Phosphonitrile grafting-modified hydrotalcite flame retardant and preparation method thereof

A technology of graft modification and hydrotalcite, which is applied in chemical instruments and methods, fibrous fillers, dyed low-molecular organic compound treatment, etc., can solve the problems that the preparation method has not been reported, achieve good application value, and improve flame retardancy Performance and mechanical properties, the effect of easy control of reaction conditions

Inactive Publication Date: 2019-10-08
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation method of composite flame retardant materials based on phosphazene and hydrotalcite has not been reported yet.

Method used

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  • Phosphonitrile grafting-modified hydrotalcite flame retardant and preparation method thereof
  • Phosphonitrile grafting-modified hydrotalcite flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh Mg(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 O and urea (according to the Mg:Al molar ratio of 2:1, the amount of urea is 3.3 times the total mass of Mg and Al), dissolved in 400mL of deionized water, reacted in the reactor at 110°C for 24h, filtered and washed, Dry overnight at 80°C to obtain Mg / Al hydrotalcite (LDH).

[0036] Put 6g of Mg / Al hydrotalcite into 300mL of ethanol and water mixture (1:3 volume ratio), and ultrasonically disperse at 50°C for 30min, weigh 0.6g of 3-aminopropyltriethoxysilane in 150mL of ethanol In the mixed solution with water (volume ratio: 9:1), slowly add the silane coupling agent solution to the hydrotalcite suspension under nitrogen gas, add acetic acid to adjust the pH to 4, and stir at 90°C for 24 hours. Filter, wash, and dry to obtain Mg / Al hydrotalcite (LDH-KH550) with amino groups on the surface.

[0037] Using tetrahydrofuran as a solvent, prepare 15g / L Mg / Al hydrotalcite suspension containing amine groups on the surface, we...

Embodiment 2

[0039] Weigh the Zn(NO 3 ) 2 ·6H 2 O, Fe(NO 3 ) 3 9H 2O and urea (according to the Zn:Fe molar ratio of 3:1, the urea amount is 3.3 times the total mass of Zn and Fe), dissolved in 400mL deionized water, reacted at 110°C in the reactor for 24h, filtered and washed, Dry overnight at 80°C to obtain Zn / Fe hydrotalcite.

[0040] Put 6g of Zn / Fe hydrotalcite into 300mL of ethanol and water mixture (1:3 volume ratio), and ultrasonically disperse at 40°C for 50min, weigh 1.5g of 3-aminopropyltriethoxysilane in 150mL of ethanol In the mixed solution with water (volume ratio: 9:1), slowly add the silane coupling agent solution to the hydrotalcite suspension under nitrogen gas, add acetic acid to adjust the pH to 4, and stir at 90°C for 24 hours. filtering, washing and drying to obtain the Zn / Fe hydrotalcite containing amino groups on the surface.

[0041] Using tetrahydrofuran as a solvent, prepare 15g / L of Zn / Fe hydrotalcite suspension containing amine groups on the surface, we...

Embodiment 3

[0043] Weigh Ni(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 O and urea (according to the Ni:Al molar ratio of 4:1, the amount of urea is 3.3 times the total mass of Ni and Al), dissolved in 400mL of deionized water, reacted at 110°C for 24h in the reactor, filtered and washed, Dry overnight at 80°C to obtain Ni / Al hydrotalcite.

[0044] Put 6g of Ni / Al hydrotalcite into 300mL of ethanol and water mixture (1:3 volume ratio), and ultrasonically disperse at 45°C for 40min, weigh 1.8g of 3-aminopropyltriethoxysilane in 150mL of ethanol In the mixed solution with water (volume ratio: 9:1), slowly add the silane coupling agent solution to the hydrotalcite suspension under nitrogen gas, add acetic acid to adjust the pH to 4, and stir at 90°C for 24 hours. Filtrate, wash, and dry to obtain Ni / Al hydrotalcite with amino groups on the surface.

[0045] Using tetrahydrofuran as a solvent, prepare 15g / L Ni / Al hydrotalcite suspension containing amine groups on the surface, weigh 2.5g hexachl...

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Abstract

The invention discloses a phosphonitrile grafting-modified hydrotalcite flame retardant and a preparation method thereof and belongs to the field of high-molecular flame retardance and interface chemistry. The preparation method comprises subjecting an amino-containing silane coupling agent to condensation with surface hydroxyl groups of hydrotalcite so that the silane coupling agent is grafted tothe surface of the hydrotalcite so as to introduce amino groups; allowing the amino groups to react with a phosphonitrile flame retardant, and grafting the phosphonitrile flame retardant to the surface of the hydrotalcite through chemical bonds. The invention is intended to graft a flame retardant, having rich flame-retarding elements, such as phosphorus and nitrogen, to the surface of hydrotalcite through chemical bonds so as to obtain novel hydrotalcite with surface modified by grafting the flame retardant; the modified hydrotalcite may be blended with various resin matrixes, so that flameretardance of the hydrotalcite is improved comprehensively, and dispersibility and compatibility of the hydrotalcite in the resin matrixes can be improved. The phosphonitrile grafting-modified hydrotalcite flame retardant prepared herein has good flame retardance, and is well compatible with resin matrixes; the preparation method is simple, has low cost and has a good actual application prospect.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a phosphazene graft modified hydrotalcite-like flame retardant and a preparation method thereof, and belongs to the field of polymer flame retardancy and hydrotalcite surface graft modification. Background technique [0002] With the increasing awareness of global safety and environmental protection, people have higher and higher requirements for fire safety and flame retardancy of products. Halogen-free, low-smoke, low-toxicity and high-efficiency environmentally friendly flame retardants have become the goal pursued by people. As a new anionic layered inorganic functional material, hydrotalcites (LDHs) have very good application prospects in catalysts, adsorbents, heat stabilizers, dyes, etc., and they are non-toxic and smoke-free, and have considerable flame retardancy In recent years, it has been widely used as a multifunctional plastic additive, and is of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K13/06C08K9/04C08K9/06C08K3/26C09C1/40C09C3/08C09C3/12
CPCC08K3/26C08K9/04C08K9/06C08K13/06C09C1/40C09C3/006C09C3/08C09C3/12
Inventor 徐圣张敏曾虹燕潘勇李思雨陈超荣吴昆田贤曜
Owner XIANGTAN UNIV
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