CN111101819B - Preparation method of hydrophobic silica aerogel heat-insulation glass - Google Patents
Preparation method of hydrophobic silica aerogel heat-insulation glass Download PDFInfo
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- CN111101819B CN111101819B CN201911289308.1A CN201911289308A CN111101819B CN 111101819 B CN111101819 B CN 111101819B CN 201911289308 A CN201911289308 A CN 201911289308A CN 111101819 B CN111101819 B CN 111101819B
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- glass
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- aerogel
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- hydrophobic silica
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- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
- E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
- E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
- E06B3/66—Units comprising two or more parallel glass or like panes permanently secured together
- E06B3/67—Units comprising two or more parallel glass or like panes permanently secured together characterised by additional arrangements or devices for heat or sound insulation or for controlled passage of light
- E06B3/6715—Units comprising two or more parallel glass or like panes permanently secured together characterised by additional arrangements or devices for heat or sound insulation or for controlled passage of light specially adapted for increased thermal insulation or for controlled passage of light
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/155—Preparation of hydroorganogels or organogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
- E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
- E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
- E06B3/66—Units comprising two or more parallel glass or like panes permanently secured together
- E06B3/677—Evacuating or filling the gap between the panes ; Equilibration of inside and outside pressure; Preventing condensation in the gap between the panes; Cleaning the gap between the panes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/24—Structural elements or technologies for improving thermal insulation
- Y02A30/249—Glazing, e.g. vacuum glazing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
- Y02B80/22—Glazing, e.g. vaccum glazing
Abstract
The invention discloses a preparation method of hydrophobic silica aerogel heat insulation glass, the time for preparing silica aerogel by adopting the method is short, the prepared aerogel has certain hydrophobicity, the structure of the aerogel is not influenced by the adsorption of water in the air, so that the heat insulation performance of the aerogel is further influenced, and the service life of the material is prolonged. The aerogel powder bonding technology is adopted, the preparation process is simple, and the prepared hydrophobic silica aerogel composite glass has structural strength obviously superior to that of vacuum glass, and has good heat preservation and insulation performance, long service life and better light transmittance.
Description
The technical field is as follows:
the invention relates to the field of building energy conservation, heat preservation and heat insulation, in particular to a preparation method of hydrophobic silica aerogel heat insulation glass.
Background art:
at present, the proportion of building energy consumption to the total energy consumption of social commodities is about 27.4%. Along with the progress of society, the living standard of people is continuously improved, the requirements on the appearance and lighting of buildings are also improved, the glass doors, windows and curtain walls with larger areas are widely applied to the buildings, the proportion of building energy consumption is continuously increased, the building energy consumption at the present stage accounts for more than 30% of the total social energy consumption, and the energy dissipated through the lighting doors and windows accounts for more than half of the building energy consumption. The heat exchange is reduced by adopting the heat insulation glass on the building, and the building energy consumption can be effectively reduced.
The heat-insulating glass which is commonly used at present is mainly hollow glass, which is mainly formed by combining two or more pieces of glass, adding a certain amount of drying agent in the middle and sealing the edges. The novel heat insulation glass mainly comprises hollow glass combined by a plurality of pieces of low-e glass, and the surface of the glass is plated with a plurality of layers of metals or other compounds, so that the outdoor far infrared radiation can be effectively blocked, and the purpose of heat insulation is achieved. However, the film layer is extremely fragile, so that the low-e glass is difficult to process and produce and has higher cost. Another type of vacuum glass is made by vacuum sealing between two layers of glass, which has very low thermal conductivity. The vacuum glass has the defects that the service life is difficult to guarantee, the sealing strips on the side edges are aged and easy to age, so that vacuum leakage is caused, and the heat insulation performance of the glass is greatly reduced. The vacuum glass interlayer is under negative pressure, so that stress concentration is easy to occur, and the safety is difficult to ensure. In addition, the manufacturing process of the vacuum glass is complex, the production cost is high, and the market popularization is not facilitated. Therefore, aerogel glass which has the advantages of heat preservation and heat insulation and higher practical value becomes the key point of market demand.
Aerogel is an ideal heat-insulating material due to the extremely low density and extremely low thermal conductivity coefficient (the thermal conductivity is as low as 0.017W/(m.K) at normal temperature and normal pressure). The aerogel prepared by the adjustment process has good light transmittance. Therefore, the aerogel glass has wide application requirements in various occasions of heat preservation, heat insulation and the like. The existing silicon dioxide aerogel glass mainly uses a traditional acid-base two-step method to prepare gel, and has the disadvantages of long gel time, complex process and long preparation period. Meanwhile, the water absorption of the silicon dioxide aerogel easily causes that all performances of the silicon dioxide aerogel are obviously reduced, and the light transmittance and heat insulation performance are common.
The invention content is as follows:
the invention aims to provide hydrophobic silica aerogel heat-insulating glass and a preparation method thereof. Compared with the traditional vacuum glass, the hydrophobic silica aerogel heat-insulating glass has the heat conductivity lower than 0.02W/(m.K) and has the visible light transmittance higher than 80 percent. The aerogel prepared has hydrophobicity, so the whole structure has longer service life.
The technical scheme of the invention comprises the following steps:
(1) preparation of silica aerogel: a co-precursor method is adopted, and 5-10 parts of 3-Aminopropyltriethoxysilane (APTES), 5-1 part of methyltrimethoxysilane (MTMS), 5-1 part of tetramethoxysilane or tetraethoxysilane and 30-96 parts of water are respectively dissolved in 75-480 parts of Acetonitrile (ACN) solvent and fully stirred. And (3) putting the two solutions into a constant temperature box with the temperature of-10 ℃ for 90min, mixing in a mould with a proper size, and gelling the mixed solution within 10-60 min. Obtaining silica wet gel;
(2) and aging the silica wet gel at room temperature for 24 hours to enable the silica wet gel to fully react, and after the silica wet gel is washed by acetonitrile for 4 times, performing supercritical drying on the silica wet gel by carbon dioxide at the temperature of 40-60 ℃, the drying pressure of 7-10 MPa and the drying time of 2-6 hours to prepare the hydrophobic silica aerogel. The prepared silicon dioxide aerogel is crushed, and the crushed sample is sieved by a 10-20-mesh sieve to obtain aerogel particles with required particle sizes.
(3) Taking two pieces of flat glass, and immersing the two pieces of flat glass into an acetonitrile solution for cleaning for 0.5-1.0 h; taking out the glass, drying the glass in a drying oven at the temperature of 60 ℃ for 2-4 h, and taking out; coating a layer of photosensitive glue on one surface of the glass; covering a layer of hydrophobic silica aerogel particles on the glued glass, covering and blowing for many times, and ensuring that the aerogel particles cover the surface of the glass as completely as possible; placing another piece of glass coated with the photosensitive adhesive on the aerogel powder, applying certain pressure on the glass, and keeping a certain gap between the two pieces of glass;
(4) carrying out ultraviolet irradiation on the glass until the photosensitive adhesive is completely cured;
(5) adding aluminum strips of a drying agent around the gap of the double-layer glass, sealing by using a sealant, and reserving an air extraction opening; vacuumizing to 100pa, and sealing the air exhaust hole;
(6) and an outer frame with a protective function is additionally arranged on the side edge of the glass.
Different from the traditional acid-base two-step catalysis method for preparing SiO2 wet gel, the hydrolysis and polycondensation reaction in the experiment are synchronously carried out, and the hydrolysis time of the silicon source solution for several hours is saved. MTMS has methoxy with extremely high activity, can be quickly hydrolyzed without acid catalysis after being mixed with water, can prolong the reaction time at low temperature to ensure the stable structure of the formed gel skeleton, and forms orthosilicic acid (Si (OH)4) with four hydroxyl groups after being hydrolyzed. Besides three hydrolyzable ethoxy groups, APTES also contains a-NH 2 group which does not participate in hydrolysis and shows alkalinity, and can be used as a catalyst for silicic acid polycondensation instead of ammonia water. While the methyl group may provide hydrophobicity. The aging is carried out at room temperature because the concentration of the reactant is low and the reaction is sufficient.
Description of the drawings:
FIG. 1 is a flow chart of a silica aerogel preparation process of the present invention
FIG. 2 is a schematic view of the structure of the hydrophobic silica aerogel heat-insulating glass of the present invention
The implementation case is as follows:
example 1:
3-Aminopropyltriethoxysilane (APTES), methyltrimethoxysilane (MTMS) and n-silicon
And (3) ethyl acetate according to a molar ratio of 5: 5: and 5, respectively dissolving 110g of 3-aminopropyltriethoxysilane, 68g of methyltrimethoxysilane, 104g of tetraethoxysilane and 48g of water in 400ml of Acetonitrile (ACN) solvent, fully stirring, cooling for 90min in a constant temperature box at the temperature of-10 ℃, uniformly mixing, and gelling after 20 min. Obtaining silica wet gel;
and (3) aging the silica wet gel at the room temperature of 20 ℃ for 24h, washing the silica wet gel with acetonitrile for 4 times every 12h, and performing supercritical drying on the silica wet gel by carbon dioxide at the temperature of 40 ℃, the drying pressure of 8MPa and the drying time of 4h to obtain the hydrophobic silica aerogel. The prepared silicon dioxide aerogel is crushed, and the crushed sample is sieved by a 10-20-mesh sieve to obtain aerogel particles with required particle sizes.
Taking two pieces of flat glass, immersing the two pieces of flat glass into an acetonitrile solution, and cleaning for 1 h; taking out the glass, drying the glass in a drying oven at 60 ℃ for 4 hours, and taking out the glass; coating a layer of photosensitive glue on one surface of the glass; covering a layer of hydrophobic silica aerogel particles on the glued glass, covering and blowing for many times, and ensuring that the aerogel particles cover the surface of the glass as completely as possible; placing another piece of glass coated with the photosensitive adhesive on the aerogel powder, applying certain pressure on the glass, and keeping a certain gap between the two pieces of glass; carrying out ultraviolet irradiation on the glass until the photosensitive adhesive is completely cured; adding aluminum strips of a drying agent around the gap of the double-layer glass, sealing by using a sealant, and reserving an air extraction opening; vacuumizing to 100pa, and sealing the air exhaust hole; and an outer frame with a protective function is additionally arranged on the side edge of the glass.
The obtained aerogel glass has the light transmittance of 82 percent and the thermal conductivity of 0.018W/(m.K).
Example 2:
3-Aminopropyltriethoxysilane (APTES), methyltrimethoxysilane (MTMS) and ethyl orthosilicate in a molar ratio of 5: 1: 1, dissolving 110g of 3-aminopropyltriethoxysilane, 13.6g of methyltrimethoxysilane, 20.5g of ethyl orthosilicate and 54g of water in 400ml of Acetonitrile (ACN) solvent respectively, fully stirring, cooling in a constant temperature oven of-10 ℃ for 90min, mixing uniformly, and gelling after 10 min. Obtaining silica wet gel;
and (3) aging the silica wet gel at the room temperature of 25 ℃ for 24h, washing the silica wet gel with acetonitrile for 4 times every 12h, and performing supercritical drying on the silica wet gel by carbon dioxide at the temperature of 60 ℃, the drying pressure of 10MPa and the drying time of 2h to obtain the hydrophobic silica aerogel. The prepared silicon dioxide aerogel is crushed, and the crushed sample is sieved by a 10-20-mesh sieve to obtain aerogel particles with required particle sizes.
Taking two pieces of flat glass, immersing the two pieces of flat glass into an acetonitrile solution, and cleaning for 0.5 h; taking out the glass, drying the glass in a drying oven at 60 ℃ for 2 hours, and taking out the glass; coating a layer of photosensitive glue on one surface of the glass; covering a layer of hydrophobic silica aerogel particles on the glued glass, covering and blowing for many times, and ensuring that the aerogel particles cover the surface of the glass as completely as possible; placing another piece of glass coated with the photosensitive adhesive on the aerogel powder, applying certain pressure on the glass, and keeping a certain gap between the two pieces of glass; carrying out ultraviolet irradiation on the glass until the photosensitive adhesive is completely cured; adding aluminum strips of a drying agent around the gap of the double-layer glass, sealing by using a sealant, and reserving an air extraction opening; vacuumizing to 100pa, and sealing the air exhaust hole; and an outer frame with a protective function is additionally arranged on the side edge of the glass.
The obtained aerogel glass has the light transmittance of 80 percent and the thermal conductivity of 0.02W/(m.K).
Claims (8)
1. The preparation method of the hydrophobic silica aerogel heat-insulating glass is characterized by comprising the following steps of:
(1) preparation of silica aerogel: respectively dissolving a mixed silicon source and water in two solvents by adopting a co-precursor method, fully stirring and cooling the two solvents, uniformly mixing the two solvents, transferring the mixed solution into a mould with a proper size, sealing the mould, and placing the mould in a thermostat with the temperature of between-5 and-10 ℃ for 10 to 60min for gelling to obtain silicon dioxide wet gel;
(2) after aging and washing the silica wet gel for several times, preparing hydrophobic silica aerogel by a supercritical drying method, crushing the prepared silica aerogel, and sieving the crushed sample by a 10-20-mesh sieve to obtain aerogel particles with the required particle size;
(3) taking two pieces of flat glass, and immersing the two pieces of flat glass into an acetonitrile solution for cleaning for 0.5-1.0 h; taking out the glass, placing the glass in a drying oven at 60 ℃ for drying for 2-4 h, and taking out; coating a layer of photosensitive glue on one surface of the glass; covering a layer of hydrophobic silica aerogel particles on the glued glass, covering and blowing for many times, and ensuring that the aerogel particles cover the surface of the glass as completely as possible; placing another piece of glass coated with the photosensitive adhesive on the aerogel powder, applying certain pressure on the glass, and keeping a certain gap between the two pieces of glass;
(4) carrying out ultraviolet irradiation on the glass until the photosensitive adhesive is completely cured;
(5) adding aluminum strips of a drying agent around the gap of the double-layer glass, sealing by using a sealant, and reserving an air extraction opening; vacuumizing to 100pa, and sealing the air exhaust hole;
(6) an outer frame with a protective function is additionally arranged on the side edge of the glass;
the silicon source is one or a mixture of 3-Aminopropyltriethoxysilane (APTES), methyltrimethoxysilane (MTMS), Tetramethoxysilane (TMOS) and Tetraethoxysilane (TEOS);
the supercritical drying method comprises the steps of putting a sample to be dried into drying equipment, introducing nitrogen, pre-pressurizing to 2-7 MPa, setting the heating temperature to be 250-300 ℃, the heating rate to be 60-150 ℃/h, the drying pressure to be 8-12 MPa, drying for 2-6 h, releasing pressure after drying is finished, and purging with nitrogen.
2. The preparation method of the hydrophobic silica aerogel heat insulation glass according to claim 1, characterized in that the molar ratio of aerogel raw material 3-Aminopropyltriethoxysilane (APTES), methyltrimethoxysilane (MTMS) and other silicon source is (5-10): (5-1): (5-1), wherein the molar ratio of the total silicon source to the solvent and the water is 1: (5-40): (2-8).
3. The method of claim 1, wherein the solvent used to prepare the sol is one or more of Acetonitrile (ACN), ethanol (EtOH), and methanol (MeOH).
4. The method for preparing the hydrophobic silica aerogel heat insulation glass according to claim 1, wherein the silica wet gel is prepared in one step by adopting a co-precursor method.
5. The method for preparing the hydrophobic silica aerogel heat insulation glass according to the claim 1, wherein the gel temperature is in a thermostat with the temperature of-5 to-10 ℃.
6. The preparation method of the hydrophobic silica aerogel heat-insulation glass according to claim 1, wherein the supercritical carbon dioxide drying method is that a sample to be dried is placed into a drying device, the drying pressure is 7-10 MPa at 40-60 ℃, and the drying time is 2-6 h.
7. A process according to claim 1The preparation method of the hydrophobic silica aerogel heat-insulation glass is characterized in that the prepared aerogel has hydrophobicity and the density is 0.08-0.12 g/m3The specific surface area exceeds 800m2/g。
8. The method for preparing hydrophobic silica aerogel heat insulation glass according to claim 1, wherein the glass is one of ordinary toughened glass, low-e glass, toughened glass and polycarbonate glass, the thickness of the glass is 3-10 mm, the gap between the two pieces of glass is 1-3 mm, the sealant is one of silicone sealant, polysulfide sealant, butyl sealant and polyurethane sealant, the outer frame body is of an aluminum alloy structure, and the part in contact with the glass is provided with adhesive strips.
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| CN201911289308.1A CN111101819B (en) | 2019-12-11 | 2019-12-11 | Preparation method of hydrophobic silica aerogel heat-insulation glass |
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| CN114180581B (en) * | 2021-11-29 | 2023-04-14 | 江西晨光新材料股份有限公司 | Synthetic method of silicon dioxide aerogel |
| CN114933307B (en) * | 2022-05-25 | 2024-02-20 | 厦门大学 | Preparation method of super-hydrophobic silica aerogel powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102606040A (en) * | 2012-04-11 | 2012-07-25 | 上海耀皮玻璃集团股份有限公司 | Hollow glass with aerogel |
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| DE2524461A1 (en) * | 1974-06-05 | 1975-12-18 | Optical Coating Laboratory Inc | MULTI-LAYER COVERING FOR BUILDING PURPOSES AND PROCESS FOR MANUFACTURING SUCH A COVERAGE |
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