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

A synergistic flame retardant and molecular sieve technology, applied in the field of flame retardants, can solve problems such as explosives, restricted use, and complicated preparation processes, and achieve the effects of improving mechanical properties and thermal stability, improving compatibility, and simple preparation processes

Active Publication Date: 2017-02-15
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 A-type 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 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 type A molecular sieve with a red phosphorus content of 35%. The flame retardant is mixed with polyethylene to prepare a flame retardant material The oxygen index is 33.1.

Embodiment 2

[0024] Mix 10g of A-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 10min, 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, 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 type A molecular sieve with a red phosphorus content of 5%. The flame retardant is mixed with polyethylene to prepare a flame retardant material The oxygen index is 27.9.

Embodiment 3

[0026] Mix 10g of A-type molecular sieve with a median particle size of 250nm and 500mL of 0.1mol / L NiCl 2 The solutions were mixed, stirred at 60°C for 65min, 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 type A molecular sieve with a red phosphorus content of 20%. The flame retardant is mixed with polyethylene to prepare a flame retardant material The oxygen index is 31.5.

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Abstract

The invention relates to a preparation method of a superfine A type molecular sieve-red phosphorus synergistic flame retardant; the method comprises the steps: mixing an A type molecular sieve with a certain amount of a 0.1 mol / L NiCl2 solution, carrying out ion exchange for 10-120 min at the temperature of 60 DEG C, filtering, washing, drying, then placing in a quartz tube reactor, introducing hydrogen gas for 10-90 min at the temperature of 400-450 DEG, then introducing hydrogen phosphide for 2-10 h at the temperature of 410-440 DEG C, and finally carrying out heating heat preservation of the sample for 10-60 min at the temperature of 260-290 DEG C in an air isolated reaction vessel, to obtain the A type molecular sieve-red phosphorus synergistic flame retardant loaded with 5-35 mass% of red phosphorus in pore passages. The preparation process is relatively simple, the deficiency of single use of a red phosphorus flame retardant is solved, and the prepared flame retardant has good flame retardant property.

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 A-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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/12C08K3/02C08K7/26C08L23/06
CPCC08K3/02C08K7/26C08K9/12C08K2003/026C08K2201/003C08L2201/02C08L2201/08C08L23/06
Inventor 杜庆洋王清涛刘正道徐会君
Owner SHANDONG UNIV OF TECH
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