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Preparation method of phosphorus-nitrogen-silicon synergistic phyllosilicate flame retardant

A layered silicate and flame retardant technology, applied in the field of flame retardant preparation, can solve problems such as poor compatibility and damage to the physical and mechanical properties of polymers, achieve durable flame retardant performance, improve flame retardant and mechanical properties, etc. The effect of high performance and thermal stability

Inactive Publication Date: 2015-07-15
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame retardant prepared by this patent needs to be roasted at high temperature, there is no organic substance on the surface, and the compatibility with organic polymers is poor. If organic polymers are added, the physical and mechanical properties of the polymers will be damaged to a certain extent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] A method for preparing a phosphorus-nitrogen-silicon synergistic layered silicate flame retardant comprises the following steps:

[0023] (1) Acidification modification of inorganic montmorillonite:

[0024] Use hydrochloric acid to adjust the pH value of pure water to 4-5, add montmorillonite, heat and stir in a water bath at 60-80°C for 20-40min, the stirring rate is 2000-4000r / min, the product is centrifugally precipitated, washed and dried to obtain acidified montmorillonite desoiling;

[0025] (2) Preparation of pentaerythritol solution:

[0026] Mix pentaerythritol and ethyl acetate, the ratio of pentaerythritol and ethyl acetate is 1-5g / 20-40ml, and then stir at 60-80°C for 1-2 hours to obtain pentaerythritol solution;

[0027] (3) Preparation of pentaerythritol modified organic montmorillonite:

[0028] Under the protection of nitrogen, mix pentaerythritol solution and acidified montmorillonite, the ratio of pentaerythritol solution and acidified montmorillon...

Embodiment 1

[0035] Use 5g of hydrochloric acid to adjust the pH value of 20g of pure water to 5, add 5g of montmorillonite, heat and stir in a water bath at 60°C for 20min at a stirring rate of 2000r / min, centrifuge the product, wash and dry it to obtain acidified montmorillonite. Mix 1 g of pentaerythritol and 20 ml of ethyl acetate, and stir at 60°C for 1 hour to obtain a pentaerythritol solution. Under the protection of nitrogen, mix 5g of pentaerythritol solution and 1g of acidified montmorillonite, heat to 70°C, keep stirring for 1 hour, and collect the solid in it, which is pentaerythritol-modified organic montmorillonite. Under the protection of nitrogen, 5g of pentaerythritol-modified organomontmorillonite and 30g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were mixed, stirred at 70°C for 2h, and the product was centrifuged Precipitate and vacuum dry at 70°C for 4 hours to obtain the target flame retardant.

[0036] The particle size of the final flame retardant ...

Embodiment 2

[0038] Use 8g of hydrochloric acid to adjust the pH value of 30g of pure water to 4.5, add 8g of montmorillonite, heat and stir in a water bath at 70°C for 30min at a stirring rate of 3000r / min, centrifuge the product, wash and dry it to obtain acidified montmorillonite. Mix 3g of pentaerythritol and 30ml of ethyl acetate, and stir at 70°C for 1.5h to obtain a pentaerythritol solution. Under the protection of nitrogen, mix 8g of pentaerythritol solution and 2g of acidified montmorillonite, heat to 80°C, heat and stir for 2h, collect the solid in it, which is pentaerythritol modified organic montmorillonite; under nitrogen protection, modify 8g of pentaerythritol to Mix organic montmorillonite with 40g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), stir at 80°C for 1.5h, centrifuge the product, and dry it in vacuum at 80°C for 3h. Get the target flame retardant.

[0039] The particle size of the final flame retardant and the center temperature of thermal weight los...

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Abstract

The invention relates to a preparation method of a phosphorus-nitrogen-silicon synergistic phyllosilicate flame retardant, which comprises the following steps: (1) carrying out acidifying modification on inorganic montmorillonite; (2) preparing a pentaerythritol solution; (3) preparing pentaerythritol modified organic montmorillonite; and (4) preparing the target flame retardant. Compared with the prior art, the phosphorus-nitrogen-silicon synergistic phyllosilicate flame retardant is applicable to rubber industry and cable industry, can substitute or partially substitute the traditional high-price environment-unfriendly flame-retardant and reinforcing material capable of damaging other properties of polymers, is beneficial to improving the traditional industry, can enhance the flame retardancy, mechanical properties and other properties of the rubber material, and is beneficial to opening the application market of montmorillonite and other mineral resources.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a phosphorus-nitrogen-silicon synergistic layered silicate flame retardant. Background technique [0002] Polymer materials such as plastics, rubber, adhesives and fibers are widely used in our daily life. The obvious disadvantage of these materials is that they are flammable or combustible, and a large amount of smoke and harmful gases will be produced when they are burned, which has a serious impact on people's daily life, especially when it involves personal safety issues. Therefore, the flame retardancy of polymer materials is extremely important. Commonly used halogenated flame retardants will decompose a large amount of toxic smoke during combustion, which can easily poison and suffocate people present, affect vision and escape, and even pose a cancer-causing threat. Therefore, many developed countries have banned their use. [0003] Com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/04C08K3/34C08K5/5313
Inventor 潘晨李茹梦吴佳明王锦成
Owner SHANGHAI UNIV OF ENG SCI
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