CN111517747A - Preparation method of pre-oxidized fiber felt-silica aerogel heat-insulation composite material - Google Patents
Preparation method of pre-oxidized fiber felt-silica aerogel heat-insulation composite material Download PDFInfo
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- CN111517747A CN111517747A CN202010315784.2A CN202010315784A CN111517747A CN 111517747 A CN111517747 A CN 111517747A CN 202010315784 A CN202010315784 A CN 202010315784A CN 111517747 A CN111517747 A CN 111517747A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Silicon Compounds (AREA)
- Thermal Insulation (AREA)
Abstract
The invention belongs to the technical field of aerogel, and particularly relates to a preparation method of a pre-oxidized fiber felt-silicon aerogel heat insulation composite material. A preparation method of a pre-oxidized fiber felt-silica aerogel heat insulation composite material comprises the following steps: preparing the composite material of water glass-acid solution, pre-oxidized silk felt-water glass-acid solution and drying the wet gel composite material. The invention uses the low-cost water glass and the pre-oxidized fiber felt for compounding to obtain the heat-insulating composite material with excellent heat-insulating property.
Description
Technical Field
The invention belongs to the technical field of aerogel, and particularly relates to a preparation method of a pre-oxidized fiber felt-silicon aerogel heat insulation composite material.
Background
Aerogel is a solid substance with the lowest density in the world, and the density can be as low as 3kg/m3The common aerogel was a silica aerogel, which was first produced by american scientists in 1931. The silica aerogel is a low-density high-porosity nano-porous amorphous solid material, has high light transmittance, is also called as 'blue smoke', is filled with gaseous dispersion media in cavities, has a continuous nano-scale three-dimensional network structure, and is a currently known solid material with the lowest density and the lowest heat conductivity coefficient in the world. The size of the cavity and the network skeleton are both nano-scale, and the composite material has unique properties in various aspects such as mechanics, acoustics, thermology, optics and the like, and has wide application prospects in the fields of aerospace, war industry, petrochemicals, minerals, electronics, automobiles and the like.
The good characteristics of high porosity, low thermal conductivity and low dielectric constant make the aerogel widely used in more fields. However, the silica aerogel has large brittleness due to the characteristics of the inorganic nano-skeleton structure, and has poor bending resistance and friction resistance, so that the industrial application is difficult to realize. At present, many manufacturers take fiber felts as a matrix, and prepare the heat insulation composite material by compounding the silicon dioxide aerogel, so that the strength of the heat insulation composite material is obviously improved. Because the water glass has low cost and is easy to obtain, the silicon dioxide aerogel takes the water glass as a source at present, has the characteristics of low cost, easy operation and high efficiency, and is favored by more and more manufacturers. The pre-oxidized fiber felt has good heat resistance and flame retardance, and can be used as a heat insulation material of a new energy battery
Chinese patent CN201811554746 develops a pre-oxidized fiber aerogel felt which is prepared by taking an organic silicon source as a precursor, and the preparation cost is higher.
The invention develops a new method for preparing the heat-insulating composite material by compounding the pre-oxidized fiber mat and the water glass solution, which is simple and easy to implement, has lower cost and is easy for industrial production.
Disclosure of Invention
A preparation method of a pre-oxidized fiber felt-silica aerogel heat insulation composite material comprises the following steps:
(1) preparing a water glass-acid solution: deionized water, a surfactant and a defoaming agent are mixed according to the proportion of 100: preparing 0.1-10:0.01-1 to obtain a solution 1, and preparing a water glass solution and deionized water according to the proportion of 1:2-10 to obtain a solution 2; preparing an acid solution and deionized water according to the proportion of 0.05-0.20:1 to obtain a solution 3; adding the solution 1 and the solution 2 into the solution 3 to prepare a water glass-acid solution;
(2) compounding pre-oxidized silk felt, water glass and acid solution: soaking the pre-oxidized fiber felt into the prepared water glass-acid solution for 30-120 seconds, and putting the water glass-acid solution soaked with the pre-oxidized fiber felt into a vacuum kettle; vacuumizing the vacuum kettle, heating the vacuum kettle to 50-60 ℃, keeping the vacuum for 30-40min to enable the pre-oxidized fiber mat and the water glass-acid solution to have a gel reaction, and taking out the wet gel composite material after the vacuum heating is finished;
(3) drying the wet gel composite: and carrying out supercritical drying or normal-pressure drying on the compounded wet gel composite material to obtain the heat-insulating composite material.
The surfactant comprises at least one of an anionic surfactant and a nonionic surfactant.
The surfactant in the step (1) is at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, ammonium dodecyl sulfate, sodium polyoxyethylene lauryl ether sulfate, sodium stearate, propylene glycol fatty acid ester and polyethylene glycol fatty acid ester.
The concentration of the surfactant in the water glass-acid solution in the step (1) is 0.1-10%.
The concentration of the defoaming agent in the water glass-acid solution in the step (1) is 0.01-1.0%.
The medium used in the supercritical equipment in the step (3) adopts one of carbon dioxide, methanol and ethanol.
The drying temperature under normal pressure in the step (3) is 60-150 ℃.
In the invention, the pre-oxidized fiber mat is a fiber obtained by high-temperature thermal stabilization treatment of polyacrylonitrile fiber, and the fiber can achieve good heat insulation and flame retardant effects after being compounded with silica aerogel. The surface has many carbon atom groups because of the high temperature carbonization treatment back of preoxidized fiber fibre, can hinder the hydrone to get into, through to preoxidized fiber fibrofelt evacuation processing, along with the taking away of gas molecule, the hydrone occupies the space that leaves after gas molecule takes away very easily, along with the entering of hydrone and the formation of wet gel, water glass solution can be fine with preoxidized fiber felt complex to can obtain the combined material of lower coefficient of heat conductivity after subsequent processing.
The invention uses the low-cost water glass and the pre-oxidized fiber felt for compounding to obtain the heat-insulating composite material with excellent heat-insulating property.
Detailed Description
In order to further introduce the technical scheme of the invention, the following embodiments are further described.
Example 1
Preparing deionized water, sodium dodecyl sulfate and a defoaming agent into a mixed solution 1 according to the proportion of 100:0.5:0.2, and standing for 30 min; the sodium water glass solution and water were mixed at a ratio of 1:3 to prepare solution 2. Solution 1, solution 2 and 10% sulfuric acid solution were mixed as 10: 50: 10 to obtain a mixed solution. Putting the pre-oxidized fiber felt into the mixed solution for soaking for 30s, putting the mixed solution in which the pre-oxidized fiber felt is soaked into a vacuum kettle, vacuumizing until the vacuum degree is close to vacuum, simultaneously heating the vacuum kettle to 50 ℃, keeping the vacuum for 30 minutes, and allowing the pre-oxidized fiber felt and the water glass-acid solution to perform gel reaction; and after 30 minutes, recovering the normal pressure of the vacuum kettle, taking out the reacted wet gel composite material, performing supercritical drying on the composite material in an environment of 60-150 ℃, and removing the ethanol solvent to obtain the aerogel heat insulation composite material. The thermal conductivity coefficient measured at 25 ℃ is 0.016-0.019W/m.k.
Examples 2 to 10
The procedure was as in example 1 except that the proportions of deionized water, sodium dodecylsulfate and defoaming agent were varied:
examples 11 to 13
The same as example 1 except that the ratio of the sodium water glass solution to water was different;
| ratio of sodium water glass solution to Water | Coefficient of thermal conductivity (W/m.k) |
| 1：5 | 0.0180 |
| 1：7 | 0.0188 |
| 1:10 | 0.0189 |
Examples 14 to 16
Except that the acid solution concentration was different from that of example 1, the rest was the same as example 1:
| acid solution concentration (%) | Coefficient of thermal conductivity (W/m.k) |
| 5 | 0.0175 |
| 15 | 0.0173 |
| 20 | 0.0169 |
Examples 17 to 19
The same procedure as in example 1 was repeated except that the pre-oxidized fiber mat was immersed in the mixed solution for a different period of time:
examples 20 to 21
The same procedure as in example 1 was repeated except that the temperature of the vacuum vessel was changed:
| temperature (. degree.C.) | Coefficient of thermal conductivity (W/m.k) |
| 55 | 0.0173 |
| 60 | 0.0175 |
Examples 22 to 23
The same as example 1 except that the mixing ratio of solution 1, solution 2 and solution 3 was different from that of example 1.
The above-mentioned embodiments are only used for explaining the inventive concept of the present invention, and do not limit the protection of the claims of the present invention, and any insubstantial modifications of the present invention using this concept shall fall within the protection scope of the present invention.
Claims (6)
1. A preparation method of a pre-oxidized fiber felt-silica aerogel heat insulation composite material is characterized by comprising the following steps:
(1) preparing a water glass-acid solution: deionized water, a surfactant and a defoaming agent are mixed according to the proportion of 100: preparing 0.1-10:0.01-1 to obtain a solution 1, and preparing a water glass solution and deionized water according to the proportion of 1:2-10 to obtain a solution 2; preparing a concentrated acid solution and deionized water according to the proportion of 0.05-0.20:1 to obtain a solution 3; adding the solution 1 and the solution 2 into the solution 3 to prepare a water glass-acid solution;
(2) compounding pre-oxidized silk felt, water glass and acid solution: soaking the pre-oxidized fiber felt into the prepared water glass-acid solution for 30-120 seconds, and putting the water glass-acid solution soaked with the pre-oxidized fiber felt into a vacuum kettle; vacuumizing the vacuum kettle, heating the vacuum kettle to 50-60 ℃, keeping the vacuum for 30-40min to enable the pre-oxidized fiber mat and the water glass-acid solution to have a gel reaction, and taking out the wet gel composite material after the vacuum heating is finished;
(3) drying the wet gel composite: and (3) drying the compounded wet gel composite material at a supercritical or normal temperature to obtain the heat insulation composite material.
2. The method for preparing a pre-oxidized fiber mat-silica aerogel thermal insulation composite material according to claim 1, wherein the method comprises the following steps: the surfactant comprises at least one of an anionic surfactant and a nonionic surfactant.
3. The method for preparing a pre-oxidized fiber mat-silica aerogel thermal insulation composite material according to claim 1, wherein the method comprises the following steps: the surfactant in the step (1) is at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, ammonium dodecyl sulfate, sodium polyoxyethylene lauryl ether sulfate, sodium stearate, propylene glycol fatty acid ester and polyethylene glycol fatty acid ester.
4. The method for preparing a pre-oxidized fiber mat-silica aerogel thermal insulation composite material according to claim 1, wherein the method comprises the following steps: the concentration of the surfactant in the water glass-acid solution in the step (1) is 0.001-1%.
5. The method for preparing a pre-oxidized fiber mat-silica aerogel thermal insulation composite material according to claim 1, wherein the method comprises the following steps: the concentration of the defoaming agent in the water glass-acid solution in the step (1) is 0.0001-0.5%.
6. The method for preparing a pre-oxidized fiber mat-silica aerogel thermal insulation composite material according to claim 1, wherein the method comprises the following steps: the medium used in the supercritical equipment in the step (3) adopts one of carbon dioxide, methanol and ethanol, and the normal-temperature drying temperature is 60-150 ℃.
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| CN202010315784.2A CN111517747A (en) | 2020-04-21 | 2020-04-21 | Preparation method of pre-oxidized fiber felt-silica aerogel heat-insulation composite material |
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