Halogen-free synergistic flame-retardant silica aerogel preparation method

A silica and synergistic flame retardant technology, applied in the direction of silica, silica, etc., can solve the problems of preparation cost and performance optimization, high calorific value of airgel combustion, etc., to achieve shortened production cycle, high hydrophobicity, The effect of low density

Inactive Publication Date: 2016-12-21
ECONANO TECH LTD BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the relatively high calorific value of combustion of airgel has become one of the main factors limiting its app

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A preparation method of halogen-free synergistic flame-retardant silica airgel, comprising the steps of:

[0041] S1, mixing the halogen-free flame retardant, the inorganic synergist and the first solvent, and dispersing by ball milling to obtain a suspension A;

[0042] S2. Mix silicon source and water, add acidic aqueous solution and mix to obtain silicic acid sol; add suspension A obtained in S1 to silicic acid sol and mix evenly, adjust pH=5.5, add drying control chemical additives, stir, heat up , heat preservation, pulverization to obtain sol B;

[0043] S3. Take the sol B obtained in S2 for solvent exchange, modify with a silane coupling agent, and dry to obtain a halogen-free synergistic flame-retardant silica airgel.

Embodiment 2

[0045] A preparation method of halogen-free synergistic flame-retardant silica airgel, comprising the steps of:

[0046] S1. Mix ammonium pyrophosphate, antimony trioxide and water, and disperse by ball milling to obtain suspension A, wherein the ball milling speed is 100r / min, the ball milling time is 9h, and the particle diameters of the balls are 8mm, 11mm, 14mm and 20mm respectively The composition of small balls, the weight ratio of ammonium pyrophosphate and antimony trioxide is 1:1, and the weight ratio of the sum of ammonium pyrophosphate and antimony trioxide to water is 1:9;

[0047]S2, mix the water glass with a modulus of 3.5 and a mass fraction of 30wt% with water, add a sulfuric acid aqueous solution with a concentration of 6mol / L and mix to obtain a silicic acid sol; add the suspension A obtained in S1 to the silicic acid sol and mix Mix evenly, adjust pH=5 with sodium carbonate aqueous solution, heat up to 40°C, keep warm for 12 hours, and pulverize to obtain s...

Embodiment 3

[0050] A preparation method of halogen-free synergistic flame-retardant silica airgel, comprising the steps of:

[0051] S1. Mix melamine cyanurate, zinc hydroxystannate and ethanol, and disperse them by ball milling to obtain suspension A, wherein the ball milling speed is 300r / min, the ball milling time is 7h, and the particle diameters of the balls are 8mm, 11mm, 14mm and 20mm respectively Composition of small balls, the weight ratio of melamine cyanurate and zinc hydroxystannate is 40:1, and the weight ratio of the sum of melamine cyanurate and zinc hydroxystannate to the first solvent is 1:19;

[0052] S2, mix the water glass with a modulus of 2 and a mass fraction of 35wt% with water, add a concentration of 4mol / L glacial acetic acid aqueous solution and mix to obtain a silicic acid sol; add the suspension A obtained in S1 to the silicic acid sol Mix well, adjust pH=6 with aqueous sodium hydroxide solution, add N,N-dimethylformamide, stir for 0.5min, raise the temperatur...

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PUM

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Abstract

The invention discloses a halogen-free synergistic flame-retardant silica aerogel preparation method, which comprises: S1, mixing a halogen-free flame retardant agent, an inorganic synergist and a first solvent, and carrying out ball milling dispersing to obtain a suspension A; S2, uniformly mixing a silicon source and water, adding an acidic aqueous solution, uniformly mixing to obtain a silicic acid sol, adding the suspension A obtained in the S1 to the silicic acid sol, uniformly mixing, adjusting the pH value to 5-6, adding a drying control chemical additive, stirring, heating, carrying out thermal insulation, and crushing to obtain a sol B; and S3, taking the sol B obtained in the S2, carrying out solvent exchange, modifying with a silane coupling agent, and drying to obtain the halogen-free synergistic flame-retardant silica aerogel. According to the present invention, the halogen-free synergistic flame-retardant silica aerogel has advantages of good flame-retardant property, low combustion heat value, low density, good hydrophobicity, large specific surface area, simple operation, and low production cost.

Description

technical field [0001] The invention relates to the technical field of silica airgel, in particular to a preparation method of a halogen-free synergistic flame-retardant silica airgel. Background technique [0002] Silica airgel is a new type of thermal insulation material with nanoporous and three-dimensional network skeleton structure, and has the advantages of small density, small pore size, high porosity, large specific surface area, and low thermal conductivity. Strong adsorption, anti-oxidation, corrosion resistance and many other advantages. Among them, the low thermal conductivity is the most notable feature of silica airgel. A large number of nanopores inside the silica airgel limit the collision between gas molecules, so that the gas molecules are approximately adsorbed on the walls of the nanopores, thereby reducing the gas-phase heat conduction and convective heat transfer inside the aerogel, making the silica The thermal conductivity of airgel is greatly reduc...

Claims

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Application Information

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IPC IPC(8): C09K21/00C09K21/04C09K21/10C01B33/16
CPCC09K21/00C01B33/16C09K21/04C09K21/10
Inventor 马丽艳刘忠程旭东龚伦伦
Owner ECONANO TECH LTD BEIJING
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