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A kind of intumescent flame retardant functionalized hydrotalcite flame retardant and preparation method thereof

An intumescent flame retardant and hydrotalcite technology, which is applied in the field of flame retardants, can solve the problems affecting the flame retardant performance and poor thermal stability of nano-composite materials, and achieve the effects of easy industrial production, stable performance and improved mechanical properties.

Active Publication Date: 2018-06-05
TAIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the organically treated hydrotalcite can be well dispersed in the polymer, the intercalation agent used is often a long carbon chain organic anion compound with poor thermal stability and no flame retardancy (such as cetyl sodium sulfate ), thus affecting the flame retardancy of polymer / hydrotalcite nanocomposites

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 10.0g of hydrotalcite to 500mL of toluene, ultrasonically disperse for 30 minutes, transfer to a dry four-neck flask equipped with mechanical stirring, thermometer, reflux condenser and dropping funnel, add 1.0g of 3-aminopropane dropwise at room temperature Trimethyloxysilane and 20 mL of toluene mixed solution, and heated to 100 ° C, continued to stir the reaction for 6 hours, cooled to 40 ° C, dropwise added 1.30 g of diethylphosphoryl chloride, 5 g of triethylamine and 30 mL of toluene mixed solution, The reaction was continued for 5 hours. Then the slurry obtained by the reaction was filtered, washed repeatedly with ethanol, and dried in an oven at 80° C. for 24 hours to obtain an intumescent flame retardant functionalized hydrotalcite flame retardant with a yield of 98.1%.

Embodiment 2

[0024] The synthesis operation of the intumescent flame retardant functionalized hydrotalcite flame retardant is the same as in Example 1. The reaction temperature of hydrotalcite and 3-aminopropyltrimethyloxysilane is 50°C, and the reaction time is 10 hours. After adding diethyl phosphorus oxychloride, the reaction is continued for 12 hours, and the reaction temperature is 0°C. Hydrotalcite and 3- The mass ratio of aminopropyltriethoxysilane is 1.0:0.25, the ratio of 3-aminopropyltriethoxysilane to diethylphosphoryl chloride is 1.0:1.5, and the solvent is ethyl acetate. The volumetric dosage of ethyl acetate is 200ml / g based on the mass of hydrotalcite, the acid-binding agent is triethylamine, the ratio of triethylamine to diethylphosphoryl chloride is 1.0:5.0, and the yield is 90.6%. .

Embodiment 3

[0026] The synthesis operation of the intumescent flame retardant functionalized hydrotalcite flame retardant is the same as in Example 1. The reaction temperature of hydrotalcite and 3-aminopropyltriethoxysilane is 130°C, and the reaction time is 2 hours. After adding diethyl phosphorus oxychloride, the reaction is continued for 2 hours, and the reaction temperature is 100°C. Hydrotalcite and 3-ammonia The mass ratio of propyltriethoxysilane is 1.0:0.01, the ratio of 3-aminopropyltriethoxysilane to diethylphosphoryl chloride is 1.0:1.0, and the solvent is xylene, xylene The volume dosage is 50ml / g based on the mass of hydrotalcite, the acid-binding agent is triethylamine, the ratio of triethylamine to diethylphosphoryl chloride is 1.0:1.0, and the yield is 87.6%.

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PUM

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Abstract

The invention provides an intumescent flame retardant functionalized hydrotalcite flame retardant. The flame retardant is good in flame retardant effect, and adopts a halogen-free system, so that secondary harm during combustion of materials is reduced. The intumescent flame retardant functionalized hydrotalcite flame retardant is prepared through the steps as follows: a silane coupling agent containing amine groups and hydrotalcite powder particles react with each other to prepare silane coupling agent modified hydrotalcite, and then, the silane coupling agent modified hydrotalcite and diethyl chlorophosphate react with each other. The flame retardant is wide in application range, good in flame resistant effect, and stable in performance; the preparation process of the flame retardant is simple and convenient in operation, the cost is low, the solvent recycling is convenient, and obtained products are easy to separate, so that the industrial production is facilitated.

Description

technical field [0001] The invention relates to a flame retardant, in particular to an intumescent flame retardant functionalized hydrotalcite flame retardant and a preparation method thereof. Background technique [0002] Intumescent flame retardant, as a kind of halogen-free flame retardant, is widely used in flame retardant polymers with the rise of flame retardant technology. When the polymer containing this type of flame retardant is heated, a uniform layer of carbon can be formed on the surface. The high-quality foam layer plays the role of heat insulation, oxygen insulation, smoke suppression, and prevents the phenomenon of dripping, and has good flame retardant performance. Intumescent flame retardants generally use phosphorus and nitrogen as the main flame retardant element, and there are usually two types: mixed type and single-component type. The mixed type intumescent flame retardant is made by mixing carbon source, acid source, and gas source compounds in a cert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/06C08K9/04C08K3/34C08L23/16
Inventor 黄国波
Owner TAIZHOU UNIV
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