08K3/02C08L23/06
CPCC08K3/02C08K9/12C08K2003/026C08L2201/02C08L2201/08C08L23/06
Inventor 杜庆洋王清涛于华芹徐会君
Owner SHANDONG UNIV OF TECH
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