CN113003947A - Preparation method of silicon-based aerogel-foam material heat insulation composite material - Google Patents
Preparation method of silicon-based aerogel-foam material heat insulation composite material Download PDFInfo
- Publication number
- CN113003947A CN113003947A CN202110315242.XA CN202110315242A CN113003947A CN 113003947 A CN113003947 A CN 113003947A CN 202110315242 A CN202110315242 A CN 202110315242A CN 113003947 A CN113003947 A CN 113003947A
- Authority
- CN
- China
- Prior art keywords
- drying
- preparation
- composite material
- sio
- foaming material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000009413 insulation Methods 0.000 title claims abstract description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 25
- 239000010703 silicon Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000006261 foam material Substances 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 51
- 238000005187 foaming Methods 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005470 impregnation Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000000377 silicon dioxide Substances 0.000 claims description 24
- 239000000919 ceramic Substances 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 229910052681 coesite Inorganic materials 0.000 claims description 19
- 229910052906 cristobalite Inorganic materials 0.000 claims description 19
- 229910052682 stishovite Inorganic materials 0.000 claims description 19
- 229910052905 tridymite Inorganic materials 0.000 claims description 19
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- 239000011240 wet gel Substances 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 238000000352 supercritical drying Methods 0.000 claims description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 239000003377 acid catalyst Substances 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000012774 insulation material Substances 0.000 abstract description 5
- 230000006835 compression Effects 0.000 abstract description 3
- 238000007906 compression Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000009422 external insulation Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 13
- 230000001681 protective effect Effects 0.000 description 8
- 239000011494 foam glass Substances 0.000 description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 7
- 239000004964 aerogel Substances 0.000 description 6
- 238000005034 decoration Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000004795 extruded polystyrene foam Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920006327 polystyrene foam Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0095—Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5035—Silica
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a preparation method of a silicon-based aerogel-foam material heat-insulation composite material. The prepared material has a three-dimensional nano porous network structure, compared with the traditional external wall external insulation material and a pure foaming material, the composite material solves the problems of poor fire resistance grade and poor oxidation resistance of the traditional thermal insulation material, and reduces the thermal conductivity of the foaming material. And the density of the material is 0.139-0.160g/cm3The compression strength is 0.3-0.6MPa, the tear strength is 4.3-4.6MPa, the thermal conductivity is 0.042-0.051W/(m.K), and the water absorption is 3-6%. The preparation method is that the acid-base two-step method is combined with a high-pressure impregnation method and a vacuum impregnation method, and finally drying treatment is carried out. The preparation method has the advantages of simple process, short reaction period, realization of recycling, environmental protection and mass production prospect.
Description
Technical Field
The invention belongs to the field of preparation processes of nano porous materials, and relates to a preparation method of a silicon-based aerogel composite foam material.
Background
The traditional external thermal insulation system for the external wall has the defects of complex thermal bridge process treatment, cracking, hollowing, dropping, troublesome operation of an external decorative surface layer after the thermal insulation layer is constructed and the like, so that the performance, the constructability and the decoration of the external thermal insulation system are limited. Aiming at the construction of an external thermal insulation and decoration integrated system and the years of research and investigation of professional teams, a thermal insulation and decoration integrated plate and an integrated construction method are explored.
The foaming material is an inorganic heat-insulating material, and has the advantages of fire resistance, flame retardance, small deformation coefficient, ageing resistance, stable performance, ecological environmental protection, life-span equal to that of a building and the like. More importantly, the fireproof grade of the material is A1 grade, the fatal defects that organic materials are afraid of naked fire and are easy to age are overcome, the domestic blank of inorganic heat-insulating materials of buildings is filled, and the material has obvious advantages in an integrated system for heat insulation and decoration outside an outer wall. SiO 22The aerogel is a novel amorphous solid material with a controllable structure, the porosity can reach 80-98%, and the minimum material density is only 3.55kg/m3And has the characteristics of low density, high porosity, low thermal conductivity and low refractive index. Compared with traditional heat-insulating materials such as rock wool boards, glass wool, polystyrene foam (EPS) boards, extruded polystyrene foam plastic (XPS) boards and the like, the material is SiO2The aerogel shows more excellent effect in the field of heat insulation.
A fiber reinforced foam glass ceramic composite thermal insulation material is prepared by everyone in Zhejiang university college of materials science and engineering, and the bulk density of the material is 174-207 kg/m3The compression strength is 0.39-0.45 MPa, and the thermal conductivity is 0.061W/(m.K). In general, the material basically meets the requirements of external wall external insulation in the building industry at present, but the wall has large load due to high density and high heat conductivity coefficientAnd the potential safety hazards such as easy peeling off, so that the foaming material is adopted as the base material, and the foaming material and the silicon-based aerogel are compounded to prepare the environment-friendly low-heat-conductivity heat-insulation board for external heat insulation of the external wall, and the heat-insulation board aims to solve the problems found at present and obtain a larger application prospect in the fields of external heat insulation of the external wall, high-temperature heat insulation and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a silicon-based aerogel-foam material heat insulation composite material.
The technical scheme of the invention is as follows: the method comprises the steps of preparing silica sol by an acid-base two-step method and a sol-gel method by taking a pretreated foaming material as a base material, compounding the base material and the silica sol by a high-pressure impregnation method and a vacuum impregnation method, and finally obtaining the environment-friendly low-thermal-conductivity silica-based aerogel-foaming material heat-insulation composite material by an ethanol supercritical drying technology. The density of the prepared silica-based aerogel-foam material heat insulation composite material is 0.139-0.160g/cm3The compression strength is 0.3-0.6MPa, the tear strength is 4.3-4.6MPa, the thermal conductivity is 0.042-0.051W/(m.K), and the water absorption is 3-6%.
The specific technical scheme of the invention is as follows: a preparation method of a silicon-based aerogel-foam material heat insulation composite material comprises the following specific steps:
(1) pretreatment of foamed materials
And completely immersing the foaming material in a container filled with the solvent, and putting the container and the foaming material into the high-pressure reaction kettle together to ensure the sealing property of the high-pressure reaction kettle. Pressurizing by gas, applying certain pressure, maintaining the pressure for certain time to change a closed pore structure into an open pore structure, opening the high-pressure reaction kettle after exhausting, and then putting the pretreated foaming material into a blast drying oven for drying to obtain the pretreated foaming material;
(2)SiO2preparation of the Sol
Pouring a silicon source reagent into a container, adding an organic solvent, deionized water, a drying control chemical additive and an acid catalyst, stirring and reacting in a water bath at a certain temperature, dropwise adding an alkaline catalyst to adjust the pH, and continuously stirring to form SiO2Sol;
(3) preparation of composite materials
Mixing SiO2Pouring the sol into a container containing pretreated foaming material, putting the container into a vacuum reactor, vacuum-dipping the sol, taking out the sol, and standing the sol to obtain the SiO taking the foaming material as a base material2A wet gel composite;
(4) drying of composite materials
SiO taking the foaming material prepared in the step (3) as a base material2And (3) continuously standing the wet gel composite material for a certain time, and then performing supercritical drying on the wet gel composite material by using ethanol to obtain the silicon-based aerogel-foam material heat-insulation composite material.
Preferably, the foaming material in the step (1) is foaming glass or foaming ceramic; the solvent is one or a mixture of more of methanol, ethanol, deionized water or acetonitrile; the high-pressure reaction kettle is an ethanol supercritical reaction kettle or a carbon dioxide supercritical reaction kettle.
Preferably, the gas pressurization in the step (1) is nitrogen, argon or carbon dioxide pressurization; the applied pressure is 2-6MPa, and the pressure maintaining time is 5-15 min; the drying temperature of the air-blast drying box is 65-80 ℃, and the drying time is 2-3 h.
Preferably, the silicon source reagent in the step (2) is tetraethyl orthosilicate; the organic solvent is one of methanol, ethanol or acetonitrile; the drying control chemical additive is one of formamide, acetamide, N-dimethylformamide or N, N-dimethylacetamide.
Preferably, the molar ratio of the silicon source reagent, the organic solvent, the deionized water and the drying control chemical additive in the step (2) is 1 (30.2-40): (2.3-3): 1.3-1.5.
Preferably, the acidic catalyst in the step (2) is one of nitric acid, hydrochloric acid, acetic acid or propionic acid; the molar ratio of the added amount of the acidic catalyst to the silicon source is (0.003-0.005): 1.
Preferably, the temperature of the water bath stirring reaction in the step (2) is 50-60 ℃, and the reaction time is 40-60 min.
Preferably, the alkaline catalyst in the step (2) is one of ammonia water, ethylenediamine, triethanolamine or sodium hydroxide, and the pH value is adjusted to 7-8; stirring for 10-15 min.
Preferably, the sol in the step (3) is directly poured into a mould containing the pretreated foaming material, and the liquid level of the sol exceeds the height of the foaming material.
Preferably, the vacuum impregnation in the step (3) is carried out for 2-3 times at intervals of 5-10 min.
Preferably, the standing time in the step (4) is 5 to 8 hours.
Has the advantages that:
(1) compared with the traditional external wall external thermal insulation material and a pure foaming material, the silicon-based aerogel-foaming material thermal insulation composite material prepared by the invention solves the problems of poor fire resistance grade and poor oxidation resistance of the traditional thermal insulation material, and reduces the thermal conductivity of the foaming material.
(2) Compared with the traditional preparation process of the aerogel composite material, the preparation method can prepare the silicon-based aerogel-foam material heat-insulation composite material in a short time, and the produced sample has good stability, and is expected to realize industrialization in industry.
(3) The silicon-based aerogel-foam material heat insulation composite material prepared by the invention has strong oxidation resistance and chemical corrosion resistance, can be recycled, and is environment-friendly.
Drawings
FIG. 1 is SiO as prepared in example 12Pore size distribution of the aerogel;
FIG. 2 is a macroscopic sample of the silica-based aerogel-foam insulation composite prepared in example 1;
FIG. 3 is a graph of the compressive strength of the silica-based aerogel-foam insulation composite prepared in example 1.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of protection.
Example 1
A certain volume of ethanol is measured and taken as a protective solvent to be put into a container, and the foamed ceramic is completely immersed into the container filled with the protective solvent and put into an ethanol supercritical high-pressure reaction kettle to ensure the air tightness of the ethanol supercritical high-pressure reaction kettle. Pressurizing by introducing nitrogen gas, applying 2MPa of pressure, maintaining the pressure for 7min to change a closed pore structure into an open pore structure, opening the ethanol supercritical high-pressure reaction kettle after exhausting, and then drying the pretreated foamed ceramic in a blast drying oven at 65 ℃ for 3 hours for later use.
Heating and continuously stirring a mixed solution which takes 0.3mol of tetraethyl orthosilicate, 11.7mol of ethanol, 0.85mol of deionized water, 0.4mol of N, N-dimethylformamide and 1ml of acetic acid (1mol/L) as an acid catalyst under the condition of water bath at 50 ℃, adding ammonia water after 40min to adjust the pH value to 7, and continuously stirring for 10min to obtain SiO2Sol; to obtain SiO2Directly pouring the sol into a container containing pretreated foamed ceramics to make SiO2The sol is submerged in the foamed ceramic. Then vacuum-soaking in a vacuum reactor for 5min for 3 times, taking out the vacuum-soaked container filled with silica sol and foamed ceramic from the vacuum reactor, and standing to obtain SiO based on foamed ceramic2A wet gel composite. The obtained SiO taking the foamed ceramic as a base material2And continuously standing the wet gel composite material for 5 hours, and immediately performing ethanol supercritical drying to obtain the silicon-based aerogel-foamed ceramic heat-insulation composite material. The density of the composite material is 0.14g/cm3The thermal conductivity is 0.042W/(m.K), the compressive strength is 0.46MPa, the tear strength is 4.37MPa, and the water absorption rate is 3 percent. The pore size distribution, macroscopic sample and compressive strength of the prepared silica-based aerogel-foamed ceramic heat-insulating composite material are respectively shown in fig. 1, fig. 2 and fig. 3. Fig. 1 shows that the composite has a nanoporous structure, which provides an important structural feature for improving thermal insulation performance; FIG. 2 shows that the pores of the foamed ceramic have been completely dilutedThe blue silica aerogel is filled and covered, which shows that the silica sol can be fully absorbed into the matrix by the vacuum impregnation method, and shows that the composite material is successfully prepared; fig. 3 illustrates that the composite material has better mechanical properties.
Example 2
A certain volume of acetonitrile is measured and taken as a protective solvent to be put into a container, and the foamed glass is completely immersed into the container filled with the protective solvent and is put into an ethanol supercritical high-pressure reaction kettle, so that the air tightness of the ethanol supercritical high-pressure reaction kettle is ensured. Pressurizing by introducing nitrogen gas, applying pressure of 4MPa, maintaining the pressure for 10min to change a closed pore structure into an open pore structure, opening the ethanol supercritical high-pressure reaction kettle after exhausting, and then drying the pretreated foamed glass in a blast drying oven at 70 ℃ for 2h for later use.
Heating a mixed solution of 0.36mol of tetraethyl orthosilicate, 12.2mol of ethanol, 0.96mol of deionized water, 0.53mol of formamide and 1.6ml of nitric acid (1mol/L) as an acid catalyst in a water bath at 55 ℃ and continuously stirring, adding sodium hydroxide after 50min to adjust the pH value to 7.5, and continuously stirring for 12min to obtain SiO2Sol; to obtain SiO2Directly pouring the sol into a container containing pretreated foamed glass to obtain SiO2The sol submerged the foamed glass. Then vacuum-impregnating in a vacuum reactor for 10 minutes 2 times, taking out the vacuum-impregnated container filled with silica sol and foam glass from the vacuum reactor, and standing to obtain SiO based on foam glass2A wet gel composite. The obtained SiO taking the foamed glass as a base material2And continuously standing the wet gel composite material for 6 hours, and immediately performing ethanol supercritical drying to obtain the silicon-based aerogel-foam glass heat insulation composite material. The density of the composite material is 0.146g/cm3The heat conductivity is 0.047W/(m.K), the compressive strength is 0.37MPa, the tear strength is 4.46MPa, and the water absorption is 3.8%.
Example 3
Measuring a certain volume of deionized water as a protective solvent, putting the deionized water into a container, completely immersing the foamed glass in the container filled with the protective solvent, and putting CO into the container2In a supercritical high-pressure reaction kettleSyndrome/pattern of CO2And (3) the air tightness of the supercritical high-pressure reaction kettle. By introducing CO2Pressurizing the gas, applying pressure of 5MPa, maintaining the pressure for 13min to change the closed pore structure into an open pore structure, and opening CO after exhausting2And (3) placing the pretreated foamed glass into a supercritical high-pressure reaction kettle, and drying the foamed glass in a forced air drying oven at the temperature of 80 ℃ for 2.5 hours for later use.
Heating a mixed solution of 0.4mol of tetraethyl orthosilicate, 12.8mol of methanol, 0.98mol of deionized water, 0.56mol of acetamide and 1.8ml of hydrochloric acid (1mol/L) as an acid catalyst in a water bath at 60 ℃ and continuously stirring, adding triethanolamine after 55min to adjust the pH value to 7.8, and continuously stirring for 10min to obtain SiO2Sol; to obtain SiO2Directly pouring the sol into a container containing pretreated foamed glass to obtain SiO2The sol submerged the foamed glass. Then vacuum-impregnating in a vacuum reactor for 5 minutes 3 times, taking out the vacuum-impregnated container filled with silica sol and foam glass from the vacuum reactor, and standing to obtain SiO based on foam glass2A wet gel composite. The obtained SiO taking the foamed glass as a base material2And continuously standing the wet gel composite material for 7 hours, and immediately performing ethanol supercritical drying to obtain the silicon-based aerogel-foam glass heat insulation composite material. The density of the composite material is 0.151g/cm3The thermal conductivity is 0.050W/(m.K), the compressive strength is 0.58MPa, the tear strength is 4.56MPa, and the water absorption is 4.1%.
Example 4
Measuring a certain volume of methanol as a protective solvent, putting the methanol into a container, completely immersing the foamed ceramic in the container filled with the protective solvent, and putting the foamed ceramic into CO2In a supercritical high-pressure reaction kettle, ensuring CO2And (3) the air tightness of the supercritical high-pressure reaction kettle. By introducing CO2Pressurizing the gas, applying 6MPa pressure, maintaining the pressure for 15min to change the closed pore structure into an open pore structure, and opening CO after exhausting2And (3) placing the pretreated foamed ceramic into a supercritical high-pressure reaction kettle, and drying for 3 hours at 65 ℃ in a forced air drying oven for later use.
0.43mol of tetraethyl orthosilicate, 13.1mol of acetonitrile, 1mol of deionized water and 0.62molN, heating and continuously stirring a mixed solution of N-dimethylacetamide and 1.9ml of propionic acid (1mol/L) as an acid catalyst in a water bath at 55 ℃, adding ethylenediamine after 60min to adjust the pH value to 8, and continuously stirring for 15min to obtain SiO2Sol; to obtain SiO2Directly pouring the sol into a container containing pretreated foamed ceramics to make SiO2The sol is submerged in the foamed ceramic. Then vacuum-dipping 3 times in a vacuum reactor for 8 minutes each time, taking out the container filled with the silica sol and the foamed ceramics which are vacuum-dipped from the vacuum reactor, and standing to obtain the SiO taking the foamed ceramics as the base material2A wet gel composite. The obtained SiO taking the foamed ceramic as a base material2And continuously standing the wet gel composite material for 8 hours, and immediately performing ethanol supercritical drying to obtain the silicon-based aerogel-foamed ceramic heat-insulation composite material. The density of the composite material is 0.157g/cm3The thermal conductivity is 0.044W/(m.K), the compressive strength is 0.60MPa, the tear strength is 4.35MPa, and the water absorption is 5.6%.
Claims (10)
1. A preparation method of a silicon-based aerogel-foam material heat insulation composite material comprises the following specific steps:
(1) pretreatment of foamed materials
Immersing the foaming material in a container filled with a solvent, putting the container and the foaming material into a high-pressure reaction kettle, pressurizing by gas, applying certain pressure, maintaining the pressure for certain time, opening the high-pressure reaction kettle after exhausting, and then putting the pretreated foaming material into a blast drying box for drying to obtain the pretreated foaming material;
(2)SiO2preparation of the Sol
Pouring a silicon source reagent into a container, adding an organic solvent, deionized water, a drying control chemical additive and an acid catalyst, stirring and reacting in a water bath at a certain temperature, dropwise adding an alkaline catalyst to adjust the pH, and continuously stirring to form SiO2Sol;
(3) preparation of composite materials
Mixing SiO2Pouring the sol into a container containing pretreated foaming material, putting the container into a vacuum reactor, vacuum-impregnating, and taking outStanding to obtain SiO taking the foaming material as a base material2A wet gel composite;
(4) drying of composite materials
SiO taking the foaming material prepared in the step (3) as a base material2And (3) continuously standing the wet gel composite material for a certain time, and then performing supercritical drying on the wet gel composite material by using ethanol to obtain the silicon-based aerogel-foam material heat-insulation composite material.
2. The method according to claim 1, wherein the foaming material in the step (1) is foamed glass or foamed ceramic; the solvent is one or a mixture of more of methanol, ethanol, deionized water or acetonitrile; the high-pressure reaction kettle is an ethanol supercritical reaction kettle or a carbon dioxide supercritical reaction kettle.
3. The method according to claim 1, wherein the gas pressurization in the step (1) is nitrogen, argon or carbon dioxide pressurization; the applied pressure is 2-6MPa, and the pressure maintaining time is 5-15 min; the drying temperature of the air-blast drying box is 65-80 ℃, and the drying time is 2-3 h.
4. The method according to claim 1, wherein the silicon source reagent in the step (2) is tetraethyl orthosilicate; the organic solvent is one of methanol, ethanol or acetonitrile; the drying control chemical additive is one of formamide, acetamide, N-dimethylformamide or N, N-dimethylacetamide.
5. The method of claim 1, wherein the silicon source reagent, the organic solvent, the deionized water, and the drying control chemical additive are present in the step (2) in a molar ratio of 1 (30.2-40): (2.3-3): (1.3-1.5).
6. The method according to claim 1, wherein the acidic catalyst in the step (2) is one of nitric acid, hydrochloric acid, acetic acid, or propionic acid; the molar ratio of the added amount of the acidic catalyst to the silicon source is (0.003-0.005): 1.
7. The preparation method according to claim 1, wherein the temperature of the water bath stirring reaction in the step (2) is 50-60 ℃ and the reaction time is 40-60 min.
8. The method according to claim 1, wherein the basic catalyst in step (2) is one of ammonia, ethylenediamine, triethanolamine or sodium hydroxide, and the pH is adjusted to 7 to 8; stirring for 10-15 min.
9. The method according to claim 1, wherein the number of times of vacuum impregnation in step (3) is 2-3 times, and the interval between each time is 5-10 min.
10. The production method according to claim 1, wherein the standing time in the step (4) is 5 to 8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110315242.XA CN113003947A (en) | 2021-03-24 | 2021-03-24 | Preparation method of silicon-based aerogel-foam material heat insulation composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110315242.XA CN113003947A (en) | 2021-03-24 | 2021-03-24 | Preparation method of silicon-based aerogel-foam material heat insulation composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113003947A true CN113003947A (en) | 2021-06-22 |
Family
ID=76406462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110315242.XA Pending CN113003947A (en) | 2021-03-24 | 2021-03-24 | Preparation method of silicon-based aerogel-foam material heat insulation composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113003947A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115196931A (en) * | 2022-08-12 | 2022-10-18 | 金陵科技学院 | Heat insulation board for building outer wall and manufacturing method thereof |
| CN115321823A (en) * | 2022-09-21 | 2022-11-11 | 厦门市足来爽工贸有限公司 | Foam glass, preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351494A (en) * | 2011-07-20 | 2012-02-15 | 厦门大学 | Method for preparing foam material reinforced silica aerogel composite material |
| CN103419371A (en) * | 2013-08-01 | 2013-12-04 | 四川大学 | Method for preparing rubber foam materiel with perforated structure |
| CN106747628A (en) * | 2017-02-22 | 2017-05-31 | 南京航空航天大学 | A kind of high temperature resistant foam strengthens SiO2Aerogel insulating material and preparation method thereof |
| CN106866180A (en) * | 2017-01-09 | 2017-06-20 | 南京工业大学 | Foamed ceramic composite SiO2Preparation method of aerogel heat insulation material |
| CN107043224A (en) * | 2017-03-29 | 2017-08-15 | 南京工业大学 | Foam glass-SiO2Method for producing aerogels |
| CN109678557A (en) * | 2019-01-16 | 2019-04-26 | 苏州宏久航空防热材料科技有限公司 | A kind of waterglass base SiO2Aeroge/carbon foam composite insulation material |
| CN111848114A (en) * | 2020-07-31 | 2020-10-30 | 航天海鹰(镇江)特种材料有限公司 | Super heat-insulating aerogel composite material and preparation process thereof |
| CN112408937A (en) * | 2020-11-12 | 2021-02-26 | 南京工业大学 | Light high-efficiency SiO2Preparation method of aerogel composite heat-insulating material |
-
2021
- 2021-03-24 CN CN202110315242.XA patent/CN113003947A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351494A (en) * | 2011-07-20 | 2012-02-15 | 厦门大学 | Method for preparing foam material reinforced silica aerogel composite material |
| CN103419371A (en) * | 2013-08-01 | 2013-12-04 | 四川大学 | Method for preparing rubber foam materiel with perforated structure |
| CN106866180A (en) * | 2017-01-09 | 2017-06-20 | 南京工业大学 | Foamed ceramic composite SiO2Preparation method of aerogel heat insulation material |
| CN106747628A (en) * | 2017-02-22 | 2017-05-31 | 南京航空航天大学 | A kind of high temperature resistant foam strengthens SiO2Aerogel insulating material and preparation method thereof |
| CN107043224A (en) * | 2017-03-29 | 2017-08-15 | 南京工业大学 | Foam glass-SiO2Method for producing aerogels |
| CN109678557A (en) * | 2019-01-16 | 2019-04-26 | 苏州宏久航空防热材料科技有限公司 | A kind of waterglass base SiO2Aeroge/carbon foam composite insulation material |
| CN111848114A (en) * | 2020-07-31 | 2020-10-30 | 航天海鹰(镇江)特种材料有限公司 | Super heat-insulating aerogel composite material and preparation process thereof |
| CN112408937A (en) * | 2020-11-12 | 2021-02-26 | 南京工业大学 | Light high-efficiency SiO2Preparation method of aerogel composite heat-insulating material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115196931A (en) * | 2022-08-12 | 2022-10-18 | 金陵科技学院 | Heat insulation board for building outer wall and manufacturing method thereof |
| CN115321823A (en) * | 2022-09-21 | 2022-11-11 | 厦门市足来爽工贸有限公司 | Foam glass, preparation method and application thereof |
| CN115321823B (en) * | 2022-09-21 | 2023-10-20 | 厦门市足来爽工贸有限公司 | Foam glass, preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106830990B (en) | Porous geopolymer/aerogel composite heat-insulating material and preparation method thereof | |
| CN110922095B (en) | Preparation method of composite silica aerogel felt | |
| CN102584162B (en) | Unitary or polybasic aerogel thermal insulation material and preparation method thereof | |
| CN103130231B (en) | A kind of silica aerogel material and preparation method thereof | |
| CN108641361B (en) | Fiber-reinforced organic silicon aerogel heat-insulation composite material and preparation method thereof | |
| CN100594197C (en) | Nano thermal insulation energy-saving material and producing technique | |
| CN103467058B (en) | Method for preparing waterproof, antifouling, environment-friendly and flame retardant insulation board by using pitchstone beads | |
| CN109650841B (en) | Fireproof sound-insulation heat-preservation aerogel composite material and preparation method thereof | |
| CN113003947A (en) | Preparation method of silicon-based aerogel-foam material heat insulation composite material | |
| CN105198375A (en) | Thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite and preparation method thereof | |
| CN113636824B (en) | Preparation method of enhanced silicon dioxide aerogel composite material | |
| CN112062515B (en) | High-strength geopolymer closed-cell foam material prepared from silicon carbide and preparation method thereof | |
| CN113264532A (en) | Super-hydrophobic light transparent high-strength SiO2Method for producing aerogels | |
| CN103821239B (en) | A kind of fire-retardant nano-pore SiO 2multistage composite thermal insulation slab and preparation method thereof | |
| CN114044647B (en) | Preparation process of A2-level nano inorganic insulation board | |
| CN106866180A (en) | Foamed ceramic composite SiO2Preparation method of aerogel heat insulation material | |
| CN102219455B (en) | Inorganic lightweight aggregate thermal insulation sheet material and preparation method thereof | |
| CN108439964B (en) | Nano-pore ceramic heat-insulating coiled material and preparation method thereof | |
| CN114835440A (en) | Carbon-fixing slag foam concrete wall material and preparation method thereof | |
| CN105601168A (en) | Inorganic thermal insulation material and preparation method thereof | |
| CN116200937B (en) | Composite heat insulation felt and preparation method thereof | |
| CN111792884A (en) | Environment-friendly heat-insulating material for buildings and preparation method thereof | |
| CN113754466B (en) | Preparation method of high-performance ceramic insulation board | |
| CN111304910A (en) | Ceramic fiber/hydrophobic silicon dioxide aerogel composite material and preparation method thereof | |
| CN110862258B (en) | Load-bearing carbon aerogel-porous silicon dioxide composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230712 Address after: 210009, 5 new model street, Gulou District, Jiangsu, Nanjing Applicant after: Nanjing Tech University Address before: 210009, 5 new model street, Gulou District, Jiangsu, Nanjing Applicant before: Nanjing Tech University Applicant before: SUQIAN ADVANCED MATERIALS INSTITUTE OF NANJING TECH University |
|
| TA01 | Transfer of patent application right | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210622 |
|
| RJ01 | Rejection of invention patent application after publication |