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Metal complex flame retardant and preparation method thereof

A technology of metal complexes and flame retardants, which is applied in the field of metal complexes and flame retardants and its preparation, can solve problems such as rare research on complexes, achieve high yield, high thermal stability, and simple post-processing Effect

Inactive Publication Date: 2017-11-14
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cyclotriphosphazene is a class of compounds whose basic skeleton is alternately arranged with P and N elements. Its unique phosphorus-nitrogen hybrid six-membered ring conjugated structure makes it have good thermal stability and flame retardancy. Cyclic triphosphazene derivatives with the capacity to design and synthesize metal-coordinating cyclotriphosphazene compounds will become a class of catalytic expansion flame retardants with great application prospects. At present, there are not many studies on this kind of complexes. See

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  • Metal complex flame retardant and preparation method thereof
  • Metal complex flame retardant and preparation method thereof
  • Metal complex flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Fully dissolve 0.1mol HCCP in 60ml tetrahydrofuran, add 0.4mol sodium carbonate and stir evenly, fill with N 2 30min; then dropwise add 50ml of tetrahydrofuran solution containing 0.72mol 4-aminopyridine therein, heat up to reflux, react for 10h, cool the solution to room temperature, filter, wash three times with tetrahydrofuran, and vacuum-dry at 80°C for 24h to obtain the ligand six ( 4-aminopyridine) cyclotriphosphazene (SFACP), yield 95%. in N 2 Under protection, add 0.1mol SFACP, 0.55mol zinc acetate, and 300ml ethanol into a 500ml three-neck flask, stir thoroughly, and after completely dissolving, heat up to reflux. After reacting for 18 hours, slowly cool the solution to room temperature, filter, and wash with ethanol Wash twice, wash once with distilled water, and vacuum dry at 80° C. for 24 hours to obtain the target product metal complex flame retardant Zn-SFACP with a yield of 87%. (The infrared spectrograms of SFACP and Zn-SFACP are shown in figure 1 , t...

Embodiment 2

[0027] Fully dissolve 0.1mol HCCP in 60ml tetrahydrofuran, add 0.9mol sodium hydroxide and stir evenly, fill with N 2 30min; then dropwise add 60ml of tetrahydrofuran solution containing 0.74mol 4-aminopyridine, heat up to reflux, react for 17h, cool the solution to room temperature, filter, wash three times with tetrahydrofuran, and vacuum dry at 80°C for 24h to obtain the ligand six ( 4-aminopyridine) cyclotriphosphazene (SFACP), yield 97%. in N 2 Under protection, add 0.1mol SFACP, 0.45mol palladium acetate, and 300ml ethanol into a 500ml three-neck flask, stir thoroughly, and after completely dissolving, heat up to reflux. After 24 hours of reaction, slowly cool the solution to room temperature, filter, and wash with ethanol Wash twice, wash once with distilled water, and vacuum dry at 80° C. for 24 hours to obtain the target product metal complex flame retardant Pd-SFACP with a yield of 80%.

Embodiment 3

[0029] in N 2 Under protection, add 0.2mol HCCP, 1.3mol 4-aminopyridine, 0.7mol triethylamine, and 160ml tetrahydrofuran into the reaction vessel, raise the temperature to reflux for 12 hours, cool and filter, wash the filter cake twice with tetrahydrofuran and once with dichloromethane , 80 ° C vacuum drying for 24 hours to obtain the ligand six (4-aminopyridine) cyclotriphosphazene (SFACP), the yield of 96%. in N 2 Under protection, add 0.1mol SFACP, 0.2mol cobalt acetate, 0.2mol nickel acetate, and 300ml ethanol into a 500ml three-neck flask, fully stir and dissolve, heat up to reflux and continue the reaction for 24h, slowly cool the solution to room temperature, filter, and wash with ethanol Wash twice, wash once with distilled water, and vacuum dry at 80° C. for 24 hours to obtain the target product metal complex flame retardant with a yield of 86%.

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Abstract

The invention discloses a metal complex flame retardant and a preparation method thereof. The metal complex flame retardant is prepared by the steps of adopting hexachlorotriphosphazene and 4-aminopyridine, and synthesizing a cyclotriphosphazene-based organic metal ligand; and then carrying out coordination reaction on the ligand and metal acetate to obtain the metal complex flame retardant with high thermal stability and high char yield. A synthesis process is easy to operate, simple in aftertreatment of a product and suitable for industrial production; and the metal complex flame retardant combines the flame retardant advantages of metal catalysis and phosphazene flame retardants, can effectively lower the addition amount of the flame retardant and is an efficient halogen-free and environmental-friendly flame retardant.

Description

technical field [0001] The invention relates to a metal complex flame retardant and a preparation method thereof, belonging to the technical field of material science flame retardant synthesis. Background technique [0002] Polymer materials are widely used in various departments of production, scientific research, national defense and people's daily life. However, ordinary polymer materials are highly flammable, which undoubtedly leaves a great safety hazard to people's lives and properties. Therefore, improving the thermal stability of materials and enhancing the flame resistance of materials has become a hot spot in the research of material modification. As an additive that can effectively prevent materials from being ignited and inhibit flame propagation, flame retardants are widely used to improve the fire resistance of materials, and have become important additives for synthetic polymer materials. Halogenated flame retardants are currently one of the largest organic f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C07F3/06C07F15/00C07F15/04C08L87/00C08K5/5399
CPCC08G83/008C07F3/003C07F15/0066C07F15/045C08K5/5399C08L87/00C08L2201/02
Inventor 许博吴笑许准胡晶钱立军司朝阳马雯朱向东
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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