CN110284318B - Preparation method of low-thermal-conductivity TiO2/SiC-Al2O3 aerogel-SiO 2 fibrofelt composite material - Google Patents

Preparation method of low-thermal-conductivity TiO2/SiC-Al2O3 aerogel-SiO 2 fibrofelt composite material Download PDF

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CN110284318B
CN110284318B CN201910627463.3A CN201910627463A CN110284318B CN 110284318 B CN110284318 B CN 110284318B CN 201910627463 A CN201910627463 A CN 201910627463A CN 110284318 B CN110284318 B CN 110284318B
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tio
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aerogel
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CN110284318A (en
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毕于铁
朱家艺
任洪波
温尚艳
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Southwest University of Science and Technology
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic System; Aluminates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof

Abstract

The invention discloses a low thermal conductivity TiO2/SiC‑Al2O3aerogel-SiO2A method of making a fiber mat composite comprising: mixing aluminum nitrate nonahydrate, water and alcohol, and adding TiO2Or SiC, stirring for 1-2 h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; injecting the mixed sol into SiO2Waiting for gelation in the fibrofelt for 10-30 min, aging for 24h after gelation, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2/SiC‑Al2O3aerogel-SiO2A fiber mat composite. The TiO being2/SiC‑Al2O3aerogel-SiO2The fiber mat composite has low thermal conductivity; can be widely applied to the production and life of the people, such as the fields of heat preservation and insulation, aerospace and the like. The method has the advantages of simple experimental process and low raw material cost, and is expected to realize industrialization.

Description

Low thermal conductivity TiO2/SiC-Al2O3aerogel-SiO2Preparation method of fibrofelt composite material
Technical Field
The invention belongs to the technical field of composite preparation, and particularly relates to TiO2/SiC-Al2O3aerogel-SiO2A fiber felt composite material, a preparation method and application thereof.
Background
The heat-insulating material is widely applied to the fields of precision electronic industry, aerospace, industrial building and the like. The heat insulating material is selected from porous heat insulating material, layered heat insulating material, powdered heat insulating material, and fibrous heat insulating material. Wherein, the fibrous heat-insulating material has the advantages of high temperature resistance, large specific heat capacity, low cost and the like, and simultaneously, SiO2The fiber has good application in the field of heat insulation due to good biocompatibility, chemical stability, high temperature resistance and the like, and is always the preferred heat insulation materialAnd (5) feeding. However, SiO2The thermal conductivity of the fiber is still high and is difficult to meet the application under the harsh condition, so the fiber is applied to SiO2The thermal conductivity of the fiber can be effectively reduced by introducing a large amount of nano-scale pores into the fiber. Al (Al)2O3The aerogel is nano-porous and has good high-temperature resistance, heat preservation and heat insulation performance, so the aerogel has wide application prospects in the fields of high-temperature catalysis, heat preservation and heat insulation, aerospace and the like, but the low mechanical property limits the application of the aerogel in practice. Mixing Al2O3Aerogel as a nanoporous filler filled into SiO2In the fiber felt, Al can be improved2O3The mechanical property of the aerogel can also reduce SiO2Thermal conductivity of the fiber mat. Mixing Al2O3Aerogel filled with SiO2In the fiber felt, not only can reduce SiO2Solid phase heat transfer and air heat convection between fibers, but at higher temperatures, SiO2The heat radiation of the fiber felt is strong, and Al is added2O3Aerogel cannot suppress heat radiation at high temperature, and at the same time, Al2O3Aerogel can also generate crystal form transformation at high temperature to cause failure, and TiO is used2SiC and Al2O3aerogel-SiO2The heat radiation can be reduced and Al can be inhibited when the fiber felt composite material is compounded2O3The aerogel generates crystal form transformation at high temperature.
Therefore, it is necessary and meaningful to research and develop a heat preservation and insulation material with simple preparation method, no toxicity, low thermal conductivity and good environmental stability.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the purpose of the invention, a low thermal conductivity TiO is provided2/SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then addingTiO2Or SiC, stirring for 1-2 h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol;
step two, injecting the mixed sol into SiO2Waiting for gelation in the fibrofelt for 10-30 min, aging for 24h after gelation, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2/SiC-Al2O3aerogel-SiO2A fiber mat composite.
Preferably, the molar ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.05-0.15: 1-2: 0.4-0.7: 0.5 to 0.6.
Preferably, the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 0.1 to 25 percent of the total molar number.
Preferably, the dosage of the SiC is 0.1-15% of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide.
Preferably, in the second step, the mixed sol and SiO2The mass ratio of the fiber felt is 1-5: 1; the supercritical drying time is 8-12 h.
Preferably, the TiO is2Or pretreating SiC, wherein the pretreatment process comprises the following steps: according to the weight portion, 5-10 portions of TiO2Or adding SiC into 50-100 parts of ethanol, then adding 0.1-0.3 part of dispersing agent, heating to 65-75 ℃, and carrying out ultrasonic treatment for 60-90 min to obtain TiO2A dispersion or a SiC dispersion; taking 10-20 parts of TiO2Adding the dispersion liquid or SiC dispersion liquid, 3-5 parts of salicylic acid and 0.5-2.5 parts of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, then placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, filtering and drying after the treatment is finished to obtain the pretreated TiO2Or SiC.
Preferably, the irradiation dose rate adopted by irradiation is 100-200 kGy/h, the irradiation dose is 400-600 kGy, and the stirring speed is 100-150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1.
Preferably, the method also comprises the step of pretreating the obtained TiO2Or the SiC is processed again, and the process is as follows: according to the weight portion, 10-15 portions of pretreated TiO2Or adding SiC and 0.1-0.5 part of rare earth compound into 8-12 parts of ethanol, and uniformly mixing to obtain a mixed material; placing the ball milling tank filled with the grinding balls and the mixed material in a ball mill for ball milling; cooling the ball-milled sample to room temperature, drying and grinding to obtain the retreated TiO2Or SiC.
Preferably, the grinding balls have the particle sizes of 1mm, 3mm, 5mm and 8mm and the mass ratio of the grinding balls to the grinding balls is 5: 3: 2: 1; the mass ratio of the grinding balls to the mixed materials is 5-8: 1; the rotating disc rotating speed of the ball mill is 250r/min, the revolution and rotation speed ratio is 1: 2, and the ball milling time is 12 hours.
Preferably, the rare earth compound is any one of lanthanum chloride, praseodymium chloride, cerium nitrate and samarium nitrate.
The invention at least comprises the following beneficial effects: TiO of the invention2/SiC-Al2O3aerogel-SiO2The fiber felt composite material is prepared from cheap and easily available aluminum nitrate nonahydrate, water, alcohol and TiO2The TiO is prepared by taking/SiC and epoxypropane as raw materials through a sol-gel method and a supercritical drying process2/SiC-Al2O3aerogel-SiO2The fiber mat composite has low thermal conductivity; TiO of the invention2/SiC-Al2O3aerogel-SiO2The fiber felt composite material can be widely applied to the production and life of the people, such as the fields of heat preservation and insulation, aerospace and the like. Such as TiO2/SiC-Al2O3aerogel-SiO2The fiber felt composite material can be used as a coating material of a conveying pipeline such as petroleum and the like, and is used under the conditions of moisture and easy corrosion. The method has the advantages of simple experimental process and low raw material cost, and is expected to realize industrialization.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 shows TiO of the present invention2/SiC-Al2O3aerogel-SiO2A preparation flow chart of the fiber felt composite material;
FIG. 2 shows TiO compounds prepared in examples 1 to 72-Al2O3aerogel-SiO2Fibrofelt composite and pure TiO2XRD spectrum of (1);
FIG. 3 shows SiC-Al prepared in examples 11 to 152O3aerogel-SiO2XRD spectrogram of the fibrofelt composite material;
FIG. 4 shows TiO prepared in examples 1 to 72-Al2O3aerogel-SiO2Fibrofelt composite and pure TiO2In the IR spectrum of (1), wherein, Al-TiO2-1 represents example 1, Al-TiO2-2 represents example 2, Al-TiO2-3 represents example 3, Al-TiO2-4 represents example 4, Al-TiO2-5 represents example 5, Al-TiO2-6 represents example 6, Al-TiO2-7 represents example 7;
FIG. 5 shows SiC-Al prepared in examples 11 to 152O3aerogel-SiO2Fiber felt composite material, pure SiC, and Al2O3aerogel-SiO2IR spectrum of fiber mat composite, wherein Al-SiC-1 represents example 11, Al-SiC-2 represents example 12; Al-SiC-3 represents example 13, Al-SiC-4 represents example 14; Al-SiC-5 represents example 15;
FIG. 6 shows TiO of the present invention2/SiC-Al2O3aerogel-SiO2Scanning electron micrographs of the fibrofelt composite wherein FIGS. 6a and 6b are TiO prepared according to example 42-Al2O3aerogel-SiO2A fiber mat composite; FIG. 6c is TiO prepared in comparative example 22-Al2O3An aerogel; FIGS. 6d and 6e are SiC-Al prepared in example 122O3aerogel-SiO2Fiber mat composite, FIG. 6f SiC-Al prepared in comparative example 32O3An aerogel;
FIG. 7 shows an embodiment of the present inventionTiO prepared in examples 3 to 52-Al2O3aerogel-SiO2N of fiber felt composite2Desorption-adsorption curve;
FIG. 8 shows SiC-Al prepared in examples 11 to 13 of the present invention2O3aerogel-SiO2N of fiber felt composite2Desorption-adsorption curve;
FIG. 9 shows TiO compounds prepared in examples 1 to 7 of the present invention2-Al2O3aerogel-SiO2The thermal conductivity of the fibrofelt composite material is obtained after the fibrofelt composite material is subjected to heat treatment for 2 hours at different temperatures; wherein a represents no heat treatment, b represents treatment at 300 ℃, and c represents treatment at 600 ℃;
FIG. 10 shows SiC-Al prepared in examples 11 to 15 of the present invention2O3aerogel-SiO2The thermal conductivity of the fibrofelt composite material is obtained after heat treatment at different temperatures; wherein a represents no heat treatment (35 ℃), b represents treatment at 300 ℃, and c represents treatment at 600 ℃;
FIG. 11 shows TiO prepared in example 4 of the present invention2-Al2O3aerogel-SiO2Water contact schematic of the fiber mat composite (measured using a surface tensiometer).
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, aluminum nitrate nonahydrate (Al (NO)3)3.9H2O), water (H)2O) and alcohol (EtOH) are mixed, and then TiO is added2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; followed by the addition of propylene oxideQuickly stirring alkane (PO) for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 0.1 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 2:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 0.5 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 3:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The using amount of the catalyst is 5 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 4:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 10 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 5:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 15 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 6:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 20 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; dried by supercritical dryingThe time is 10 h.
Example 7:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 25 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 8:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 10 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time is 10 h;
TiO added in the step one2Is pretreated TiO2The pretreatment process comprises the following steps: according to the weight portion, 5 portions of TiO2Adding into 50 parts of ethanol, adding 0.1 part of dispersant, heating to 65 ℃, and performing ultrasonic treatment for 60min to obtain TiO2A dispersion liquid; taking 10 parts of TiO2Adding the dispersion, 3 parts of salicylic acid and 1 part of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, filtering and drying to obtain pretreated TiO2(ii) a The irradiation dose rate adopted by the irradiation is 200kGy/h, the irradiation dose is 600kGy, and the stirring speed is 150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1;
TiO prepared in this example2-Al2O3aerogel-SiO2The thermal conductivity of the fibrofelt composite material is tested after heat treatment for 2 hours at 300 ℃ and 600 ℃, respectively, the thermal conductivity at 35 ℃ is 0.019W/(m.K), the thermal conductivity at 300 ℃ is 0.023W/(m.K), and the thermal conductivity at 600 ℃ is 0.027W/(m.K).
Example 9:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 10 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, and agingDissolving for 24h, adding alcohol, performing solvent exchange soaking for 3 times, each for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time is 10 h;
TiO added in the step one2Is pretreated TiO2The pretreatment process comprises the following steps: according to the weight portion, 5 portions of TiO2Adding into 50 parts of ethanol, adding 0.1 part of dispersant, heating to 65 ℃, and performing ultrasonic treatment for 60min to obtain TiO2A dispersion liquid; taking 10 parts of TiO2Adding the dispersion, 3 parts of salicylic acid and 1 part of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, filtering and drying to obtain pretreated TiO2(ii) a 10 portions of pretreated TiO2Adding 0.2 part of praseodymium chloride into 10 parts of ethanol, and uniformly mixing to obtain a mixed material; placing the ball milling tank filled with the grinding balls and the mixed material in a ball mill for ball milling; cooling the ball-milled sample to room temperature, drying and grinding to obtain the retreated TiO2(ii) a The particle size of the grinding balls is 1mm, 3mm, 5mm and 8mm, and the mass ratio of the grinding balls to the grinding balls is 5: 3: 2: 1; the mass ratio of the grinding balls to the mixed materials is 6: 1; the rotating disc rotating speed of the ball mill is 250r/min, the revolution and rotation speed ratio is 1: 2, and the ball milling time is 12 hours; the irradiation dose rate adopted by the irradiation is 200kGy/h, the irradiation dose is 600kGy, and the stirring speed is 150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1.
TiO prepared in this example2-Al2O3aerogel-SiO2The thermal conductivity of the fiber felt composite material is tested after heat treatment for 2 hours at 300 ℃ and 600 ℃, respectively, the thermal conductivity at 35 ℃ is 0.015W/(m.K), the thermal conductivity at 300 ℃ is 0.020W/(m.K), and the thermal conductivity at 600 ℃ is 0.024W/(m.K).
Example 10:
low-thermal-conductivity TiO2-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 10 percent of the total molar number;
step two, injecting the mixed sol into SiO2Waiting for gelling in fiber felt for 20min, aging for 24h, adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time is 10 h;
TiO added in the step one2Is pretreated TiO2The pretreatment process comprises the following steps: according to the weight portion, 5 portions of TiO2Adding into 50 parts of ethanol, adding 0.1 part of dispersant, heating to 65 ℃, and performing ultrasonic treatment for 60min to obtain TiO2A dispersion liquid; taking 10 parts of TiO2Adding the dispersion, 3 parts of salicylic acid and 1 part of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, filtering and drying to obtain pretreated TiO2(ii) a 10 portions of pretreated TiO2Adding 0.2 part of lanthanum chloride into 10 parts of ethanol, and uniformly mixing to obtain a mixed material; placing the ball milling tank filled with the grinding balls and the mixed material in a ball mill for ball milling; cooling the ball-milled sample to room temperature, drying and grinding to obtain the retreated TiO2(ii) a The particle size of the grinding balls is 1mm, 3mm, 5mm and 8mm, and the mass ratio of the grinding balls to the grinding balls is 5: 3: 2: 1; the mass ratio of the grinding balls to the mixed materials is 6: 1; the rotating disc rotating speed of the ball mill is 250r/min, the revolution and rotation speed ratio is 1: 2, and the ball milling time is 12 hours; what is needed isThe irradiation dose rate adopted by the irradiation is 200kGy/h, the irradiation dose is 600kGy, and the stirring speed is 150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1.
TiO prepared in this example2-Al2O3aerogel-SiO2The thermal conductivity of the fiber felt composite material is tested after heat treatment for 2 hours at 300 ℃ and 600 ℃, respectively, the thermal conductivity at 35 ℃ is 0.015W/(m.K), the thermal conductivity at 300 ℃ is 0.021W/(m.K), and the thermal conductivity at 600 ℃ is 0.025W/(m.K).
Comparative example 1:
low-thermal-conductivity Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, aluminum nitrate nonahydrate (Al (NO)3)3.9H2O), water (H)2O) and alcohol (EtOH) are mixed and stirred for 1.5h until the aluminum salt is completely hydrolyzed; then adding Propylene Oxide (PO) and quickly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555;
step two, injecting the mixed sol into SiO2Waiting for gelation in fiber felt for 20min, aging for 24 hr, adding alcohol for solvent exchange soaking for 3 times (24 hr each time), and supercritical drying to obtain Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Comparative example 2:
low-thermal-conductivity TiO2-Al2O3A method of preparing an aerogel composite comprising the steps of:
step one, aluminum nitrate nonahydrate (Al (NO)3)3.9H2O), water (H)2O) and alcohol (EtOH) are mixed, and then TiO is added2Stirring for 1.5h until the aluminum salt is completely hydrolyzed; then adding Propylene Oxide (PO) and quickly stirring for 3min to obtain mixed sol; the aluminum nitrate nonahydrate and the alcoholThe molar ratio of water to propylene oxide is 0.1: 1.5: 0.57: 0.555; the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 10 percent of the total molar number;
step two, waiting for the mixed sol-gel, wherein the gel time is 20min, aging for 24h after the gel, then adding alcohol to perform solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2-Al2O3An aerogel composite; the supercritical drying time was 10 h.
Example 11:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 0.1 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 12:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 0.5 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 13:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 5 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 14:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 10 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 15:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 15 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time was 10 h.
Example 16:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 0.5 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time is 10 h;
the SiC added in the first step is pretreated SiC, and the pretreatment process comprises the following steps: adding 5 parts by weight of SiC into 50 parts by weight of ethanol, then adding 0.1 part by weight of dispersing agent, heating to 65 ℃, and carrying out ultrasonic treatment for 60min to obtain SiC dispersion liquid; adding 10 parts of SiC dispersion liquid, 3 parts of salicylic acid and 1 part of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, then placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, and after the treatment is finished, filtering and drying to obtain pretreated SiC; the irradiation dose rate adopted by the irradiation is 200kGy/h, the irradiation dose is 600kGy, and the stirring speed is 150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1.
SiC-Al prepared in this example2O3aerogel-SiO2The thermal conductivity of the fiber felt composite material was tested after heat treatment at 300 ℃ and 600 ℃ for 2h, respectively, and the thermal conductivity was 0.018W/(m.K) at 35 ℃, 0.020W/(m.K) at 300 ℃ and 0.022W/(m.K) at 600 ℃.
Example 17:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 0.5 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time is 10 h;
the SiC added in the first step is pretreated SiC, and the pretreatment process comprises the following steps: adding 5 parts by weight of SiC into 50 parts by weight of ethanol, then adding 0.1 part by weight of dispersing agent, heating to 65 ℃, and carrying out ultrasonic treatment for 60min to obtain SiC dispersion liquid; adding 10 parts of SiC dispersion liquid, 3 parts of salicylic acid and 1 part of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, then placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, and after the treatment is finished, filtering and drying to obtain pretreated SiC; adding 10 parts of pretreated SiC and 0.2 part of praseodymium chloride into 10 parts of ethanol, and uniformly mixing to obtain a mixed material; placing the ball milling tank filled with the grinding balls and the mixed material in a ball mill for ball milling; cooling the ball-milled sample to room temperature, drying and grinding to obtain the reprocessed SiC; the particle size of the grinding balls is 1mm, 3mm, 5mm and 8mm, and the mass ratio of the grinding balls to the grinding balls is 5: 3: 2: 1; the mass ratio of the grinding balls to the mixed materials is 6: 1; the rotating disc rotating speed of the ball mill is 250r/min, the revolution and rotation speed ratio is 1: 2, and the ball milling time is 12 hours; the irradiation dose rate adopted by the irradiation is 200kGy/h, the irradiation dose is 600kGy, and the stirring speed is 150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1.
SiC-Al prepared in this example2O3aerogel-SiO2The thermal conductivity of the fibrofelt composite material is tested after heat treatment for 2 hours at 300 ℃ and 600 ℃ respectively, and the thermal conductivity at 35 ℃ is 0.014W/(m.K) The thermal conductivity at 300 ℃ was 0.017W/(mK) and the thermal conductivity at 600 ℃ was 0.020W/(mK).
Example 18:
low-thermal-conductivity SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material comprises the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 0.5 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, injecting the mixed sol into SiO2Waiting for gelling in the fibrofelt for 20min, aging for 24h after gelling, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3aerogel-SiO2A fiber mat composite; mixed sol and SiO2The mass ratio of the fiber felt is 2: 1; the supercritical drying time is 10 h;
the SiC added in the first step is pretreated SiC, and the pretreatment process comprises the following steps: adding 5 parts by weight of SiC into 50 parts by weight of ethanol, then adding 0.1 part by weight of dispersing agent, heating to 65 ℃, and carrying out ultrasonic treatment for 60min to obtain SiC dispersion liquid; adding 10 parts of SiC dispersion liquid, 3 parts of salicylic acid and 1 part of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, then placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, and after the treatment is finished, filtering and drying to obtain pretreated SiC; adding 10 parts of pretreated SiC and 0.2 part of lanthanum chloride into 10 parts of ethanol, and uniformly mixing to obtain a mixed material; placing the ball milling tank filled with the grinding balls and the mixed material in a ball mill for ball milling; cooling the ball-milled sample to room temperature, drying and grinding to obtain the reprocessed SiC; the particle size of the grinding balls is 1mm, 3mm, 5mm and 8mm, and the mass ratio of the grinding balls to the grinding balls is 5: 3: 2: 1; the mass ratio of the grinding balls to the mixed materials is 6: 1; the rotating disc rotating speed of the ball mill is 250r/min, the revolution and rotation speed ratio is 1: 2, and the ball milling time is 12 hours; the irradiation dose rate adopted by the irradiation is 200kGy/h, the irradiation dose is 600kGy, and the stirring speed is 150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1.
SiC-Al prepared in this example2O3aerogel-SiO2The thermal conductivity of the fibrofelt composite material is tested after heat treatment for 2 hours at 300 ℃ and 600 ℃, respectively, the thermal conductivity at 35 ℃ is 0.015W/(m.K), the thermal conductivity at 300 ℃ is 0.019W/(m.K), and the thermal conductivity at 600 ℃ is 0.021W/(m.K).
Comparative example 3:
low-thermal-conductivity SiC-Al2O3A method of preparing an aerogel composite comprising the steps of:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, then adding SiC, and stirring for 1.5 hours until aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol; the mol ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.1: 1.5: 0.57: 0.555; the dosage of the SiC is 0.5 percent of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
step two, waiting for the mixed sol-gel, wherein the gel time is 20min, aging for 24h after the gel, then adding alcohol to perform solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain SiC-Al2O3An aerogel composite; the supercritical drying time was 10 h.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.

Claims (4)

1. Low-thermal-conductivity TiO2/SiC-Al2O3aerogel-SiO2The preparation method of the fiber felt composite material is characterized by comprising the following steps:
step one, mixing aluminum nitrate nonahydrate, water and alcohol, and then adding TiO2Or SiC, stirring for 1-2 h until the aluminum salt is completely hydrolyzed; then adding propylene oxide and rapidly stirring for 3min to obtain mixed sol;
step two, injecting the mixed sol into SiO2Waiting for gelation in the fibrofelt for 10-30 min, aging for 24h after gelation, then adding alcohol for solvent exchange soaking for 3 times, each time for 24h, and finally performing supercritical drying to obtain TiO2/SiC-Al2O3aerogel-SiO2A fiber mat composite;
the molar ratio of the aluminum nitrate nonahydrate to the alcohol to the water to the propylene oxide is 0.05-0.15: 1-2: 0.4-0.7: 0.5 to 0.6;
the TiO is2The dosage of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide accounts for 0.1 to 25 percent of the total molar number;
the dosage of the SiC is 0.1-15% of the total mole number of the aluminum nitrate nonahydrate, the alcohol, the water and the propylene oxide;
in the second step, the mixed sol and SiO2The mass ratio of the fiber felt is 1-5: 1; the supercritical drying time is 8-12 h;
subjecting the TiO to a reaction2Or pretreating SiC, wherein the pretreatment process comprises the following steps: according to the weight portion, 5-10 portions of TiO2Or adding SiC into 50-100 parts of ethanol, then adding 0.1-0.3 part of dispersing agent, heating to 65-75 ℃, and carrying out ultrasonic treatment for 60-90 min to obtain TiO2A dispersion or a SiC dispersion; taking 10-20 parts of TiO2Adding the dispersion liquid or SiC dispersion liquid, 3-5 parts of salicylic acid and 0.5-2.5 parts of betaine into a sealed container, introducing nitrogen into the sealed container to saturate the nitrogen, sealing, then placing the sealed container in an electron accelerator of 2.5MeV and 40mA for irradiation stirring treatment, filtering and drying after the treatment is finished to obtain the pretreated TiO2Or SiC;
the irradiation dose rate adopted by irradiation is 100-200 kGy/h, the irradiation dose is 400-600 kGy, and the stirring speed is 100-150 r/min; the dispersing agent is 1-ethyl-3-methylimidazolium lactic acid and triethanolamine in a weight ratio of 2: 1.
2. The low thermal conductivity TiO of claim 12/SiC-Al2O3aerogel-SiO2The preparation method of the fibrofelt composite material is characterized by further comprising the step of pretreating the obtained TiO2Or the SiC is processed again, and the process is as follows: according to the weight portion, 10-15 portions of pretreated TiO2Or adding SiC and 0.1-0.5 part of rare earth compound into 8-12 parts of ethanol, and uniformly mixing to obtain a mixed material; placing the ball milling tank filled with the grinding balls and the mixed material in a ball mill for ball milling; cooling the ball-milled sample to room temperature, drying and grinding to obtain the retreated TiO2Or SiC.
3. The low thermal conductivity TiO of claim 22/SiC-Al2O3aerogel-SiO2The preparation method of the fibrofelt composite material is characterized in that the particle size of the grinding balls is 1mm, 3mm, 5mm and 8mm, and the mass ratio of the grinding balls to the grinding balls is 5: 3: 2: 1; the mass ratio of the grinding balls to the mixed materials is 5-8: 1; the rotating disc rotating speed of the ball mill is 250r/min, the revolution and rotation speed ratio is 1: 2, and the ball milling time is 12 hours.
4. The low thermal conductivity TiO of claim 22/SiC-Al2O3aerogel-SiO2The preparation method of the fibrofelt composite material is characterized in that the rare earth compound is any one of lanthanum chloride, praseodymium chloride, cerium nitrate and samarium nitrate.
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