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P/N/Si multi-element synergistic integrated nano flame retardant as well as preparation method and application thereof

A nano-flame retardant and multi-component technology, applied in the field of flame retardant, can solve the problems that it is difficult to meet the development requirements of green chemistry, the toxicity and oxidation of raw materials are strong, and the flame retardant efficiency is barely improved, so as to suppress the release of toxic fumes, The effect of reducing the possibility and improving the flame retardant effect

Active Publication Date: 2021-11-26
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, some raw materials in the preparation process of the flame retardant in this patent are extremely toxic and oxidative, and it is difficult to meet the development requirements of green chemistry
Patent CN110128836A relates to a phosphorus-silicon flame retardant and its preparation method. The inventor uses phenylphosphoryl dichloride to react with hydroxyl-terminated silicone oil, and prepares a new type of phosphorus-containing silicon by replacing two chlorine atoms of phenylphosphoryl dichloride. Flame retardant, but the flame retardant efficiency is slightly improved, and the limiting oxygen index is up to 25%.
Patent CN105175780A relates to a nitrogen-phosphorus-silicon-containing acrylate flame retardant and a method for preparing a flame-retardant epoxy acrylate coating. The flame-retardant coating prepared by the inventor has high light transmittance, strong flame retardancy, and mechanical properties It has the advantages of excellent performance and good thermal stability, but its preparation process is complicated, which is not conducive to large-scale industrial production

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  • P/N/Si multi-element synergistic integrated nano flame retardant as well as preparation method and application thereof
  • P/N/Si multi-element synergistic integrated nano flame retardant as well as preparation method and application thereof
  • P/N/Si multi-element synergistic integrated nano flame retardant as well as preparation method and application thereof

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Experimental program
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Effect test

preparation example Construction

[0032] Such as figure 1 Shown, a kind of P / N / Si multiple synergistic integrated nano-flame retardant and preparation method thereof, comprises the following steps:

[0033] (1) Dissolve an appropriate amount of transition metal salt compound in an appropriate amount of methanol, and stir evenly;

[0034] (2) Dissolve an appropriate amount of 2-methylimidazole in an appropriate amount of methanol, dropwise add it to the solution in step (1), and after ultrasonic stirring, centrifuge to obtain the product, wash it with a solvent for 2 to 5 times, and then wash it at 50 to 80 Dry in an oven at ℃ for 3-10 hours to obtain MOF;

[0035] (3) Take an appropriate amount of MOF powder and disperse it in methanol. After forming a uniform suspension, add a certain amount of phytic acid dropwise, and stir the reaction at room temperature. After the reaction, the product is obtained by centrifugation, washed 2 to 5 times with solvent, and Dry in an oven at 50-80°C for 3-10 hours to obtain...

Embodiment 1

[0040] (1) Take 5.6g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 25mL of methanol, and stirred evenly;

[0041] (2) Dissolve 12.0g of 2-methylimidazole in 25mL of methanol, add dropwise to the solution in step (1), and after ultrasonic stirring for 12 hours, centrifuge to obtain the product, wash it with solvent for 3 times, and then place it in an oven at 80°C Dry for 10h to obtain ZIF-8;

[0042] (3) Get 0.5g ZIF-8 powder and disperse it in 25mL methanol, after forming a uniform suspension, add 5mL of 0.5wt% phytic acid dropwise, and stir and react at room temperature for 12h. Wash with solvent for 3 times, and then dry in an oven at 80°C for 10 hours to obtain ZIF-8@PA;

[0043](4) Take 0.625g CTAB and disperse it in 30mL ethanol, and stir it ultrasonically for 30min;

[0044] (5) Add 0.5g ZIF-8@PA to the solution in step (4), and ultrasonically form a uniform suspension;

[0045] (6) Take 0.25g TEOS and dilute it in 25mL ethanol, then add it dropwise to the mixed solution i...

Embodiment 2

[0047] (1) Take 6.4g Co(NO 3 ) 2 ·6H 2 O was dissolved in 25mL of methanol, and stirred evenly;

[0048] (2) Dissolve 8.9g of 2-methylimidazole in 25mL of methanol, add it dropwise to the solution in step (1), and after ultrasonic stirring for 12 hours, centrifuge to obtain the product, wash it with a solvent for 3 times, and then place it in an oven at 80°C Dry for 10h to obtain ZIF-67;

[0049] (3) Get 1.0g ZIF-67 powder and disperse it in 25mL methanol, after forming a uniform suspension, add 20mL of 0.5wt% phytic acid dropwise, and stir and react at room temperature for 12h. Wash with solvent for 3 times, and then dry in an oven at 80°C for 10 hours to obtain ZIF-67@PA;

[0050] (4) Take 0.5g CTAB and disperse it in 30mL ethanol, and stir it ultrasonically for 30min;

[0051] (5) Add 0.6g ZIF-67@PA to the solution in step (4), and ultrasonically form a uniform suspension;

[0052] (6) Dilute 0.1 g of TEOS in 25 mL of ethanol, then dropwise add it to the mixed solutio...

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Abstract

The invention discloses a P / N / Si multi-element synergistic integrated nano flame retardant as well as a preparation method and application thereof. The flame retardant comprises a transition metal organic framework, and a phytic acid coating layer and a SiO2 coating layer which sequentially coat the transition metal organic framework. The preparation method comprises the following steps: preparing the transition metal organic framework MOF; dropwise adding a certain amount of phytic acid into a MOF uniform suspension, carrying out stirring reaction at room temperature, and after the reaction is finished, centrifuging, washing and drying to obtain MOF@PA; and growing SiO2 on the surface of the MOF@ PA by taking the MOF@ PA as a core and adopting a sol-gel method. The flame retardant combines excellent characteristics of flame-retardant elements such as P, N, Si, transition metal and the like, not only can play a synergistic role to improve the flame-retardant effect and effectively inhibit release of toxic smoke, but also can be widely applied to high polymer materials such as polyurethane, epoxy resin, polypropylene and the like to improve the flame-retardant property of the high polymer materials and reduce the possibility of casualties.

Description

technical field [0001] The invention relates to the field of flame retardant technology, in particular to a P / N / Si multiple synergistic integrated nano flame retardant and its preparation method and application. Background technique [0002] Adding chlorine- and bromine-containing flame retardants to flame-retardantly treat flammable polymer materials has the advantages of simple use, low cost, and good flame-retardant effects. However, polymer materials containing halogen flame retardants will produce dense smoke and a large amount of corrosive gases when burned, causing damage to the environment and human health. With the global strong appeal for green and environmentally friendly flame retardants, the research and development of green and environmentally friendly halogen-free flame retardants has become one of the important topics of current flame retardant research. [0003] Phosphorus-based flame retardants, as one of the most promising environmentally friendly substit...

Claims

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Application Information

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IPC IPC(8): C08L87/00C08K3/36C08K5/521C08G83/00C08L75/04C08L63/00C08L23/12
CPCC08K3/36C08K5/521C08G83/008C08L75/04C08L63/00C08L23/12C08L2201/02C08L87/00
Inventor 周克清印恋公凯利鲁江涛
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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