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Polymer modified layered silicate flame retardant and preparation method thereof

A modified layer and silicate technology, which is applied in the direction of silicon compounds, chemical instruments and methods, dyed low-molecular organic compounds, etc. Broad molecular mass distribution, affecting the application performance of flame retardant polymers, etc., to achieve the effect of improving flame retardant and mechanical properties

Inactive Publication Date: 2013-10-16
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are still many problems in montmorillonite that need to be further studied and solved, such as: the flame retardant and smoke suppression effects of layered silicate are not significant, and the solution to this problem is extremely critical for the application of organic montmorillonite as a flame retardant
Wang Jincheng et al. (Wang Jincheng et al., dendritic flame retardant layered silicate and its preparation method, ZL 201010022884.2) modified montmorillonite with dendritic polymers, and the flame retardant effect was improved to a certain extent, but the polymer The relative molecular mass distribution is relatively wide, which affects its flame retardant effect and application performance in polymers to a certain extent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Mix 10g of inorganic montmorillonite with 10g of dodecylbishydroxyethylmethyl ammonium chloride, add 10mL of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1.5), stir at 70°C for 4h, and then separate the solid and liquid , washed, and dried in vacuum at 90° C. for 3 h to collect the organic montmorillonite.

[0033] Disperse 10g of organic montmorillonite in a 30g ice-water bath, add 1 mole of triethylamine, then dropwise add 1 mole of 2-bromoisobutyryl bromide to the solution, react at 20°C for 48h, wash the product with ethanol, and centrifuge. Dry in vacuum to obtain brominated organic montmorillonite.

[0034] Weigh 10g of brominated organomontmorillonite, 1 mole of CuCl, 0.1 mole of CuCl 2 , ultrasonically dispersed into 100g of anisole, and then added a mixture of 1 mole of butanediamine, 1 mole of acrylonitrile and 0.1 mole of iron, and quickly put the sealed tube into liquid nitrogen, after 3 times of freezing, vacuuming, The circulation ...

Embodiment 2

[0038] Mix 20g of inorganic montmorillonite with 20g of octadecyl bishydroxydimethylbenzyl ammonium chloride, add 10mL of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1.6), stir at 75°C for 3.5h, and then solidify The liquid was separated, washed, and dried in vacuum at 80°C for 3.5 hours to collect the organic montmorillonite.

[0039] Disperse 10 g of organic montmorillonite in a 40 g ice-water bath, add 1 mole of triethylamine, then dropwise add 1.5 moles of 2-bromoisobutyryl bromide to the solution, react at 30°C for 36 h, wash the product with ethanol, and centrifuge. Dry in vacuum to obtain brominated organic montmorillonite.

[0040] Weigh 10g of brominated organomontmorillonite, 3 moles of CuCl, 0.6 moles of CuCl 2 , ultrasonically dispersed into 130g of anisole, and then added a mixture of 3 moles of butanediamine, 6 moles of acrylonitrile and 0.6 moles of cobalt, and quickly put the sealed tube into liquid nitrogen, after 4 times of freezing, ...

Embodiment 3

[0044] Mix 40g of inorganic montmorillonite with 30g of octadecyl bishydroxytrimethylammonium bromide, add 10mL of aqueous ethanol (the volume ratio of ethanol to water is 1:1.7), stir at 80°C for 3h, and then separate the solid and liquid. After washing, vacuum drying at 70°C for 4 hours, the organic montmorillonite was collected.

[0045] Disperse 10g of organic montmorillonite in a 50g ice-water bath, add 1 mole of triethylamine, then dropwise add 2 moles of 2-bromoisobutyryl bromide to the solution, react at 40°C for 24h, wash the product with ethanol, and centrifuge. Dry in vacuum to obtain brominated organic montmorillonite.

[0046] Weigh 10g of brominated organomontmorillonite, 4 moles of CuCl, 1.2 moles of CuCl 2 , ultrasonically dispersed into 160g of anisole, and then added a mixture of 4 moles of butanediamine, 12 moles of acrylonitrile and 1.2 moles of nickel, and quickly put the sealed tube into liquid nitrogen, after 5 times of freezing, vacuuming, The circula...

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PUM

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Abstract

The invention discloses a polymer modified layered silicate flame retardant and a preparation method thereof. The preparation method includes the following steps: (1) mixing inorganic montmorillonite and an organic intercalation agent, adding ethanol water solution, and then collecting organic montmorillonite; (2) dispersing the organic montmorillonite in an ice-water bath, adding triethylamine, adding 2-methylpropionyl bromide in the solution, reacting, and then collecting the bromized organic montmorillonite from reaction products; and (3) dispersing the bromized organic montmorillonite, CuCi and CuCi2 in anisole, adding butanediamine, acrylonitrile and a catalyst, freezing, vacuumizing, and dissolving, reacting, placing in the environment at the temperature of 10-30 DEG C, stopping reaction, and collecting products from reaction products. The polymer modified layered silicate flame retardant and the preparation method of the polymer modified layered silicate flame retardant can be applied to rubber industries and cable industries, can improve anti-flaming and mechanical properties and the like of rubber materials, and has substantial economic benefit and certain social influence.

Description

technical field [0001] The invention relates to a silicate flame retardant and a preparation method thereof. Background technique [0002] With the development of economy and urban construction, the fire loss is on the rise, so the prevention of fire is very important at home and abroad. Commonly used halogenated flame retardants decompose a large amount of toxic smoke during combustion, which can easily poison and suffocate personnel present and affect vision and escape. Hydroxide integrates the triple functions of flame retardant, smoke suppression and filling. It is non-toxic and non-corrosive substances produced during combustion. The raw materials are easy to obtain and cheap. The impact is serious. Therefore, it is of great significance to research and develop new flame retardants that meet the requirements of fire safety and environmental protection and have little effect on the mechanical and electrical properties of materials. [0003] Montmorillonite is one of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/40C01B33/44C08K9/04C08K3/34C09C1/42C09C3/10C09C3/08
Inventor 王锦成吴鼎赵艺郝文莉
Owner SHANGHAI UNIV OF ENG SCI