CN117125961A - Preparation method of centrifugal spinning ceramic fiber aerogel - Google Patents
Preparation method of centrifugal spinning ceramic fiber aerogel Download PDFInfo
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- 238000009987 spinning Methods 0.000 title claims abstract description 100
- 239000000835 fiber Substances 0.000 title claims abstract description 74
- 239000004964 aerogel Substances 0.000 title claims abstract description 29
- 239000000919 ceramic Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000007246 mechanism Effects 0.000 claims abstract description 68
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000005245 sintering Methods 0.000 claims abstract description 36
- 239000012528 membrane Substances 0.000 claims abstract description 32
- 238000005507 spraying Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000011049 filling Methods 0.000 claims description 35
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 34
- 229920000642 polymer Polymers 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 16
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 7
- 229920001661 Chitosan Polymers 0.000 claims description 7
- 235000010413 sodium alginate Nutrition 0.000 claims description 7
- 239000000661 sodium alginate Substances 0.000 claims description 7
- 229940005550 sodium alginate Drugs 0.000 claims description 7
- 239000002033 PVDF binder Substances 0.000 claims description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 6
- 229920001046 Nanocellulose Polymers 0.000 claims description 4
- 239000012774 insulation material Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000011800 void material Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 101
- 229920002284 Cellulose triacetate Polymers 0.000 description 11
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 101150038956 cup-4 gene Proteins 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000131 polyvinylidene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6224—Fibres based on silica
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The application discloses a preparation method of centrifugal spinning ceramic fiber aerogel, which comprises the following steps: a spinnable solution is provided. And (3) carrying out centrifugal spinning on the spinnable solution through a centrifugal spinning device, and spraying the spinnable solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane. Immersing the two-dimensional fiber membrane in a polymer-ethanol solution, taking out, drying, stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel. According to the preparation method, the spinnable solution is prepared into the two-dimensional fiber membrane by utilizing centrifugal spinning, then the two-dimensional fiber membrane is immersed in the polymer-ethanol solution, then the two-dimensional fiber membrane is taken out, dried and stacked into a three-dimensional structure, and then the organic matters are removed by sintering, so that the ceramic fiber aerogel with the void structure is obtained.
Description
Technical Field
The application relates to the field of aerogel, in particular to a preparation method of centrifugal spinning ceramic fiber aerogel.
Background
In recent years, attention has been paid to flexible ceramic fiber aerogel materials, and attention has been paid to the materials, and the materials have been widely studied and applied, which have excellent properties such as low density, high porosity, high specific surface area, low thermal conductivity, chemical stability and thermal stability.
The preparation method of the ceramic fiber aerogel has the advantages of low yield, poor efficiency and difficult industrialization, or limited raw material selection, complex process, high cost and lack of a preparation method with simple flow, low cost and easy industrialization.
Disclosure of Invention
The application provides a preparation method of centrifugal spinning ceramic fiber aerogel, which can simplify the preparation process and reduce the preparation cost.
The application adopts the following technical scheme:
the application provides a preparation method of centrifugal spinning ceramic fiber aerogel, which comprises the following steps: a spinnable solution is provided. And (3) carrying out centrifugal spinning on the spinnable solution through a centrifugal spinning device, and spraying the spinnable solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane. Immersing the two-dimensional fiber membrane in a polymer-ethanol solution,
and then taking out, drying, stacking into a three-dimensional structure, and then sintering to obtain the ceramic fiber aerogel.
Further, the spinnable solution comprises any one or a combination of a plurality of silicate solutions, nanocellulose solutions, sodium alginate solutions and chitosan solutions.
Further, the solvent of the silicate solution comprises one or a combination of several of ethanol, hydrochloric acid, tetraethoxysilane and N, N-dimethylformamide.
Further, the concentration of the spinnable solution is 1.0-15.0wt%.
Further, the motor speed of the centrifugal spinning device is 2000-4000 rpm, and the diameter of the spinning hole is 0.1-1mm.
Further, the spinning interval of centrifugal spinning is 30-50cm.
Further, the spinning temperature of the centrifugal spinning is 0-185 ℃.
Further, the sintering temperature is 200-1500 ℃, and the sintering temperature is kept for 12 hours.
Further, the polymer of the polymer-ethanol solution includes at least one of PVA, PVB, PVDF.
The application also provides a centrifugal spinning device applying the preparation method, which comprises a shell, a rotor, a motor, a collecting mechanism, a filling mechanism, a heat preservation mechanism, a heating mechanism and a power supply mechanism. The housing has an air inlet. The rotor is arranged in the shell, the side wall of the rotor is provided with a spinning hole, and the rotor is used for containing polymer solution. The motor is arranged in the shell, and is connected with the rotating cup and used for driving the rotating cup to rotate. The collecting mechanism is arranged in the shell and is arranged on the periphery of the rotating cup in a surrounding mode, and the collecting mechanism is used for forming a two-dimensional fiber film. The filling mechanism is arranged in the shell, the filling mechanism defines a filling cavity, the bottom wall of the filling cavity is provided with a filling opening, the filling opening faces the top opening of the rotating cup, and the filling mechanism is used for collecting polymer solution into the filling cavity and supplying the polymer solution in the filling cavity to the rotating cup. The heat preservation mechanism is arranged in the shell and arranged on the outer wall of the rotating cup and the outer wall of the filling mechanism, and the heat preservation mechanism is used for carrying out heat preservation and heating on polymer solution in the rotating cup and the filling cavity. The heating mechanism is arranged outside the shell and at the air inlet, and the heating mechanism is used for adjusting the air inlet temperature at the air inlet. The power supply mechanism is arranged outside the shell, the power supply mechanism is connected with the motor, the heat preservation mechanism and the heating mechanism, the anode of the power supply mechanism is inserted into the polymer solution in the filling cavity, the cathode of the power supply mechanism is connected with the grounded collecting mechanism, and the power supply mechanism is used for providing power.
The application also provides an application of the ceramic fiber aerogel prepared by the preparation method as a heat preservation and insulation material.
Compared with the prior art, the application has the following beneficial effects:
according to the preparation method, the spinnable solution is prepared into the two-dimensional fiber membrane by utilizing centrifugal spinning, then the two-dimensional fiber membrane is immersed in the polymer-ethanol solution, then the two-dimensional fiber membrane is taken out, dried and stacked into a three-dimensional structure, and then the organic matters are removed by sintering, so that the ceramic fiber aerogel with the void structure is obtained.
Drawings
FIG. 1 is an SEM image of a ceramic fiber aerogel according to an embodiment of the application;
fig. 2 is a schematic structural view of a centrifugal spinning device in an embodiment of the application.
Detailed Description
The technical method in the embodiments of the present application will be clearly and completely described below. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The embodiment of the application provides a preparation method of centrifugal spinning ceramic fiber aerogel, which comprises the following steps:
step one, providing a spinnable solution.
In the above step, the spinnable solution is a polymer solution, a polymer suspension, or a polymer-ceramic precursor solution. The spinnable solution contains a polymeric phase and a ceramic dispersed or particulate phase.
The spinnable solution is any one or a combination of a plurality of silicate solutions, nanocellulose solutions, sodium alginate solutions and chitosan solutions. For example, the spinnable solution is a silicate solution, such as a tetraethyl silicate solution. The spinnable solution is a nanocellulose solution, such as a Cellulose Triacetate (CTA) solution. The spinnable solution is a mixed solution of silicate, sodium alginate and chitosan.
Wherein the solvent of the silicate solution comprises one or a combination of more of ethanol, hydrochloric acid, tetraethoxysilane (TEOS) and N, N-Dimethylformamide (DMF). For example, the solvent of the silicate solution is ethanol. The solvent of the silicate solution is a mixed solution of hydrochloric acid and tetraethoxysilane. The preparation method of the silicate solution comprises the following steps: dissolving silicate in one or more solvents selected from ethanol, hydrochloric acid, TEOS and DMF, and stirring to obtain silicate solution.
The concentration of the spinnable solution is 1.0-15.0wt%, such as 1.0wt%, 5.0wt%, 10.0wt%, 15.0wt%. Preferably 2.0-12.0wt%, such as 2.0wt%, 7.0wt%, 12.0wt%.
And secondly, carrying out centrifugal spinning on the spinnable solution through a centrifugal spinning device, and spraying the spinnable solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane.
In the above steps, the spinnable solution is sprayed from the spinning hole of the centrifugal spinning device by using the centrifugal force generated by the centrifugal spinning device in a high-speed rotation state, the sprayed spinnable solution is stretched in the jet movement process, and the solvent in the spinnable solution is volatilized under the action of hot air and sprayed onto the collecting surface of the collecting mechanism, so that the two-dimensional fiber membrane is prepared.
The motor speed of the centrifugal spinning device is 2000-4000 rpm, such as 2000 rpm, 3000 rpm, 4000 rpm. Preferably 4000 rpm. The diameter of the spinneret orifice is 0.1-1mm, such as 0.1mm, 0.5mm, 1mm. Preferably 0.8mm.
The spinning interval of centrifugal spinning is 30-50cm, such as 30cm, 40cm, 50cm. Preferably 50cm
The spinning temperature of the centrifugal spinning is 0-185 ℃, such as 0 ℃, 50 ℃, 100 ℃, 150 ℃ and 185 ℃. Preferably 50-140℃such as 50℃80℃100℃140 ℃. More preferably 100 ℃.
And thirdly, immersing the two-dimensional fiber membrane in a polymer-ethanol solution, taking out, drying, folding or stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel.
In the above step, the polymer of the polymer-ethanol solution includes at least one of polyvinyl alcohol (PVA), polyvinyl butyral (PVB), and polyvinylidene fluoride (PVDF). For example, the polymer of the polymer-ethanol solution is polyvinyl alcohol (PVA). The polymers of the polymer-ethanol solution are polyvinyl butyral (PVB) and polyvinylidene fluoride (PVDF).
And (3) sintering the product with the three-dimensional structure at high temperature, and removing organic components and residues in the fiber, wherein the average diameter of the sintered fiber is obviously reduced.
The sintering temperature is 200-1500deg.C, such as 200deg.C, 500 deg.C, 1000 deg.C, and 1500deg.C. Preferably 800-1300deg.C, such as 800 deg.C, 1000 deg.C, 1300 deg.C. More preferably 1260 ℃. Sintering is maintained for 12 hours.
Compared with direct sintering of a two-dimensional fiber membrane, the method is beneficial to increasing the elasticity of a product by forming a three-dimensional structure (particularly a three-dimensional lamellar connected structure).
The ceramic fiber aerogel prepared by the preparation method has a micro-nano pore structure and low thermal conductivity, and achieves the advantages of low fiber density, high specific surface area, good heat insulation performance and good heat preservation effect. SEM images of the ceramic fiber aerogel prepared by the preparation method of the application are shown in fig. 1.
In addition, the preparation method prepares the spinnable solution into the two-dimensional fiber membrane by utilizing the centrifugal spinning with simple operation and high yield, then dips the two-dimensional fiber membrane into the polymer-ethanol solution, then takes out the two-dimensional fiber membrane, dries the two-dimensional fiber membrane, stacks the two-dimensional fiber membrane into a three-dimensional structure, and then sinters the three-dimensional structure to remove organic matters, so that the ceramic fiber aerogel with the void structure is obtained.
Referring to fig. 2, the embodiment of the application also provides a centrifugal spinning device applying the preparation method, which comprises a shell 1, a rotor 4, a motor 6, a collecting mechanism 3, a filling mechanism 2, a heat preservation mechanism 5, a heating mechanism and a power supply mechanism.
The housing 1 has an air inlet.
The rotor 4 is used for holding a polymer solution. The rotor 4 is arranged in the housing 1. The side wall of the rotor 4 has spinning holes 7.
The motor 6 is used for driving the rotary cup 4 to rotate. The motor 6 is disposed within the housing 1. The motor 6 is connected with the rotor 4.
The collecting means 3 is used for forming a two-dimensional fibrous membrane. The collecting mechanism 3 is arranged in the shell 1 and is arranged around the periphery of the rotating cup 4.
The filling mechanism 2 is used for collecting the polymer solution into the filling chamber and supplying the polymer solution in the filling chamber to the rotor 4. The filling means 2 are arranged in the housing 1 and above the rotor 4. The filling means 2 define a filling chamber, the bottom wall of which has a filling opening facing the top opening of the rotor 4.
The heat preservation mechanism 5 is used for carrying out heat preservation and heating on the polymer solution in the rotating cup 4 and the filling cavity so as to prevent the polymer solution from being solidified too fast. The heat preservation mechanism 5 is arranged in the shell 1 and arranged on the outer wall of the rotary cup 4 and the outer wall of the filling mechanism 2.
The heating mechanism is used for adjusting the air inlet temperature at the air inlet so as to adjust the internal temperature of the outer shell 1, thereby providing different experimental temperatures. The heating mechanism is arranged outside the shell 1 and at the air inlet.
The power supply mechanism is used for providing power. The power supply mechanism is arranged outside the housing 1. The power supply mechanism is connected with the motor 6, the heat preservation mechanism 5 and the heating mechanism, the anode of the power supply mechanism is inserted into the polymer solution in the filling cavity, and the cathode is connected with the grounded collecting mechanism 3.
The embodiment of the application also provides an application of the ceramic fiber aerogel prepared by the preparation method as a heat insulation material.
The following is a detailed description of specific embodiments:
example 1
Step one, dissolving tetraethyl silicate in ethanol, hydrochloric acid and deionized water, and stirring to obtain a tetraethyl silicate solution. Wherein the concentration of the tetraethyl silicate solution is 5wt%, and the mass ratio of the tetraethyl silicate to the ethanol to the hydrochloric acid to the deionized water is 1:11:0.01:8.
And step two, centrifugally spinning the tetraethyl silicate solution through a centrifugal spinning device, and spraying the tetraethyl silicate solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane. Wherein, the motor rotating speed of the centrifugal spinning device is 2000 revolutions per minute, the diameter of the spinning hole is 0.1mm, the spinning interval of the centrifugal spinning is 30cm, and the spinning temperature of the centrifugal spinning is 50 ℃. And (3) ejecting the tetraethyl silicate solution from a spinning hole of the centrifugal spinning device by utilizing the centrifugal force generated by the centrifugal spinning device in a high-speed rotation state, wherein the ejected tetraethyl silicate solution is stretched in the jet flow movement process, and the solvent in the tetraethyl silicate solution is volatilized under the action of hot air.
And thirdly, immersing the two-dimensional fiber membrane in a polyvinyl alcohol-ethanol solution, taking out, drying, stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel. Wherein the sintering temperature is 800 ℃, and the sintering time is 12 hours. After the organic components and residues in the fiber are removed by sintering, the average diameter of the fiber after sintering is obviously reduced.
Example 2
Step one, dissolving tetraethyl silicate in ethanol, hydrochloric acid and deionized water, and stirring to obtain a tetraethyl silicate solution. Wherein the concentration of the tetraethyl silicate solution is 10wt%, and the mass ratio of the tetraethyl silicate to the ethanol to the hydrochloric acid to the deionized water is 1:5:0.02:4.
And step two, centrifugally spinning the tetraethyl silicate solution through a centrifugal spinning device, and spraying the tetraethyl silicate solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane. Wherein, the motor rotating speed of the centrifugal spinning device is 3000 r/min, the diameter of the spinning hole is 0.2mm, the spinning interval of the centrifugal spinning is 40cm, and the spinning temperature of the centrifugal spinning is 60 ℃. And (3) ejecting the tetraethyl silicate solution from a spinning hole of the centrifugal spinning device by utilizing the centrifugal force generated by the centrifugal spinning device in a high-speed rotation state, wherein the ejected tetraethyl silicate solution is stretched in the jet flow movement process, and the solvent in the tetraethyl silicate solution is volatilized under the action of hot air.
And thirdly, immersing the two-dimensional fiber membrane in polyvinylidene fluoride-ethanol solution, taking out, drying, stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel. Wherein the sintering temperature is 1000 ℃ and maintained for 12 hours. After the organic components and residues in the fiber are removed by sintering, the average diameter of the fiber after sintering is obviously reduced.
Example 3
Step one, dissolving tetraethyl silicate in ethanol, hydrochloric acid and deionized water, and stirring to obtain a tetraethyl silicate solution. Wherein the concentration of the tetraethyl silicate solution is 12wt%, and the mass ratio of the tetraethyl silicate to the ethanol to the hydrochloric acid to the deionized water is 1:4:0.02:4.
And step two, centrifugally spinning the tetraethyl silicate solution through a centrifugal spinning device, and spraying the tetraethyl silicate solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane. Wherein, the motor rotating speed of the centrifugal spinning device is 4000 revolutions per minute, the diameter of the spinning hole is 0.8mm, the spinning interval of the centrifugal spinning is 50cm, and the spinning temperature of the centrifugal spinning is 100 ℃. And (3) ejecting the tetraethyl silicate solution from a spinning hole of the centrifugal spinning device by utilizing the centrifugal force generated by the centrifugal spinning device in a high-speed rotation state, wherein the ejected tetraethyl silicate solution is stretched in the jet flow movement process, and the solvent in the tetraethyl silicate solution is volatilized under the action of hot air.
And thirdly, immersing the two-dimensional fiber membrane in a polyvinyl butyral-ethanol solution, taking out, drying, stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel. Wherein the sintering temperature is 1260 ℃ and maintained for 12 hours. After the organic components and residues in the fiber are removed by sintering, the average diameter of the fiber after sintering is obviously reduced.
Example 4
Step one, cellulose triacetate powder is dried for half a day. 1 g of cellulose triacetate powder was dissolved in a mixed solution of 50ml of absolute ethanol and 50ml of 1, 4-dioxane solution, and stirred at 60℃for 3 hours to obtain a homogeneous solution, i.e., a cellulose triacetate solution, in which the concentration of cellulose triacetate was 10mg/cm 3 。
And step two, performing centrifugal spinning on the cellulose triacetate solution through a centrifugal spinning device, and spraying the cellulose triacetate solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane. Wherein, the motor rotation speed of the centrifugal spinning device is 2500 rpm, the diameter of the spinning hole is 1mm, the spinning interval of the centrifugal spinning is 35cm, and the spinning temperature of the centrifugal spinning is 140 ℃. And (3) spraying the cellulose triacetate solution from a spinning hole of the centrifugal spinning device by utilizing the centrifugal force generated by the centrifugal spinning device in a high-speed rotation state, wherein the sprayed cellulose triacetate solution is stretched in the jet flow movement process, and the solvent in the cellulose triacetate solution is volatilized under the action of hot air.
And thirdly, immersing the two-dimensional fiber membrane in a polyvinyl butyral-ethanol solution, taking out, drying, stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel. Wherein the sintering temperature is 1300 ℃, and the sintering time is 12 hours. After the organic components and residues in the fiber are removed by sintering, the average diameter of the fiber after sintering is obviously reduced.
Example 5
And secondly, dissolving 10g of sodium alginate and 10g of water-soluble chitosan in 100ml of deionized water to prepare a solution containing 10wt.% of sodium alginate and chitosan, and then mixing the solution with the silicate solution of the example 1 according to the volume ratio of 1:2, and vigorously stirring the mixture for 2 hours at 40 ℃ to obtain a mixed solution of silicate, sodium alginate and chitosan.
And step two, carrying out centrifugal spinning on the mixed solution through a centrifugal spinning device, and spraying the mixed solution onto a collecting surface of a collecting mechanism to prepare the two-dimensional fiber membrane. Wherein, the motor rotating speed of the centrifugal spinning device is 3500 revolutions
And/min, wherein the diameter of the spinning hole is 0.8mm, the spinning interval of centrifugal spinning is 45cm, and the spinning temperature of the centrifugal spinning is 185 ℃. And (3) ejecting the mixture solution from a spinning hole of the centrifugal spinning device by utilizing the centrifugal force generated by the centrifugal spinning device in a high-speed rotation state, wherein the ejected mixture solution is stretched in the jet flow movement process, and the solvent in the mixture solution is volatilized under the action of hot air.
And thirdly, immersing the two-dimensional fiber membrane in a polyvinyl alcohol-ethanol solution, taking out, drying, stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel. Wherein the sintering temperature is 1500
At c and held for 12 hours. After the organic components and residues in the fiber are removed by sintering, the average diameter of the fiber after sintering is obviously reduced.
Test examples
The test examples examined the properties of the products of examples 1-3, and the results were as follows:
the foregoing has shown and described the basic principles, principal features and advantages of the application. It will be understood by those skilled in the art that the present application is not limited to the foregoing embodiments, which have been described in the foregoing embodiments and description merely illustrates the principles of the application, and various changes and modifications may be made therein without departing from the spirit and scope of the application, the scope of which is defined in the appended claims, specification and their equivalents.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present application and not for limiting the scope of the present application, and although the present application has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present application may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present application.
Claims (10)
1. The preparation method of the centrifugal spinning ceramic fiber aerogel is characterized by comprising the following steps of:
providing a spinnable solution;
carrying out centrifugal spinning on the spinnable solution through a centrifugal spinning device, and spraying the spinnable solution onto a collecting surface of a collecting mechanism to prepare a two-dimensional fiber membrane;
and immersing the two-dimensional fiber membrane in a polymer-ethanol solution, taking out, drying, stacking into a three-dimensional structure, and sintering to obtain the ceramic fiber aerogel.
2. The method of claim 1, wherein,
the spinnable solution comprises any one or a combination of a plurality of silicate solutions, nanocellulose solutions, sodium alginate solutions and chitosan solutions.
3. The method of claim 2, wherein,
the solvent of the silicate solution comprises one or a combination of more of ethanol, hydrochloric acid, ethyl orthosilicate and N, N-dimethylformamide.
4. The method of claim 1, wherein,
the concentration of the spinnable solution is 1.0-15.0wt%.
5. The method of claim 1, wherein,
the rotating speed of the motor of the centrifugal spinning device is 2000-4000 revolutions per minute, and the diameter of the spinneret orifice is 0.1-1mm.
6. The method of claim 1, wherein,
the spinning interval of centrifugal spinning is 30-50cm;
the spinning temperature of the centrifugal spinning is 0-185 ℃.
7. The method of claim 1, wherein,
the sintering temperature is 200-1500 ℃, and the sintering time is kept for 12 hours.
8. The method of claim 1, wherein,
the polymer of the polymer-ethanol solution comprises at least one of PVA, PVB, PVDF.
9. A centrifugal spinning apparatus applying the production method according to any one of claims 1 to 8, characterized by comprising:
a housing having an air inlet;
the rotary cup is arranged in the shell, the side wall of the rotary cup is provided with a spinning hole, and the rotary cup is used for containing polymer solution;
the motor is arranged in the shell and connected with the rotating cup, and the motor is used for driving the rotating cup to rotate;
the collecting mechanism is arranged in the shell and surrounds the periphery of the rotating cup, and the collecting mechanism is used for forming a two-dimensional fiber film;
a filling mechanism disposed within the housing, the filling mechanism defining a filling cavity, a bottom wall of the filling cavity having a filling port facing a top opening of the rotor, the filling mechanism for collecting polymer solution into the filling cavity and supplying the polymer solution within the filling cavity to the rotor;
the heat preservation mechanism is arranged in the shell, is arranged on the outer wall of the rotating cup and the outer wall of the filling mechanism, and is used for carrying out heat preservation and heating on the polymer solution in the rotating cup and the filling cavity;
the heating mechanism is arranged outside the shell and at the air inlet, and is used for adjusting the air inlet temperature at the air inlet;
the power supply mechanism is arranged outside the shell, the power supply mechanism is connected with the motor, the heat preservation mechanism and the heating mechanism, the positive electrode of the power supply mechanism is inserted into the polymer solution in the filling cavity, the negative electrode of the power supply mechanism is connected with the collecting mechanism which is grounded, and the power supply mechanism is used for providing power.
10. Use of the centrifugally spun ceramic fiber aerogel produced by the production process of any one of claims 1 to 8 as a thermal insulation material.
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| CN115142154A (en) * | 2022-07-26 | 2022-10-04 | 西安交通大学 | Silicon dioxide fiber aerogel, preparation method and modification method thereof |
| CN115161879A (en) * | 2022-07-12 | 2022-10-11 | 广东职业技术学院 | Method for preparing polyvinyl butyral micro-nano fiber through rotor centrifugal spinning and application |
| CN218842422U (en) * | 2022-07-12 | 2023-04-11 | 广东职业技术学院 | Rotor centrifugal spinning experimental device |
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