Compounds containing phosphorus, nitrogen and transition metal elements, and preparation method thereof

A technology of transition metal elements and compounds, which is applied in the field of compounds containing phosphorus, nitrogen and transition metal elements and their preparation, can solve the problems of reduced catalytic flame retardant efficiency, failure to achieve flame retardant effect, poor uniform dispersion, etc., to reduce Peak heat release, prevent thermal degradation, and high flame retardant efficiency

Inactive Publication Date: 2013-11-06
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Transition metal oxides are inorganic compounds, so their uniform dispersion in organic polymer materials is poor, and their applications are limited
Organic multidentate ligands enrich the types of transition metal chelates, but due to their poor thermal stability, they are easily decomposed during the processing of polymer materials, which reduces the efficiency of catalytic flame retardancy. burning effect

Method used

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  • Compounds containing phosphorus, nitrogen and transition metal elements, and preparation method thereof
  • Compounds containing phosphorus, nitrogen and transition metal elements, and preparation method thereof
  • Compounds containing phosphorus, nitrogen and transition metal elements, and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0070] Add 400ml of absolute ethanol solution containing 0.2mol salicylaldehyde into a 1L flask with condensing reflux and mechanical stirring, raise the temperature to 70°C within half an hour, then dissolve 0.1mol o-phenylenediamine in 200ml of absolute ethanol Slowly add it dropwise into the flask, finish the drop within 1 hour, continue to react for 0.5 hour, finally evaporate about 300ml of ethanol under reduced pressure, let the remaining mixture stand overnight, filter and wash with ethanol for 3 times, and then dry to obtain o-phenyl Diamine salicylaldehyde Schiff base 30.52g (about 0.096mol).

[0071] 0.1mol diethyl phosphite and 0.02mol o-phenylenediamine salicylaldehyde Schiff base are dispersed in 300ml absolute ethanol, and the mixture is placed in a 500ml three-neck flask with condensing reflux and mechanical stirring device for nitrogen gas flow, Heat to 65°C within half an hour. After reacting for 0.5 hours, add a small amount of sodium ethylate dropwise as a c...

Embodiment 2

[0085] Add 400ml of absolute ethanol solution containing 0.2mol salicylaldehyde into a 1L flask with condensing reflux and mechanical stirring, raise the temperature to 75°C within half an hour, then dissolve 0.1mol o-phenylenediamine in 200ml of absolute ethanol Slowly add it dropwise into the flask, finish dropping within 2 hours, continue to react for 0.5 hour, finally distill off about 300ml of ethanol under reduced pressure, leave the rest of the mixture overnight, filter and wash with ethanol for 3 times, then dry to obtain o-phenyl 31.43 g (about 0.097 mol) of diamine salicylaldehyde Schiff base.

[0086] 0.1mol diethyl phosphite and 0.04mol o-phenylenediamine salicylaldehyde Schiff base are dispersed in 300ml absolute ethanol, and the mixture is placed in a 500ml three-neck flask with condensing reflux and mechanical stirring device for nitrogen gas flow, Heat to 80°C within half an hour. After 1 hour of reaction, add a small amount of sodium ethoxide dropwise as a cat...

Embodiment 3

[0091] Add 400ml of absolute ethanol solution containing 0.2mol salicylaldehyde into a 1L flask with condensing reflux and mechanical stirring, raise the temperature to 80°C within half an hour, then dissolve 0.1mol of o-phenylenediamine in 200ml of absolute ethanol Slowly add it dropwise into the flask, finish dropping within 2 hours, continue to react for 4 hours, finally distill off about 300ml of ethanol under reduced pressure, leave the remaining mixture standing overnight, filter and wash with ethanol for 3 times, and then dry to obtain o-phenyl Diamine salicylaldehyde Schiff base 29.24g (about 0.94mol).

[0092] 0.1mol diethyl phosphite and 0.05mol o-phenylenediamine salicylaldehyde Schiff base are dispersed in 300ml absolute ethanol, and the mixture is placed in a 500ml three-neck flask with condensing reflux and mechanical stirring device for nitrogen gas flow, Heat to 90°C within half an hour, after 2.5 hours of reaction, add a small amount of sodium ethylate dropwis...

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Abstract

The invention discloses compounds containing phosphorus, nitrogen and transition metal elements. The compounds with the structure also contain transition metal with a catalytic flame-retardant effect besides phosphorus and nitrogen elements required in the traditional flame retardant. A method for preparing the compounds with the structure is simple; and the obtained product has higher yield, does not contain halogen, is environment-friendly, has high thermal decomposition temperature, and can be used for flame-retardant engineering plastic. A general structural formula of the compounds is shown in the following formula (I).

Description

technical field [0001] The invention relates to a design and preparation method of a novel ligand containing phosphorus and nitrogen elements and a chelated transition metal ion compound, in particular to a compound containing phosphorus, nitrogen and transition metal elements and a preparation method thereof. Background technique [0002] The currently used polymer material flame retardants are divided into physical flame retardant and chemical flame retardant according to their mechanism. The physical approach is to interfere with polymer combustion by cooling, diluting, and forming a thermal insulation layer; while the chemical approach is to change the degradation mode of the polymer by terminating the free radical chain reaction to achieve flame retardancy. [0003] In already commercialized flame retardants, such as Al(OH) 3 , Mg(OH) 2 etc. are flame retardants that belong to the physical route. They have the advantages of less smoke generation and no toxic gas, but ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40C07F9/6574C08K5/5353C08K5/5357
Inventor 方征平曹贞虎张艳
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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