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Phosphorus-nitrogen compound modified montmorillonite fire retardant and preparation method thereof

A montmorillonite and compound technology, which is applied in the field of phosphorus-nitrogen compound modified montmorillonite flame retardant and its preparation, can solve the problem of polymer physical and mechanical performance, electrical performance and insulation performance decline, affecting polymer/montmorillonite The flame retardant properties, tensile strength, and impact strength of the soil-removing composite materials are reduced, and the effects of reducing secondary hazards, improving mechanical properties, and improving dispersibility are achieved.

Active Publication Date: 2015-12-16
TAIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current synergy between nano-montmorillonite and intumescent flame retardants is still at the stage of direct physical blending of the two, and it is difficult to achieve uniform dispersion of the two in the polymer matrix, so there is still a lot of room for improvement in the synergistic effect , and most of the intumescent flame retardants participating in the synergistic flame retardant are small molecule flame retardants, which have poor compatibility with polymers, which will reduce the physical and mechanical properties, electrical properties and insulation properties of polymers, especially lead to the tensile properties of materials. The tensile strength and impact strength are greatly reduced
[0003] Although the organically treated montmorillonite can be well dispersed in the polymer, the intercalation agent used is often a long carbon chain modifier with poor thermal stability and no flame retardant effect, which affects the quality of the polymer. / Flame retardant properties of montmorillonite composites

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 10g of montmorillonite to 150mL of toluene, ultrasonically disperse it for 30 minutes, transfer it to a dry four-necked flask equipped with a magnetic stirrer, a thermometer, a reflux condenser and a dropping funnel, and add 1.1295g of N-aminoethyl - Mixture of γ-aminopropyltrimethoxysilane and 30mL toluene, raise the temperature to 105°C, continue stirring for 5 hours, cool down to 65°C, add dropwise 2.494g of 2-oxo-2-chloro-5,5-di The mixed solution of methyl-1,3,2-dioxaphosphorinane, 3.6 g of triethylamine and 20 mL of toluene was continued to react for 4.5 hours. Then the suspension obtained by the reaction was filtered, washed repeatedly with methanol, and dried in an oven at 80° C. for 24 hours to obtain a phosphorus-nitrogen compound-modified montmorillonite flame retardant with a yield of 94.5%.

Embodiment 2

[0024] The synthesis operation of the phosphorus-nitrogen compound modified montmorillonite flame retardant is the same as that in Example 1. The reaction temperature between montmorillonite and N-aminoethyl-γ-aminopropyltrimethoxysilane is 75°C, and the reaction time is 6 hours. Add 2-oxo-2-chloro-5,5-dimethyl- After 1,3,2-dioxaphosphorinane, the reaction was continued for 12 hours, the reaction temperature was 20°C, and the mass ratio of montmorillonite to 3-aminopropyltriethoxysilane was 1.0:0.30, 3- The ratio of aminopropyltriethoxysilane to 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane is 1.0:2.5, Solvent selects butyl acetate for use, and the volume consumption of butyl acetate is 150ml / g based on the quality of montmorillonite, and acid-binding agent selects triethylamine for use, and triethylamine and 2-oxo-2-chloro-5,5-di The molar ratio of methyl-1,3,2-dioxaphosphorinane was 1.0:2.5, and the yield was 96.1%.

Embodiment 3

[0026] The synthesis operation of the phosphorus-nitrogen compound modified montmorillonite flame retardant is the same as that in Example 1. The reaction temperature between montmorillonite and 3-aminopropyltriethoxysilane is 140°C, and the reaction time is 3 hours. Add 2-oxo-2-chloro-5,5-dimethyl-1,3,2 -Continue to react for 2 hours after dioxaphosphine, the reaction temperature is 100°C, the mass ratio of montmorillonite to 3-(2-aminoethylamino)propyltriethoxysilane is 1.0:0.03, 3-aminopropyltriethoxysilane and 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane have a ratio of 1.0: 3.0, the solvent is selected xylene, the volume consumption of xylene is 65ml / g based on the mass of montmorillonite, the acid binding agent is selected pyridine, pyridine and 2-oxo-2-chloro-5,5-dimethyl-1 , The molar ratio of 3,2-dioxaphosphorinane was 1.0:3.5, and the yield was 92.1%.

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Abstract

The invention relates to a fire retardant, particularly to a phosphorus-nitrogen compound modified montmorillonite fire retardant and a preparation method thereof. The phosphorus-nitrogen compound modified montmorillonite fire retardant is prepared through the following method comprising the following steps: reacting an amido-containing silane coupling agent with montmorillonite, so as to obtain silane coupling agent modified montmorillonite; then, reacting the silane coupling agent modified montmorillonite with 2-oxo-2-chlorine-5,5-dimethyl-1,3,2-dioxaphosphorinane, so as to obtain the phosphorus-nitrogen compound modified montmorillonite fire retardant. According to the fire retardant disclosed by the invention, montmorillonite is chemically modified by using a phosphorus-nitrogen compound, so that the dispersity of montmorillonite in polymers is improved, and the problem that the mechanical property of high polymer materials is damaged due to the situation that a fire retardant is added is solved; the fire retardant disclosed by the invention is wide in application range, good in fire retardant effect and stable in property; the fire retardant disclosed by the invention is easy and convenient to operate in preparation process and low in cost, the solvent is convenient to recycle, and the obtained product is easy to separate and industrialize.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a phosphorus-nitrogen compound modified montmorillonite flame retardant and a preparation method thereof. Background technique [0002] Compared with traditional filled polymers, polymer / montmorillonite composites have the advantages of less dosage, low cost, high flame retardant performance, and less smoke generation, but their application range is severely limited due to the low flame retardant level. In order to further improve the flame retardant properties of polymer / montmorillonite composites, the polymer materials were modified by compounding montmorillonite and intumescent flame retardants (containing phosphorus and nitrogen compounds). For the intumescent flame retardant-montmorillonite synergistic flame retardant system, the structural characteristics of the intumescent flame retardant-montmorillonite modified polymer determine the existence of a synergistic flame retardant mechanis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/06C08K9/04C08K3/34C08L23/16C08K13/06C08K3/04C08K3/26C08K5/09C08K3/22C09C1/42C09C3/12C09C3/08
Inventor 黄国波
Owner TAIZHOU UNIV
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