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Concerted catalysis flame-retardant metal complex containing P/N/Si/S/Ni and preparation method of complex

A metal complex and synergistic catalysis technology, applied in the field of intumescent metal flame retardants, can solve the problems of poor flame retardant efficiency of intumescent organic flame retardants, toxic fumes and large usage of halogen flame retardants , to achieve the effect of simple and easy control of the reaction process, improved flame retardant effect, mild and stable synthesis process conditions

Active Publication Date: 2017-03-29
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above technical background, the present invention provides an intermediate II in order to solve the problems of non-environmental protection properties such as smoke and toxicity of halogenated flame retardants and the poor flame retardant efficiency and large usage of intumescent organic flame retardants. Its preparation method, and the target product of this intermediate II - the metal complex containing P / N / Si / S / Ni synergistic catalytic flame retardancy and its preparation method

Method used

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  • Concerted catalysis flame-retardant metal complex containing P/N/Si/S/Ni and preparation method of complex
  • Concerted catalysis flame-retardant metal complex containing P/N/Si/S/Ni and preparation method of complex
  • Concerted catalysis flame-retardant metal complex containing P/N/Si/S/Ni and preparation method of complex

Examples

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Effect test

Embodiment 1

[0038] A preparation method of a metal complex containing P / N / Si / S / Ni synergistically catalyzed and flame-retardant is:

[0039] (1) In 30mL of dichloromethane, first add 2.3mL (10mmol) of 3-aminopropyltriethoxysilane, then slowly add 4.1mL (23mmol) of diphenylphosphorous chloride, then slowly add 3.1 mL (22 mmol) of triethylamine; after stirring overnight at room temperature, a light yellow suspension was obtained, which was filtered through a sand core to remove the triethylamine hydrochloride solid to obtain a light yellow liquid, which was rotary evaporated to remove dichloromethane to obtain Solid crude product; finally, it was washed with tetrahydrofuran, recrystallized from dichloromethane and dried in vacuo to obtain a pale white solid, namely intermediate I (yield 89%); melting point was 66-68°C.

[0040] (2) In a mixed solvent of 35mL absolute ethanol + 10mL dichloromethane, first add 1.19g (5.0mmol) of nickel dichloride hexahydrate and stir vigorously until complete...

Embodiment 2

[0045] A preparation method of a metal complex containing P / N / Si / S / Ni synergistically catalyzed and flame-retardant is:

[0046] (1) In 30mL of dichloromethane, first add 2.3mL (10mmol) of 3-aminopropyltriethoxysilane, then slowly add 4.1mL (23mmol) of diphenylphosphorous chloride, then slowly add 3.1 mL (22 mmol) of triethylamine; after stirring overnight at room temperature, a light yellow suspension was obtained, which was filtered through a sand core to remove the triethylamine hydrochloride solid to obtain a light yellow liquid, which was rotary evaporated to remove dichloromethane to obtain Solid crude product; finally, it was washed with tetrahydrofuran, recrystallized from dichloromethane and dried in vacuo to obtain a pale white solid, which is intermediate I (yield 88%).

[0047] (2) In a mixed solvent of 35mL absolute ethanol + 10mL dichloromethane, first add 1.10g (5.0mmol) of anhydrous nickel dibromide and stir vigorously until completely dissolved, then add 3.25g...

Embodiment 3

[0050] A preparation method of a metal complex containing P / N / Si / S / Ni synergistically catalyzed and flame-retardant is:

[0051] (1) In 30mL of dichloromethane, first add 2.3mL (10mmol) of 3-aminopropyltriethoxysilane, then slowly add 4.1mL (23mmol) of diphenylphosphorous chloride, then slowly add 3.1 mL (22 mmol) of triethylamine; after stirring overnight at room temperature, a light yellow suspension was obtained, which was filtered through a sand core to remove the triethylamine hydrochloride solid to obtain a light yellow liquid, which was rotary evaporated to remove dichloromethane to obtain Solid crude product; finally, it was washed with tetrahydrofuran, recrystallized from dichloromethane and dried in vacuo to obtain a pale white solid, which is intermediate I (91% yield).

[0052] (2) In a mixed solvent of 35mL anhydrous methanol + 10mL dichloromethane, first add 1.34g (5.0mmol) of anhydrous nickel diiodide and stir vigorously until completely dissolved, then add 3.25...

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Abstract

The invention relates to an intumescent metal flame-retardant agent, in particular to a concerted catalysis flame-retardant metal complex containing P / N / Si / S / Ni and a preparation method of the complex. An intermediate II can be used for preparing various concerted catalysis flame-retardant metal complexes containing P / N / Si / S / Ni. According to the metal complex, the four flame-retardant elements including P, N, Si and S are integrated into one molecule and coordinated on a metal atom, synergetic intumescent flame resistance of various flame-retardant elements and catalyzing carbonization flame resistance of metal elements are fully achieved, and the flame-retardant effect of the metal complex serving as a flame-retardant agent is greatly improved. Molecules of the flame-retardant agent do not contain halogen atoms and contain siloxane groups easy to react and decompose, so no harmless gas or formaldehyde is released in the combustion process, and the requirement for environmental friendliness in the flame-retardant combustion process of modern flame-retardant agents is met. Meanwhile, under the condition that consumption is small, the metal complex can be used for durability flame-retardant treatment of various cotton fabric substrates, and a good expected flame-retardant effect can be achieved.

Description

technical field [0001] The invention relates to an intumescent metal flame retardant, in particular to a P / N / Si / S / Ni synergistic catalytic flame-retardant metal complex and a preparation method thereof. Background technique [0002] With the rapid development of science and technology, the number and scope of use of polymer materials are increasing day by day, but they have one thing in common that is flammable or combustible, and a flame retardant is an effective substance that can prevent materials from igniting or inhibit flame propagation . Therefore, the design and preparation of flame retardants has become a research hotspot in the field of flame retardant polymer materials and has attracted much attention. See: Chen, L.; Wang, Y.Z. Polym. Adv. Technol., 2010, 21, 1-19. [0003] In the development and application of flame retardants, halogenated flame retardants are still the most used organic flame retardants in the world due to their advantages of less addition and...

Claims

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Application Information

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IPC IPC(8): C07F15/04D06M13/513C08K5/548D06M101/06
CPCC07F15/045C08K5/544D06M13/513D06M2101/06D06M2200/30
Inventor 赵培华李玉龙毋登辉马钟义
Owner ZHONGBEI UNIV
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