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Intumescent flame retardant functional silicate and preparation method thereof

An intumescent flame retardant and a functionalized technology, applied in the field of preparation of multifunctional flame retardant fillers, can solve the problems of large addition amount, poor dispersion of polymer matrix, large amount of smoke, etc., to promote reinforcement and improve flame retardant performance. , the effect of promoting dispersion

Active Publication Date: 2012-10-31
SOUTH CHINA UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention aims at the good flame retardant effect of the organic flame retardant, but the amount of smoke is large and the cost is high when burning, which affects the mechanical properties of the polymer matrix material; although the inorganic flame retardant has the advantages of being halogen-free, non-toxic, and low-smoke, it is There are problems such as low flame retardant effect, large amount of addition, poor dispersion in polymer matrix, etc., providing an intumescent flame retardant functionalized silicate integrating reinforcement, flame retardant, and smoke suppression functions and its preparation method

Method used

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  • Intumescent flame retardant functional silicate and preparation method thereof
  • Intumescent flame retardant functional silicate and preparation method thereof
  • Intumescent flame retardant functional silicate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Weigh 22.1g (0.1mol) of Y-aminopropyltriethoxysilane and 50mL of toluene into a 250mL four-neck flask, blow in nitrogen, then add 10.1g (0.1mol) of triethylamine for continuous Stir; 22g (0.1mol) of diphenylphosphorus chloride was dissolved in 25mL of toluene, and then slowly added dropwise into the four-necked flask with a constant pressure dropping funnel, the dropping time was 2h, and the temperature rose to 65 ℃, under the protection of nitrogen, continue to react for 10 hours to obtain the product, filter, and distill the filtrate under reduced pressure to obtain the viscous product N-(P,P'-diphenyl)phosphoryl-(3-triethoxysilyl) Propylamine) (DPTSPA) 36.45g, the yield is 90%.

[0038](2) 50g of montmorillonite was pre-ground on a ball mill for 30min, 15g of synthetic viscous product (DPTSPA) was added dropwise to 15mL of 95% (volume concentration) ethanol, and ultrasonically dispersed for 30min (ultrasonic frequency was 20kHz, ultrasonic power was 400W) Add dr...

Embodiment 2

[0043] (1) Weigh 25g of montmorillonite and stir vigorously to disperse it in 100mL of absolute ethanol, then add dropwise 45% ammonia water to adjust the pH value to 9-10, and dissolve 10g of Y-aminopropyltriethoxysilane in 20mL of 95% ethanol (volume concentration) ultrasonically disperse for 30min (ultrasonic frequency is 20kHz, ultrasonic power is 400W), then add to the montmorillonite solution, continue stirring at 60°C for 12h, centrifuge, extract the precipitate with acetone for 48h, and vacuum dry at 80°C for 4h to obtain The product, the grafting rate of silane coupling agent is about 15wt%.

[0044] (2) 20g of amino-modified montmorillonite and 80mL of toluene were placed in a 250mL four-neck flask, nitrogen was introduced, and 0.1mol of sodium carbonate was added, stirring continuously; 22g (0.1mol) of diphenylphosphorous chloride was dissolved in 25mL of toluene, and then slowly drop it into a four-neck flask with a constant pressure dropping funnel, the dropping t...

Embodiment 3

[0047] (1) Weigh 50g of halloysite and stir vigorously to disperse it in 100mL of absolute ethanol, then add dropwise 45% ammonia water to adjust the pH value to 9-10, 23g of N-β(aminoethyl)-Y-aminopropyltrimethyl Oxysilane was dissolved in 20mL 95% ethanol and ultrasonically dispersed for 30min (ultrasonic frequency 20kHz, ultrasonic power 400W), then added to the halloysite solution, stirred at 60°C for 10h, centrifuged, and the precipitate was extracted with acetone for 48h, 80 The product was dried under vacuum at ℃ for 4 hours, and the grafting rate of the silane coupling agent was about 8wt%.

[0048] (2) Put 30g of amino-modified halloysite and 80mL of toluene in a 250mL four-neck flask, blow nitrogen into it, then add 0.05mol of sodium bicarbonate, and keep stirring; 7.7g (0.05mol) of phosphorus oxychloride dissolves in 25mL of acetonitrile, and then slowly drop it into a four-neck flask with a constant pressure dropping funnel. The time for dropping is not less than 3...

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Abstract

The invention discloses an intumescent flame retardant functional silicate and a preparation method thereof. According to the invention, the preparation method comprises the following two methods: one method comprises the steps of first preparing silane coupling agent organic functional silicate, and then preparing the intumescent flame retardant functional silicate on the basis of the former step; and the second method comprises the steps of first preparing a modified silane coupling agent containing phosphorus and nitrogen flame retardant elements, and then modifying inorganic silicate by using the modified silane coupling agent on the basis of the former step. According to the invention, the intumescent flame retardant functional silicate comprises an organic part B and an inorganic part A, wherein the organic part B is grafted to the inorganic part A in such a way that a silanol group formed by after a silane coupling agent containing amino has dehydration reaction with hydroxyls on the surface and between layers of the inorganic part A; and the organic part B is formed in such a way that a phosphoryl chloride compound has elimination reaction with an amino silane coupling agent. The intumescent flame retardant functional silicate disclosed by the invention is integrated with reinforcing, flame retardant and smoke suppressing functions.

Description

technical field [0001] The invention relates to the preparation of a multifunctional flame retardant filler, in particular to a method for preparing an organic / inorganic (organic expansion type phosphorus nitrogen flame retardant / silicate) hybrid nano flame retardant filler. Background technique [0002] Polymer materials, whether it is plastic, rubber, or fiber, generally have a low oxygen index and are flammable materials. When they burn, they will produce a lot of smoke and toxic gases, which will poison people and even kill them. How to reduce the combustion performance of polymer materials has become an important issue. Technological and social issues of growing concern. In recent years, fires caused by polymer materials have occurred frequently, posing a great threat to people's lives and property safety. It is caused by polymer materials with poor flammability. Therefore, all countries have done a lot of work on the development, production, application, testing and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/544C08L75/08C09C1/42C09C1/28C09C3/12
Inventor 陈勇军刘岚贾志欣贾德民李斌张秀芹陈钢何燕岭
Owner SOUTH CHINA UNIV OF TECH
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