A kind of preparation method of fluorosilane surface modified ultrafine ammonium polyphosphate

A technology of ammonium polyphosphate and surface modification, applied in coatings, fireproof coatings, etc., can solve the problems of high energy consumption, complex thermal surface treatment process, selection and treatment process to be studied, etc., to achieve experimental parameter control, surface The effect of simple processing technology and equipment, and easy large-scale production

Active Publication Date: 2020-06-26
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN1597024 discloses an anti-resurrection superfine ammonium phosphate dry powder fire extinguishing agent and its preparation method, which adopts silicone oil and fluorocarbon surfactant to carry out dry method modification to the superfine dry powder fire extinguishing agent powder with ammonium polyphosphate as the base material respectively. The superfine dry powder fire extinguishing agent after treatment can float on the surface of diesel oil and water, but its two-step thermal surface treatment process is complicated and consumes a lot of energy, which limits its application. Therefore, the selection and treatment process of surfactants need to be studied

Method used

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  • A kind of preparation method of fluorosilane surface modified ultrafine ammonium polyphosphate
  • A kind of preparation method of fluorosilane surface modified ultrafine ammonium polyphosphate
  • A kind of preparation method of fluorosilane surface modified ultrafine ammonium polyphosphate

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Experimental program
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Effect test

Embodiment 1

[0032] (1) Use a supersonic jet mill to crush ammonium polyphosphate into an ultrafine powder with a particle size of 90% ≤ 5 μm;

[0033] (2) Dry the refined powder at a high temperature of 100°C for 12 hours;

[0034] (3) Spray the n-hexane solution of perfluorodecyltriethoxysilane on the surface of ultrafine ammonium polyphosphate powder at a stirring rate of 1500 r / min, wherein the amount of perfluorodecyltriethoxysilane is super 0.5% of the weight of the fine powder, wherein the amount of n-hexane is 4 times that of perfluorodecyltriethoxysilane;

[0035] (4) Mix well and place in an oil bath at 80°C for 2 hours;

[0036] (5) Cooling, crushing, sieving and performance testing.

[0037] The superfine ammonium polyphosphate powder of above-mentioned preparation is carried out performance test, and characterizing result is as follows:

[0038] (1) Use the optical method contact angle / interfacial tension SL200KS contact angle tester authorized by American Kono Industries C...

Embodiment 2

[0041] (1) Use a supersonic jet mill to crush ammonium polyphosphate into an ultrafine powder with a particle size of 90% ≤ 5 μm;

[0042] (2) Dry the refined powder at a high temperature of 110°C for 10 hours;

[0043] (3) Spray the tridecafluorooctyltriethoxysilane isopropanol solution on the surface of the ultrafine ammonium polyphosphate powder at a stirring rate of 1500 r / min, in which the tridecafluorooctyltriethoxysilane The amount is 3% of the weight of the ultrafine powder, and the amount of isopropanol is 5 times that of tridecafluorooctyltriethoxysilane;

[0044] (4) Mix well and place in an oil bath at 110°C for 1 hour;

[0045](5) Cooling, crushing, sieving and performance testing.

[0046] The superfine ammonium polyphosphate powder of above-mentioned preparation is carried out performance test, and characterizing result is as follows:

[0047] (1) Use the optical method contact angle / interfacial tension SL200KS contact angle tester authorized by American Kono...

Embodiment 3

[0050] (1) Use a supersonic jet mill to crush ammonium polyphosphate into an ultrafine powder with a particle size of 90% ≤ 5 μm;

[0051] (2) Dry the refined powder at a high temperature of 110°C for 10 hours;

[0052] (3) Spray the perfluorodecyltriethoxysilane acetone solution on the surface of the ultrafine ammonium polyphosphate powder at a stirring rate of 1000 r / min, wherein the amount of perfluorodecyltriethoxysilane is ultrafine 5% of the weight of the powder, where the amount of acetone is 6 times that of perfluorodecyltriethoxysilane;

[0053] (4) Mix well and place in an oil bath at 90°C for 1.5 hours;

[0054] (5) Cooling, crushing, sieving and performance testing.

[0055] The superfine ammonium polyphosphate powder of above-mentioned preparation is carried out performance test, and characterizing result is as follows:

[0056] (1) Use the optical method contact angle / interfacial tension SL200KS contact angle tester authorized by the American Kono Industry Co....

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Abstract

The invention discloses a preparation method of superfine ammonium polyphosphate modified by fluorosilane surface. The method comprises: (1) pulverizing ammonium polyphosphate into ultrafine powder with a particle size of 90% less than or equal to 5 μm; (2) drying at high temperature; (3) spraying the fluorosilane organic solution on the surface of the ultrafine powder under stirring; (4) heat treatment; (5) cooling, crushing and sieving to obtain hydrophobic and oleophobic ultrafine ammonium polyphosphate powder. The method adopts a dry modification process, is simple and environmentally friendly, has high production efficiency, is easy to scale production, and the prepared hydrophobic and oleophobic powder can be widely used in ultrafine dry powder fire extinguishing agents, intumescent flame retardant coatings and fire retardant coatings, etc. field.

Description

technical field [0001] The invention relates to the field of surface modification of flame retardant materials, in particular to a preparation method of fluorosilane surface modified ultrafine ammonium polyphosphate. Background technique [0002] Because ammonium polyphosphate (APP) contains high flame retardant elements such as phosphorus and nitrogen (theoretical phosphorus and nitrogen content are 31.92% and 14.44%, respectively), and there is a P-N synergistic effect, it is currently the most popular inorganic phosphorus flame retardant. One of the most important varieties. Both APP itself and pyrolysis products are non-toxic, and have the advantages of thermal stability, excellent flame retardant performance, no corrosion and smoke suppression, etc. And fireproof coatings and other fields, but APP is an inorganic polymer compound with strong hydrophilicity and certain solubility. During use, it is easy to migrate from the inside of the material to the surface and gradu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09D5/18C09K21/12C09K21/14
CPCC09D5/185C09K21/12C09K21/14
Inventor 付阳阳陆松张和平
Owner UNIV OF SCI & TECH OF CHINA
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