CN111268995A - Honeycomb nano-pore structure composite heat insulation material and preparation method thereof - Google Patents
Honeycomb nano-pore structure composite heat insulation material and preparation method thereof Download PDFInfo
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/04—Manufacture of glass fibres or filaments by using centrifugal force, e.g. spinning through radial orifices; Construction of the spinner cups therefor
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- 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
- C03C13/00—Fibre or filament compositions
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0006—Honeycomb structures
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
- C04B38/0054—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity the pores being microsized or nanosized
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- 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
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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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- 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
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention discloses a composite heat-insulating material with a honeycomb nano-pore structure and a preparation method thereof. Compared with glass fiber composite heat insulation materials synthesized by other methods, the composite heat insulation material prepared by the method has the advantages that the nano particles are not easy to fall off, the heat conductivity coefficient is lower, and the structural stability and the mechanical property of the composite heat insulation material are greatly improved.
Description
Technical Field
The invention belongs to the technical field of functional composite materials, and relates to a composite heat-insulating material with a honeycomb nano-pore structure and a preparation method thereof.
Background
The superfine glass fiber belongs to a cotton-shaped porous non-metallic material with excellent performance, and has the characteristics of excellent heat insulation and sound absorption performance, light weight, good electrical insulation, shock resistance, temperature resistance, A-level non-combustibility, strong chemical corrosion resistance and the like. At present, the superfine glass fiber is widely applied to the field of heat insulating materials of buildings, transportation vehicles, nuclear power, household appliance refrigeration and the like. As a novel porous functional material, pores and solid phase particles of the aerogel internal structure are in a nanometer order, so that the aerogel has excellent performances of high porosity, low thermal conductivity, high specific surface area, low dielectric constant, semitransparent material and the like, and has a huge application prospect in the field of super heat-insulating materials. How to compound superfine glass fiber and aerogel nanoparticles, how to effectively introduce a large amount of nanometer pores into the fiber to prepare a fiber/nanoparticle composite material with a multilevel pore structure, how to enable the obtained material to have a stable honeycomb-shaped nanopore structure, and how to form a compact stacking state by tightly intertwining the fibers, thereby greatly improving the structural stability and mechanical properties of the material, which are the key points of the current thermal insulation material research.
The invention discloses a high-temperature-resistant glass fiber reinforced aerogel composite felt and a preparation method thereof, and discloses the high-temperature-resistant glass fiber reinforced aerogel composite felt and the preparation method thereof, wherein the high-temperature-resistant glass fiber reinforced aerogel composite felt is formed by vacuum packaging a hot melting layer and a composite core material, the hot melting layer is a glass fiber shell, the porosity in the hot melting layer is in gradient distribution along the thickness direction of the composite felt, the composite core material is superfine glass fiber reinforced aerogel, and the volume content of aerogel particles in the composite core material is also in gradient distribution along the thickness direction of the composite felt. The heat preservation and heat insulation performance of the material is influenced, the whole vacuum packaging is realized, and the heat conductivity coefficient of the material is greatly reduced.
In a patent with publication number CN105819823B, a preparation method of a silica aerogel and glass fiber mat composite material is disclosed, which comprises the following steps: placing the glass fiber mat in a suitable container in a rolled form or a laid flat form; the silica aerogel sol-gel process adopts a novel 'two-step catalysis method' of acid catalysis hydrolysis and fluorine ion catalysis polycondensation; injecting the prepared sol-gel precursor solution into the paved glass fiber felt, exhausting air in the glass fiber felt, and filling gaps in the glass fiber felt with the sol-gel precursor solution; the sol-gel precursor solution is gelled in the gaps of the glass fiber mat to obtain a glass fiber mat gel composite material, and the gelled glass fiber mat composite material is rolled again; and modifying the recoiled glass fiber mat and silicon dioxide gel composite material in an ethanol solution of hexamethyldisilazane, and drying the gel composite material by a supercritical fluid to obtain the silicon dioxide aerogel and glass fiber mat composite material.
In a patent of a preparation method of a hydrophobic silica aerogel composite fiber felt material with publication number CN108569912A, a preparation method of a hydrophobic silica aerogel composite fiber felt material is disclosed, which comprises mixing tetraethoxysilane, ethanol, water and an acid catalyst to obtain silica sol; adding an alkali catalyst into silica sol, stirring uniformly, pouring the mixture into a fiber felt (ceramic and glass fiber felt) to be immersed, standing to obtain a gel composite material, placing the composite material gelled in the fiber felt into a mother solution, aging for a certain time, then carrying out solvent exchange to obtain a composite material, immersing the composite material into a solution containing a surface modifier with a certain concentration, standing for modification, and then drying the composite material at normal pressure to obtain the hydrophobic silica aerogel composite fiber felt material. The invention has the advantages of simple process, short production period, lower cost, low requirement on equipment and excellent product performance, and the prepared composite material has the performances of super-hydrophobic property, strong adsorbability, low heat conductivity coefficient and the like.
In the three patents disclosed above, the aerogel nanoparticles are bonded with the fibers only by intermolecular forces, so that the nanoparticles loaded on the fibers are easy to fall off in the use process, and the material is brittle, vibration-resistant and non-resilient. Meanwhile, high-concentration nanoparticles are easy to agglomerate on the surface of the fiber, so that the effective specific surface area of the fiber is reduced, and the fiber becomes brittle. Therefore, aiming at the problem of how the aerogel nanoparticles are uniformly distributed in the internal network structure of the superfine glass fiber cotton and form stronger bonding force with fibers, the superfine glass fibers and the aerogel nanoparticles are organically combined to form a uniform and stable apparent structure, and the problem to be solved urgently is to prepare the composite heat-insulating material with low thermal conductivity, excellent mechanical property and stable structure.
Disclosure of Invention
The invention aims to provide a composite heat-insulating material which is prepared by carrying out freeze forming, vacuum freeze drying and nitrogen atmosphere calcining on aerogel solution containing dispersed superfine glass fibers to enable aerogel nanoparticles to grow on the surfaces of the superfine glass fibers in situ and enable layered ice crystals to continuously grow and extrude fibers to form a honeycomb-shaped nano-pore structure. By controlling 55-92 wt% of superfine glass fiber, 12-45 wt% of aerogel, 1.5-6 wt% of opacifier and 0.15-2.25 wt% of water-resistant modifier; wherein the microglass fibers consist of: SiO22：57.5～73.5wt％，Na2O+K2O：8～10.5wt％，Al2O3+MgO+CaO：15.5～24wt％， B2O3：4～8wt％，Fe2O3+ ZnO + BaO: < 1.3 wt% composition. The fiber diameters of the prepared superfine glass fibers are normally distributed at 0.6-2.4 mu m in 98.5 percent, and the average pore diameters of the aerogel are normally distributed at 25-40 nm in 99.9 percent, so that a honeycomb-shaped nano-pore structure is formed inside the prepared composite heat-insulating material, aerogel nano-particles grow on the surface of the superfine glass fibers in situ to form strong binding force, the heat conductivity coefficient of the prepared composite heat-insulating material is effectively reduced, and the mechanical property of the composite heat-insulating material is improved.
In order to achieve the purpose of preparing the composite heat-insulating material with the cellular nanopore structure, the invention also provides a preparation method of the composite heat-insulating material with the cellular nanopore structure, which comprises the following steps:
(1) selecting a proper amount of waste plate glass, quartz sand, albite, potash feldspar, borax, soda ash, calcite, dolomite, zinc oxide and barium carbonate according to the components of the superfine glass fiber, uniformly mixing the components in proportion, putting the mixture into a kiln for smelting, calcining the mixture into glass liquid with uniform components, then flowing into a centrifugal disc rotating at a high speed, and finally throwing out the superfine glass fiber with uniform fiber diameter;
(2) completely dipping and dispersing the prepared superfine glass fiber into a mixed solution of an aerogel precursor, an opacifier and a water-resistant modifier, and completely freezing and molding the mixed solution containing the dispersed fiber;
(3) vacuum freeze-drying the frozen and molded mixture to enable aerogel nanoparticles to grow on the surface of the superfine glass fiber in situ to form a nanopore complex;
(4) and calcining the nanopore composite body in a nitrogen atmosphere to finally prepare the composite heat-insulating material with the cellular nanopore structure.
The advantages of the invention are as follows: by utilizing the organic combination of the superfine glass fiber and the aerogel, aerogel nanoparticles grow on the surface of the superfine glass fiber in situ, and the layered ice crystals continuously grow and extrude the fiber to form a honeycomb-shaped nano-pore structure, and the prepared composite heat-insulating material has the characteristics of low heat conductivity coefficient, stable structure, excellent mechanical property and the like. Compared with other aerogel and glass fiber composite heat insulation materials, the composite heat insulation material is more compact in conductive compounding, less prone to powder falling, more convenient for subsequent machining and longer in service life.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will become apparent to those skilled in the art after reading the present invention, as defined in the appended claims.
Example 1
Weighing 70 parts of waste plate glass, 9 parts of quartz sand, 3 parts of soda ash, 3.5 parts of potassium feldspar powder, 3 parts of sodium feldspar powder, 4.5 parts of borax, 3 parts of dolomite, 3 parts of calcite, 0.5 part of zinc oxide and 0.5 part of barium carbonate according to the weight ratio, uniformly mixing, putting into a kiln for calcining, and smelting into glass liquid with uniform components and no impurities and transparency, wherein the temperature of the obtained glass liquid is 1290 ℃. Then, the glass liquid is thrown out of the superfine glass fiber through a centrifugal disc rotating at a high speed, the flow rate of the glass liquid when the glass liquid is drained into the centrifugal machine is 385kg/h, the rotating speed of the centrifugal disc is 2350r/min, the temperature is 975 ℃, and 99.3 percent of the fiber diameter of the prepared superfine glass fiber is normally distributed in the range of 1.4-2.2 mu m. 1.0g was preparedThe superfine glass fiber is cut into pieces and dispersed in the raw material with the molar ratio of n (H)2O): n(NaOH)＝1:9.5×10-415 wt% ZrO2Dispersing the mixture in aerogel precursor solution of 3 wt% of SiC opacifier and 2 wt% of trimethylchlorosilane water-resistant modifier for 6min by using a high-speed homogeneous dispersion machine at the rotating speed of 12500rpm, and then carrying out freeze drying for 12h in a freeze dryer with the vacuum degree of 55Pa and the temperature of-15 ℃. Finally, placing the freeze-dried nanopore complex in a nitrogen atmosphere at 600 ℃ for calcining for 40min and preserving heat for 1h, wherein the temperature rise speed is set to be 5 ℃ min-1And finally, preparing the composite heat-insulating material with the honeycomb nano-pore structure.
The detection shows that the prepared composite heat-insulating material: the internal pore structure is cellular nano-pore, the porosity is more than or equal to 99.5 percent, the average pore diameter is less than or equal to 35nm, and the volume density is 0.355 mg-cm-3The maximum compressive stress is 10.5kPa, the initial height can still be recovered when the compressive strain reaches 80 percent, and the thermal conductivity is 0.0135W/(m.K).
Example 2
Weighing 63 parts of waste plate glass, 11 parts of quartz sand, 4 parts of soda ash, 5 parts of potassium feldspar powder, 3 parts of sodium feldspar powder, 3 parts of borax, 4 parts of dolomite, 5 parts of calcite, 1 part of zinc oxide and 1 part of barium carbonate according to the weight ratio, uniformly mixing, then putting into a kiln for calcining, and smelting into glass liquid with uniform components and no impurities and transparency, wherein the temperature of the obtained glass liquid is 1295 ℃. Then, the glass liquid is thrown out of the superfine glass fiber through a centrifugal disc rotating at a high speed, the flow rate of the glass liquid when the glass liquid is drained into a centrifugal machine is 400kg/h, the rotating speed of the centrifugal disc is 2350r/min, the temperature is 985 ℃, and 99.5 percent of the fiber diameter of the prepared superfine glass fiber is normally distributed at 0.8-2 mu m. 1.8g of the prepared ultrafine glass fibers were chopped and dispersed in a raw material molar ratio of n (H)2O): n(NaOH)＝1:1×10-335 wt% of Al2O3Dispersing the mixture in aerogel precursor solution of 4.5 wt% of SiC opacifier and 2.2 wt% of hexamethyldisilane water-resistant modifier for 5min at 13000rpm by using a high-speed homogenizing dispersion machine, and then carrying out freeze drying for 14h in a freeze dryer with the vacuum degree of 40Pa and the temperature of-20 ℃. Finally placing the freeze-dried nano-pore complexCalcining at 650 deg.C for 30min in nitrogen atmosphere, and maintaining the temperature for 1h, with the temperature rise rate set at 5 deg.C/min-1And finally, preparing the composite heat-insulating material with the honeycomb nano-pore structure.
The detection shows that the prepared composite heat-insulating material: the internal pore structure is cellular nano-pore, the porosity is more than or equal to 99.9 percent, the average pore diameter is less than or equal to 25nm, and the volume density is 0.155 mg-cm-3The maximum compressive stress is 12kPa, the initial height can still be recovered when the compressive strain reaches 88 percent, and the thermal conductivity is 0.0115W/(m.K).
The invention has been described with reference to a single embodiment, but it is not intended to limit the invention to the exact form and detail shown and described, and it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (11)
1. The composite heat-insulating material with the cellular nano-pore structure is characterized by comprising the following components in percentage by weight: 55-92 wt% of superfine glass fiber, 12-45 wt% of aerogel, 1.5-6 wt% of opacifier and 0.15-2.25 wt% of water-resistant modifier; wherein the microglass fibers consist of: SiO 2: 57.5-73.5 wt%, Na2O + K2O: 8-10.5 wt%, Al2O3+ MgO + CaO: 15.5-24 wt%, B2O 3: 4-8 wt%, Fe2O3+ ZnO + BaO: < 1.3 wt%.
2. The composite heat insulating material with a cellular nano-pore structure of claim 1, wherein the diameters of the ultrafine glass fibers are all normally distributed within 0.6 to 2.4 μm at 98.5%.
3. The composite heat-insulating material with the cellular nano-pore structure as claimed in claim 1, wherein the aerogel is one or more of SiO2, ZrO2, B2O3, Al2O3, BN, fullerene, graphene and carbon nanotube aerogel, and the average pore diameter of 99.9% is normally distributed in the range of 25-40 nm.
4. The composite heat-insulating material with the cellular nano-pore structure as claimed in claim 1, wherein the opacifier is one or more of TiO2, SiC, Fe3O4, B4C and carbon black, and the content of the opacifier accounts for 1.5-6 wt% of the total weight of the composite heat-insulating material.
5. The composite heat-insulating material with the cellular nanopore structure as claimed in claim 1, wherein the water-resistant modifier is one or more of trimethylchlorosilane, hexamethyldisilane, hexamethylsiloxane and hydroxyl amino silicone oil, and the content of the water-resistant modifier is 0.15-2.25 wt% of the total weight of the composite heat-insulating material.
6. The preparation method of the cellular nanopore structure composite heat insulation material according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) selecting a proper amount of waste plate glass, quartz sand, albite, potash feldspar, borax, soda ash, calcite, dolomite, zinc oxide and barium carbonate according to the components of the superfine glass fiber, uniformly mixing the components in proportion, putting the mixture into a kiln for smelting, calcining the mixture into glass liquid with uniform components, then flowing into a centrifugal disc rotating at a high speed, and finally throwing out the superfine glass fiber with uniform fiber diameter;
(2) completely dipping and dispersing the prepared superfine glass fiber into a mixed solution of an aerogel precursor, an opacifier and a water-resistant modifier, and completely freezing and molding the mixed solution containing the dispersed fiber;
(3) vacuum freeze-drying the frozen and molded mixture to enable aerogel nanoparticles to grow on the surface of the superfine glass fiber in situ to form a nanopore complex;
(4) and calcining the nanopore composite body in a nitrogen atmosphere to finally prepare the composite heat-insulating material with the cellular nanopore structure.
7. The preparation method according to claim 6, wherein in the step (1), 57 to 83 parts by mass of waste plate glass, 9 to 16 parts by mass of quartz sand, 3 to 9 parts by mass of soda ash, 1.5 to 5 parts by mass of potassium feldspar, 0.5 to 5.5 parts by mass of albite, 1 to 6 parts by mass of borax, 2.5 to 10.5 parts by mass of dolomite, 4 to 9.5 parts by mass of calcite, 0.5 to 1 part by mass of zinc oxide, and 0.5 to 2.5 parts by mass of barium carbonate are weighed.
8. The method according to claim 6, wherein in the step (1), the temperature of the molten glass is 1290 ± 10 ℃ and the temperature of the high-speed rotating centrifugal disk is 970 ± 10 ℃; when the glass liquid is guided into the centrifugal machine, the glass liquid flow is 225-455 kg/h, and the rotation speed of the centrifugal disc is 2050-2350 r/min.
9. The preparation method according to claim 6, wherein in the step (2), the raw materials in the aerogel precursor solution are in the following molar ratios: n (H2O): n (NaOH) ═ 1:8 × 10-4 to 1:1 × 10-3, the dispersion of the mixed solution is carried out at a shear rate of 10000 to 14000rpm for 5 to 8 minutes, and the mixed solution is frozen and molded at an average freezing rate of 5 ℃ min-1 for 10 to 15 minutes.
10. The preparation method according to claim 6, wherein in the step (3), the vacuum degree of the vacuum freeze drying is 40-65 Pa, the freeze drying temperature is-35 to-5 ℃, and the freeze drying time is 10-16 h.
11. The method according to claim 6, wherein in the step (4), the temperature of the calcination in the nitrogen atmosphere is raised at a rate of 5 ℃ min-1, and the calcination is carried out at 550 to 700 ℃ for 25 to 45min in the nitrogen atmosphere and the temperature is maintained for 1 to 1.5 hours.
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Application publication date: 20200612 |
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