CN109180140B - Nano aerogel and preparation method thereof - Google Patents
Nano aerogel and preparation method thereof Download PDFInfo
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- CN109180140B CN109180140B CN201810901177.7A CN201810901177A CN109180140B CN 109180140 B CN109180140 B CN 109180140B CN 201810901177 A CN201810901177 A CN 201810901177A CN 109180140 B CN109180140 B CN 109180140B
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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
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00025—Aspects relating to the protection of the health, e.g. materials containing special additives to afford skin protection
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
Abstract
A nanometer aerogel and a preparation method thereof comprise the following components in parts by mass: nano silicon dioxide: 15-25 parts of titanium oxide: 40-55 parts of copper oxide: 10-15 parts of alumina: 20-30 parts. The nanometer aerogel obtained by the invention is used as a functional component, and the nanometer aerogel is rich in pore structure and gas is a poor heat conductor, so that the heat insulation performance of the nanometer aerogel in a use scene can be improved after the nanometer aerogel is added; after certain metal elements are compounded in the nano aerogel, the nano aerogel has a very good decomposition effect on formaldehyde due to large porosity and the catalytic action of metal ions.
Description
The technical field is as follows:
the invention relates to a nano aerogel and a preparation method thereof.
Background art:
aerogels are sometimes referred to as "solid smoke" or "frozen smoke" because of their translucent color and ultra-light weight. The new material seems fragile and durable and can bear the high temperature of 1400 ℃. These properties of aerogels have many uses in aerospace exploration. Aerogel materials have been used in Russian "peace" number space stations and in American "Mars pathfinder" detectors. Aerogels are now increasingly used. However, in the prior art, there is no deep research on how to remove formaldehyde by using aerogel and the requirements of aerogel components in the use scene.
The invention content is as follows:
the invention provides a nano aerogel and a preparation method thereof, which can obtain a product with low density, good heat insulation effect and formaldehyde purification effect, and solves the problems in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a nanometer aerogel comprises the following components in parts by weight: nano silicon dioxide: 15-25 parts of titanium oxide: 40-55 parts of copper oxide: 10-15 parts of alumina: 20-30 parts.
A preparation method of nano aerogel, wherein the nano aerogel is prepared by the following steps: mixing the following raw materials in parts by weight: 95-130.6 parts of copper chloride: 17-25.4 parts of aluminum chloride: 52.2-78.2 parts of ethyl orthosilicate: 52-86.7 parts of the aerogel, then putting the aerogel into 150-300 parts of alcohol solvent, adopting a solvothermal method, drying and roasting to obtain the nano aerogel.
Preferably, the temperature of the solvothermal method is 240-250 ℃, the pressure is 8-12Mpa, and the reaction time is 0.8-1.2 h.
Preferably, the titanium tetrachloride is an alcoholic solution with the mass fraction of 4-6%.
Preferably, the copper chloride is an alcoholic solution with the mass fraction of 1.5-2.5%.
Preferably, the aluminum chloride is an alcohol solution with the mass fraction of 2-4%.
Preferably, the ethyl orthosilicate is an alcoholic solution with the mass fraction of 1.6-2.4%.
Preferably, the alcohol solvent is n-butanol and/or ethanol and/or isopropanol.
Preferably, the tin chloride is also contained by 1 to 5 parts by mass.
Preferably, the stannic chloride is an alcoholic solution with the mass fraction of 4-6%.
The invention has the following advantages: the nano aerogel is used as a functional component, and the nano aerogel is rich in pore structure and gas is a poor heat conductor, so that the heat insulation performance of the nano aerogel in a use scene can be improved after the nano aerogel is added; after certain metal elements are compounded in the nano aerogel, the nano aerogel has a very good decomposition effect on formaldehyde due to large porosity and the catalytic action of metal ions.
The specific implementation mode is as follows:
in order to clearly illustrate the technical features of the present invention, the present invention is explained in detail by the following embodiments.
Nano aerogel synthesis example:
nano aerogel example 1:
s1, uniformly mixing and stirring the raw materials: mixing the following raw materials in parts by weight: 95g, copper chloride: 17g, aluminum chloride: 52.2g, ethyl orthosilicate: 52g of alcohol solvent of 150g is added; the titanium tetrachloride is an alcoholic solution with the mass fraction of 4%; the copper chloride is an alcoholic solution with the mass fraction of 1.5%; the aluminum chloride is an alcohol solution with the mass fraction of 2%; the ethyl orthosilicate is an alcoholic solution with the mass fraction of 1.6%; the alcohol solvent is n-butyl alcohol;
s2, solvothermal synthesis: the temperature is 240 ℃, the pressure is 8Mpa, and the reaction time is 1.2 h;
s3, drying and roasting: drying at 20-30 deg.C for 48h, maintaining at 70 deg.C for 48h in a vacuum drying oven, and calcining in a muffle furnace to obtain No. 1 nanometer aerogel.
Nano aerogel example 2:
s1, uniformly mixing and stirring the raw materials: mixing the following raw materials in parts by weight: 130.6g, copper chloride: 25.4g, aluminum chloride: 78.2g, ethyl orthosilicate: 86.7g of alcohol solvent is added into the mixture, and then 300g of alcohol solvent is added into the mixture; the titanium tetrachloride is an alcohol solution with the mass fraction of 6%; the copper chloride is an alcohol solution with the mass fraction of 2.5%; the aluminum chloride is an alcoholic solution with the mass fraction of 4%; the ethyl orthosilicate is an alcoholic solution with the mass fraction of 2.4%; the alcohol solvent is ethanol;
s2, solvothermal synthesis: the temperature is 240 ℃ and 250 ℃, the pressure is 8-12Mpa, and the reaction time is 0.8-1.2 h;
s3, drying and roasting: drying at 20-30 deg.C for 48h, maintaining at 70 deg.C for 48h in a vacuum drying oven, and calcining in a muffle furnace to obtain No. 2 nanometer aerogel.
Nano aerogel example 3:
s1, uniformly mixing and stirring the raw materials: mixing the following raw materials in parts by weight: 112.8g, copper chloride: 21.2g, aluminum chloride: 65.2g, ethyl orthosilicate: 69.4g, then 225g of alcohol solvent is added; the titanium tetrachloride is an alcohol solution with the mass fraction of 5%; the copper chloride is an alcohol solution with the mass fraction of 2%; the aluminum chloride is an alcoholic solution with the mass fraction of 3%; the ethyl orthosilicate is an alcoholic solution with the mass fraction of 2%; the alcohol solvent is isopropanol;
s2, solvothermal synthesis: the temperature is 245 ℃, the pressure is 10Mpa, and the reaction time is 1 h;
s3, drying and roasting: drying at 20-30 deg.C for 48h, maintaining at 70 deg.C for 48h in a vacuum drying oven, and calcining in a muffle furnace to obtain No. 3 nanometer aerogel.
Nano aerogel example 4:
s1, uniformly mixing and stirring the raw materials: mixing the following raw materials in parts by weight: 95g, copper chloride: 17g, aluminum chloride: 52.2g, ethyl orthosilicate: 52g, 1g of stannic chloride; then adding 150g of alcohol solvent; the titanium tetrachloride is an alcoholic solution with the mass fraction of 4%; the copper chloride is an alcoholic solution with the mass fraction of 1.5%; the aluminum chloride is an alcohol solution with the mass fraction of 2%; the ethyl orthosilicate is an alcoholic solution with the mass fraction of 1.6%; the stannic chloride is an alcoholic solution with the mass fraction of 5%; the alcohol solvent is n-butyl alcohol, and the mass fraction of ethanol is 1: 1, a mixed solvent;
s2, solvothermal synthesis: the temperature is 240 ℃, the pressure is 8Mpa, and the reaction time is 1.2 h;
s3, drying and roasting: drying at 20-30 deg.C for 48h, maintaining at 70 deg.C for 48h in a vacuum drying oven, and calcining in a muffle furnace to obtain No. 4 nanometer aerogel.
Nano aerogel example 5:
s1, uniformly mixing and stirring the raw materials: mixing the following raw materials in parts by weight: 130.6g, copper chloride: 25.4g, aluminum chloride: 78.2g, ethyl orthosilicate: 86.7g, 5g of stannic chloride; then 300g of alcohol solvent is added; the titanium tetrachloride is an alcohol solution with the mass fraction of 6%; the copper chloride is an alcohol solution with the mass fraction of 2.5%; the aluminum chloride is an alcoholic solution with the mass fraction of 4%; the ethyl orthosilicate is an alcoholic solution with the mass fraction of 2.4%; the stannic chloride is an alcoholic solution with the mass fraction of 5%; the alcohol solvent is ethanol, and the mass fraction of isopropanol is 1: 1, a mixed solvent;
s2, solvothermal synthesis: the temperature is 240 ℃ and 250 ℃, the pressure is 8-12Mpa, and the reaction time is 0.8-1.2 h;
s3, drying and roasting: drying at 20-30 deg.C for 48h, maintaining at 70 deg.C for 48h in a vacuum drying oven, and calcining in a muffle furnace to obtain No. 5 nanometer aerogel.
Nano aerogel example 6:
s1, uniformly mixing and stirring the raw materials: mixing the following raw materials in parts by weight: 112.8g, copper chloride: 21.2g, aluminum chloride: 65.2g, 3g of stannic chloride; ethyl orthosilicate: 69.4g, then 225g of alcohol solvent is added; the titanium tetrachloride is an alcohol solution with the mass fraction of 5%; the copper chloride is an alcohol solution with the mass fraction of 2%; the aluminum chloride is an alcoholic solution with the mass fraction of 3%; the ethyl orthosilicate is an alcoholic solution with the mass fraction of 2%; the stannic chloride is an alcoholic solution with the mass fraction of 5%; the alcohol solvent is n-butanol, ethanol and isopropanol, and the mass fraction of the alcohol solvent is 1: 1: 1, a mixed solvent;
s2, solvothermal synthesis: the temperature is 245 ℃, the pressure is 10Mpa, and the reaction time is 1 h;
s3, drying and roasting: drying at 20-30 deg.C for 48h, maintaining at 70 deg.C for 48h in a vacuum drying oven, and calcining in a muffle furnace to obtain No. 6 nanometer aerogel.
The properties of the 1-6 nanometer aerogel are characterized as follows:
| product(s) | Apparent density (g/cm)-3) | Porosity (%) |
| No. 1 nano aerogel | 0.17 | 92 |
| No. 2 nano aerogel | 0.19 | 89 |
| No. 3 nano aerogel | 0.19 | 88 |
| No. 4 nano aerogel | 0.15 | 95 |
| No. 5 nano aerogel | 0.16 | 94 |
| No. 6 nano aerogel | 0.16 | 94 |
Therefore, the stannic chloride has better effects on improving the porosity of the aerogel and improving the fluffy degree of the aerogel.
Characterization of the effect of formaldehyde treatment:
1g of the above aerogel was placed in each of square boxes having an inner size of 50cmx50cmx50cm, and then formaldehyde was sprayed so that the concentration of formaldehyde was 0.1g/m3Left and right, then after standing for 48 hours, the formaldehyde concentration was measured, and a blank set was set, and 1g of activated carbon was put in, and the results were as follows.
From the above, the treatment efficiency of the aerogel on formaldehyde is greatly improved by adopting the method; after the tin chloride is adopted, the formaldehyde treatment efficiency is greatly improved due to the increase of the pore structure.
Application test:
coating synthesis example:
coating example 1:
s1, mixing: mixing No. 2 nano aerogel: 5g, acrylic emulsion: 30g, melamine: 35g, pentaerythritol: 40g, ammonium polyphosphate: 50g, sepiolite fiber: 5g, talcum powder: 5g, expandable graphite: 5g, aqueous wetting dispersant: 0.2g, modified organobentonite: 0.02g of water-based leveling agent: 0.05g of the coating is added with a proper amount of water and mixed, and then the mixture is stirred uniformly to obtain the coating;
s2, brushing: coating the coating on the outer side of an I-shaped steel beam I36b standard to obtain a No. 1 sample, wherein the thickness of the coating is 4.5-5.5 mm;
and S3 and No. 1 samples detect related parameters according to the method of GB14907-2002 steel structure fireproof paint.
Coating example 2:
s1, mixing: mixing No. 2 nano aerogel: 20g, acrylic emulsion: 50g, melamine: 80g, pentaerythritol: 65g, ammonium polyphosphate: 80g, sepiolite fiber: 15g, talcum powder: 15g, expandable graphite: 15g, aqueous wetting dispersant: 0.8g, modified organobentonite: 0.08g of water-based leveling agent: 0.2g of the coating is added with a proper amount of water and mixed, and then the mixture is uniformly stirred to obtain the coating;
s2, brushing: coating the coating on the outer side of an I-shaped steel beam I36b standard to obtain a No. 2 sample, wherein the thickness of the coating is 4.5-5.5 mm;
and (4) detecting related parameters by using samples S3 and 2 according to a method of GB14907-2002 steel structure fireproof paint. Coating example 3:
s1, mixing: mixing No. 2 nano aerogel: 13g, acrylic emulsion: 40g, melamine: 58g, pentaerythritol: 53g, ammonium polyphosphate: 65g, sepiolite fiber: 10g, talcum powder: 10g, expandable graphite: 10g, aqueous wetting dispersant: 0.5g, modified organobentonite: 0.05g of water-based leveling agent: 0.13g of the coating is added with a proper amount of water and mixed, and then the mixture is uniformly stirred to obtain the coating;
s2, brushing: coating the coating on the outer side of an I-shaped steel beam I36b standard to obtain a No. 3 sample, wherein the thickness of the coating is 4.5-5.5 mm;
and (4) detecting related parameters by using samples S3 and 3 according to a method of GB14907-2002 steel structure fireproof paint.
Coating example 4:
s1, mixing: mixing No. 5 nano aerogel: 5g, acrylic emulsion: 30g, melamine: 35g, pentaerythritol: 40g, ammonium polyphosphate: 50g, sepiolite fiber: 5g, talcum powder: 5g, expandable graphite: 5g, aqueous wetting dispersant: 0.2g, modified organobentonite: 0.02g of water-based leveling agent: 0.05g of the coating is added with a proper amount of water and mixed, and then the mixture is stirred uniformly to obtain the coating;
s2, brushing: coating the paint on the outer side of an I-shaped steel beam with the thickness of 4.5-5.5 mm in the standard I-shaped steel beam I36b to obtain a No. 4 sample;
and (4) detecting related parameters by using samples S3 and 4 according to a method of GB14907-2002 steel structure fireproof paint.
Coating example 5:
s1, mixing: mixing No. 5 nano aerogel: 20g, acrylic emulsion: 50g, melamine: 80g, pentaerythritol: 65g, ammonium polyphosphate: 80g, sepiolite fiber: 15g, talcum powder: 15g, expandable graphite: 15g, aqueous wetting dispersant: 0.8g, modified organobentonite: 0.08g of water-based leveling agent: 0.2g of the coating is added with a proper amount of water and mixed, and then the mixture is uniformly stirred to obtain the coating;
s2, brushing: coating the paint on the outer side of an I-shaped steel beam with the thickness of 4.5-5.5 mm in the standard I-shaped steel beam I36b to obtain a No. 5 sample;
and (5) detecting related parameters by using samples S3 according to the method of GB14907-2002 steel structure fireproof paint. Coating example 6:
s1, mixing: mixing No. 5 nano aerogel: 13g, acrylic emulsion: 40g, melamine: 58g, pentaerythritol: 53g, ammonium polyphosphate: 65g, sepiolite fiber: 10g, talcum powder: 10g, expandable graphite: 10g, aqueous wetting dispersant: 0.5g, modified organobentonite: 0.05g of water-based leveling agent: 0.13g of the coating is added with a proper amount of water and mixed, and then the mixture is uniformly stirred to obtain the coating;
s2, brushing: coating the coating on the outer side of an I-shaped steel beam I36b standard to obtain a No. 6 sample, wherein the thickness of the coating is 4.5-5.5 mm;
and (4) detecting related parameters by using samples S3 and 6 according to a method of GB14907-2002 steel structure fireproof paint.
Coating example 7:
s1, mixing: mixing No. 5 nano aerogel: 20g, acrylic emulsion: 50g, melamine: 80g, pentaerythritol: 65g, ammonium polyphosphate: 80g, sepiolite fiber: 15g, talcum powder: 15g, ordinary graphite: 15g, aqueous wetting dispersant: 0.8g, modified organobentonite: 0.08g of water-based leveling agent: 0.2g of the coating is added with a proper amount of water and mixed, and then the mixture is uniformly stirred to obtain the coating;
s2, brushing: coating the paint on the outer side of an I-shaped steel beam with the thickness of 4.5-5.5 mm in the standard I-shaped steel beam I36b to obtain a No. 7 sample;
and (4) detecting related parameters by using samples S3 and 7 according to a method of GB14907-2002 steel structure fireproof paint.
Coating example 8:
s1, mixing: mixing No. 5 nano aerogel: 20g, acrylic emulsion: 50g, melamine: 80g, pentaerythritol: 65g, ammonium polyphosphate: 80g, sepiolite fiber: 15g, talcum powder: 15g, expandable graphite: 15g, aqueous wetting dispersant: 0.8g, sodium-based organobentonite: 0.08g of water-based leveling agent: 0.2g of the coating is added with a proper amount of water and mixed, and then the mixture is uniformly stirred to obtain the coating;
s2, brushing: coating the paint on the outer side of an I-shaped steel beam with the thickness of 4.5-5.5 mm in the standard I-shaped steel beam I36b to obtain a No. 8 sample;
and (4) detecting related parameters by using samples S3 and 8 according to a method of GB14907-2002 steel structure fireproof paint.
In addition, the paints obtained in paint examples 1 to 8 were applied to the inner wall of a cube box having an inner wall area of 50cmx50cmx50cm to a thickness of 2 to 3mm, and then formaldehyde was sprayed so that the formaldehyde concentration was about 0.1g/m3, and then left to stand for 48 hours, and the formaldehyde concentration was measured, and a blank set was set and a normal aqueous paint was applied, and the results were as follows.
From the above, the treatment efficiency of the coating for formaldehyde is greatly improved; after the tin chloride is adopted, the formaldehyde treatment efficiency is greatly improved due to the increase of the pore structure.
The above-described embodiments should not be construed as limiting the scope of the invention, and any alternative modifications or alterations to the embodiments of the present invention will be apparent to those skilled in the art.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (7)
1. A nano aerogel, characterized by: the paint comprises the following components in parts by mass: nano silicon dioxide: 15-25 parts of titanium oxide: 40-55 parts of copper oxide: 10-15 parts of alumina: 20-30 parts of a solvent; the nano aerogel is prepared by the following steps: mixing the following raw materials in parts by mass: 1-5 parts; titanium tetrachloride: 95-130.6 parts of copper chloride: 17-25.4 parts of aluminum chloride: 52.2-78.2 parts of ethyl orthosilicate: 52-86.7 parts of the aerogel, then putting the aerogel into 150-300 parts of alcohol solvent, and drying and roasting the aerogel to obtain the nano aerogel by adopting a solvothermal method; the stannic chloride is an alcoholic solution with the mass fraction of 4-6%.
2. A nanoaerogel as claimed in claim 1, characterized in that: the temperature of the solvothermal method is 240 ℃ and 250 ℃, the pressure is 8-12Mpa, and the reaction time is 0.8-1.2 h.
3. A nanoaerogel as claimed in claim 1, characterized in that: the titanium tetrachloride is an alcoholic solution with the mass fraction of 4-6%.
4. A nanoaerogel as claimed in claim 1, characterized in that: the copper chloride is an alcoholic solution with the mass fraction of 1.5-2.5%.
5. A nanoaerogel as claimed in claim 1, characterized in that: the aluminum chloride is an alcohol solution with the mass fraction of 2-4%.
6. A nanoaerogel as claimed in claim 1, characterized in that: the ethyl orthosilicate is an alcoholic solution with the mass fraction of 1.6-2.4%.
7. A nanoaerogel as claimed in claim 1, characterized in that: the alcohol solvent is n-butanol and/or ethanol and/or isopropanol.
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