Method for preparing mesoporous silica/ammonium polyphosphate compound fire retardant

A technology of mesoporous silica and composite flame retardant, which can be used in fire-resistant coatings, etc., can solve the problems of affecting wood decoration and visual effects, poor compatibility of wood materials, a large amount of smoke and poisonous gas, etc., to achieve high pore volume and improve poor dispersion. , the effect of high specific surface area

Inactive Publication Date: 2014-07-23
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, APP has the following disadvantages as an inorganic flame retardant: (1) strong moisture absorption, easy to agglomerate, not suitable for use in high temperature and humid environments; (2) poor compatibility with wood materials, easy to migrate (3) Depolymerization reaction will occur under the action of water or acid and alkali, and it will be easily soluble in water and lost; (4) While being flame retardant, it will also catalyze the production of lots of smoke and gas

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 8.4 g of dodecyltrimethylammonium bromide in a mixed solution of 630 ml of methanol and 1500 ml of water, add 15 ml of 1M NaOH solution, and stir well. Then, add 12.4g tetraethyl orthosilicate dropwise, react at room temperature for 8 hours, transfer to a polytetrafluoroethylene bottle at 90°C and seal and age for 24 hours, filter to obtain a white powder, and dry it in vacuum. silicon oxide.

[0019] Add 85% phosphoric acid and urea into the three-necked flask in a molar ratio of 1:1.6, stir, slowly raise the temperature to 80°C, react for 30 minutes and the solution becomes clear, then add mesoporous silica with a mass ratio of 35%, and stir for 4 hours. Filtrate while hot, rinse with absolute ethanol three times, dry, send the powder into a box-type reactor, polymerize and solidify at 220°C for 2 hours, crush and sieve after cooling, and obtain a composite of mesoporous silica / ammonium polyphosphate flame retardant.

Embodiment 2

[0021] Dissolve 8.4 g of dodecyltrimethylammonium bromide in a mixed solution of 630 ml of methanol and 1500 ml of water, add 15 ml of 1M NaOH solution, and stir well. Then, add 12.4g tetraethyl orthosilicate dropwise, react at room temperature for 8 hours, transfer to a polytetrafluoroethylene bottle at 90°C and seal and age for 24 hours, filter to obtain a white powder, and dry it in vacuum. silicon oxide.

[0022] Add 85% phosphoric acid and urea into the three-necked flask in sequence at a molar ratio of 1:1.8, stir, slowly raise the temperature to 80°C, and react for 20 minutes, and the solution becomes clear, then add mesoporous silica with a mass ratio of 30%, and stir for 6 hours , filtered while hot, rinsed with absolute ethanol three times, dried in the air, sent the powder into a box-type reactor, polymerized and solidified at 230°C for 1 hour, crushed and sieved after cooling, and obtained mesoporous silica / ammonium polyphosphate Composite flame retardant.

Embodiment 3

[0024] Dissolve 8.4 g of dodecyltrimethylammonium bromide in a mixed solution of 630 ml of methanol and 1500 ml of water, add 15 ml of 1M NaOH solution, and stir well. Then, add 12.4g tetraethyl orthosilicate dropwise, react at room temperature for 8 hours, transfer to a polytetrafluoroethylene bottle at 90°C and seal and age for 24 hours, filter to obtain a white powder, and dry it in vacuum. silicon oxide.

[0025] Add 85% phosphoric acid and urea into a three-necked flask in a molar ratio of 1:2.0, stir, slowly raise the temperature to 80°C, react for 10 minutes and the solution becomes clear, then add mesoporous silica with a mass ratio of 25%, and stir for 8 hours , filtered while hot, rinsed with absolute ethanol three times, dried, sent the powder into a box-type reactor, polymerized and solidified at 240°C for 1 hour, crushed and sieved after cooling, and obtained mesoporous silica / ammonium polyphosphate Composite flame retardant.

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Abstract

A method for preparing a mesoporous silica / ammonium polyphosphate composite flame retardant, comprising the following steps: adding 85% phosphoric acid and urea into a reactor according to a certain ratio, mixing, and reacting at a low temperature for a period of time to obtain a transparent solution; Then add an appropriate amount of mesoporous silica, fully soak, filter and separate, rinse with absolute ethanol, and dry naturally; send the obtained powder into a box furnace, foam at high temperature, polymerize and solidify for a period of time, crush and sieve, that is A mesoporous silica / ammonium polyphosphate composite flame retardant is obtained. The composite flame retardant prepared by the invention is nano-particles with good dispersibility, ammonium polyphosphate is generated "in situ" in the silica carrier, has good moisture resistance, is not easy to migrate, has excellent synergistic flame retardant and smoke suppression effects, and can Widely used in flame retardant of various materials.

Description

technical field [0001] The invention relates to a method for preparing a novel mesoporous silica / ammonium polyphosphate nanocomposite flame retardant, in particular to a method for preparing a mesoporous silica / ammonium polyphosphate composite flame retardant. Background technique [0002] Fire is a common catastrophic problem faced by people all over the world, which has caused huge loss of life and property to human society. With the gradual improvement of people's living standards, the consumption of polymer materials and wood materials for construction and interior decoration is increasing year by year. However, both polymer materials and wood materials are flammable and combustible materials, which can easily lead to the spread of fire. When burning, they release a large amount of heat energy, which intensifies the fire hazard, and the released large amount of smoke and gas cause poisoning and casualties. Therefore, the flame retardant and smoke suppression treatment o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K21/04
Inventor 夏燎原胡云楚袁利萍陈旬吴义强吴志平
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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