CN109758988B - C-Al2O3-B4Preparation method of C composite aerogel - Google Patents
C-Al2O3-B4Preparation method of C composite aerogel Download PDFInfo
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Abstract
The invention relates to C-Al2O3‑B4A preparation method of C composite aerogel belongs to the technical field of composite material preparation processes. The method comprises the steps of uniformly stirring aluminum chloride crystals, water and ethanol to obtain a clear faint yellow aluminum chloride crystal hydrolysis solution, adding a preferred boron source, citric acid, formaldehyde, resorcinol, water, ethanol, propylene oxide and a reaction catalyst into the solution, and uniformly stirring to obtain C-Al2O3‑B4C, compounding the aerogel sol solution, and standing for gelation. Then processing the sample by adopting a supercritical drying technology, and finally carrying out high-temperature heat treatment on the sample to finally obtain the blocky C-Al2O3‑B4C, composite aerogel. C-Al prepared by the invention2O3‑B4The C composite aerogel has the advantages of simple and easily-operated process, rich and simple raw materials, high specific area, low density, low thermal conductivity and the like, can effectively solve the defect of low strength of the aerogel, and has good application prospect and unlimited potential in the aspect of high-temperature heat insulation materials with the temperature of more than 1200 ℃.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic nano materials with high-temperature heat insulation characteristics, and relates to a massive C-Al2O3-B4C, a preparation method of the composite aerogel.
Background
With the progress of science and technology, high-temperature heat treatment technology is required in more and more fields, however, most of heat preservation and insulation materials used in the industry are traditional heat insulation materials such as inorganic fiber felts, porous ceramic plates and alumina refractory bricks, the heat preservation and insulation effect is poor, and the heat conductivity is rapidly improved along with the increase of the use temperature. Aerogel material phase to phase transferThe material has great advantages in heat insulation, is a new generation of high-efficiency energy-saving heat insulation material, and can greatly reduce energy consumption in the production process. At present, in the field of high-temperature heat insulation, oxide aerogel is used more, but the strength is low, and the high-temperature stability is poor; carbon aerogel has very remarkable heat insulating property in a vacuum environment, but is easily oxidized in an aerobic environment and cannot exhibit the heat insulating property. Thus, C-Al2O3-B4The C composite aerogel combines the advantages of oxide aerogel and carbon aerogel, and is relative to pure Al2O3Aerogel and carbon aerogel have more in the performance breakthrough, not only can solve oxide aerogel high temperature stability poor and carbon aerogel easily oxidized problem under aerobic environment effectively, and great structural strength makes it also have huge application prospect outside the high temperature thermal-insulated field moreover.
Disclosure of Invention
The invention aims to provide a C-Al heat insulation type high-temperature resistant aerogel with higher strength and high temperature resistance of over 1200 ℃ in order to overcome the defects of lower strength, poor high-temperature thermal stability and the like of the oxide aerogel researched at present2O3-B4C, a preparation method of the composite aerogel.
The technical scheme of the invention is as follows: C-Al2O3-B4The preparation method of the C composite aerogel comprises the following specific steps:
(1) uniformly stirring the aluminum chloride crystal, water and ethanol to obtain a clear aluminum chloride crystal hydrolysis solution;
(2) adding formaldehyde, resorcinol, propylene oxide and a reaction catalyst into the aluminum chloride crystal hydrolysis solution, and uniformly stirring to obtain a solution A;
(3) a boron source, a reaction catalyst, deionized water and absolute ethyl alcohol are mixed according to a molar ratio of 1: (0.005-0.03): (20-60): (8-25) after ultrasonic dispersion, heating and uniformly stirring to obtain a boron source hydrolysis solution;
(4) adding formaldehyde, resorcinol and a network forming agent into the boron source hydrolysis solution, and uniformly stirring to obtain a solution B;
(5) adding the solution B into the solution A in the step (2), and continuously stirring to obtain C-Al2O3-B4C, compounding aerogel sol solution;
(6) the C-Al obtained in the step (5)2O3-B4Pouring the composite aerogel sol solution into a mold to react until gel is formed, and putting the gel into an oven for aging treatment;
(7) adding absolute ethyl alcohol into the gel obtained in the step (6) for solvent replacement;
(8) performing CO treatment on the composite wet gel subjected to solvent replacement in the step (7)2Supercritical drying treatment in which CO2Supercritical drying method using CO2Under the protection of gas, controlling the reaction temperature to be 45-50 ℃, the pressure of a high-pressure reaction kettle to be 10-12 MPa, and the reaction time to be 1-2 d;
(9) heating the sample treated in the step (8) to 1350-1600 ℃ at a heating rate of 2-4 ℃/min under the protection of inert atmosphere, and carrying out heat treatment for 5-10 hours to finally obtain C-Al2O3-B4C, composite aerogel.
Preferably, in the step (1), the molar ratio of water to ethanol is 1: (0.2-5), and controlling the mass concentration of the aluminum chloride crystal hydrolysis solution to be 15-20%.
Preferably, in step (2), resorcinol: formaldehyde: aluminum chloride crystal: propylene oxide: the molar ratio of the reaction catalyst is 1: 2: (1-2): (7-15): (0.002-0.02).
Preferably, the reaction catalyst in step (2) and step (3) is one of anhydrous sodium carbonate or sodium hydroxide.
The heating and stirring temperature in the step (3) is preferably 40 to 50 ℃.
Preferably, the network forming agent in the step (4) is one of anhydrous citric acid, citric acid monohydrate or sodium citrate.
Preferably, in the step (4), resorcinol and formaldehyde: a boron source: the molar ratio of the network former is 1: 2: (0.5-2): (0.5-2).
Preferably, the molar ratio of the aluminum chloride in the solution A to the boron source in the solution B in the step (5) is 1: (0.5 to 2)
Preferably, the temperature of the oven in the step (6) is 40-70 ℃, and the aging is carried out for 1-2 d; and (4) replacing the solvent in the step (7) once every 10-12 h, wherein the replacement is performed 3-6 times in total.
Preferably, the inert atmosphere in step (9) is one of helium or argon.
Has the advantages that:
(1) the process is simple, and the raw materials are low in price and easy to obtain. The method adopts cheap and easily-obtained inorganic salt as an aluminum source, uses boric acid or boron oxide as a boron source, utilizes a sol-gel method combined with a supercritical drying technology, and has simple and easily repeated process operation.
(2) Excellent performance and wide application range. C-Al compared to conventional oxide aerogel materials2O3-B4The C composite aerogel has excellent performances of low density, high strength, low thermal conductivity and the like. At the same time, C-Al2O3-B4The C composite aerogel also has excellent performances such as high structural strength, high-temperature physical and chemical property stability and the like, and can be widely applied to the fields of refractory materials, engineering ceramics, aerospace and the like.
Drawings
FIG. 1 shows C-Al prepared in example 12O3-B4And C, a real photograph of the composite aerogel material.
Detailed Description
Example 1
1mol of aluminum chloride crystal, 10mol of deionized water and 6mol of absolute ethyl alcohol are fully and uniformly stirred until the solution is a faint yellow clear aluminum chloride crystal hydrolysis solution with the mass concentration of 19.11%. Then, 1mol of resorcinol, 2mol of formaldehyde, 0.002mol of anhydrous sodium carbonate as a reaction catalyst and 7mol of propylene oxide as a network forming agent are added into the hydrolysis solution, and the mixture is fully and uniformly stirred to obtain a solution A. 0.5mol of boric acid, 0.0025mol of anhydrous sodium carbonate as a reaction catalyst, 10mol of deionized water and 4mol of anhydrous ethanol are ultrasonically dispersed uniformly, and the mixture is heated and stirred at 40 ℃ to obtain a clear solution. Then, 1mol of resorcinol, 2mol of formaldehyde and 0.5mol of anhydrous citric acid as a network forming agent are added into the solution and stirred uniformly to obtain a solution B. Pouring the solution B into the solution A, fully mixing, and continuously stirring for 30min until the solution is completely uniform, thereby obtaining C-Al2O3-B4And C, pouring the composite aerogel sol solution into a mold, and waiting for gelation. The gel time is about 8h at room temperature, the gel is put into a 40 ℃ oven for high-temperature aging for 2d after being gelled, so as to be fully reacted, and then the ethanol is used as an aging liquid to replace the impurity ions in the wet gel for 3 times, and each time is 12 h. Then adding C-Al2O3-B4Placing the C composite wet gel into a high-temperature high-pressure kettle, and utilizing CO2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 10MPa, the temperature is controlled at 45 ℃, and the supercritical drying time is 1 d. Finally, heating the sample to 1350 ℃ at the heating rate of 2 ℃/min under the protection of helium atmosphere, keeping the temperature for 5 hours, and cooling to room temperature to obtain C-Al2O3-B4C, composite aerogel. The characterization shows that: the prepared C-Al2O3-B4The specific surface area of the C composite aerogel is 402m2(iv)/g, compressive strength is calculated as 25% thickness deflection, compressive strength is 1776 kPa. Prepared C-Al2O3-B4A photomicrograph of the composite aerogel material is shown in fig. 1.
Example 2
1mol of aluminum chloride crystal, 11mol of deionized water and 7mol of absolute ethyl alcohol are fully and uniformly stirred until the solution is a faint yellow clear aluminum chloride crystal hydrolysis solution with the mass concentration of 17.50%. Then, 1mol of resorcinol, 2mol of formaldehyde, 0.002mol of anhydrous sodium carbonate as a reaction catalyst and 7mol of propylene oxide as a network forming agent are added into the hydrolysis solution, and the mixture is fully and uniformly stirred to obtain a solution A. 2mol of boric acid, 0.06mol of reaction catalyst anhydrous sodium carbonate, 120mol of deionized water and 50mol of anhydrous ethanol are ultrasonically dispersed uniformly, and the clear solution is obtained by heating and stirring at 40 ℃. Then adding 1mol of resorcinol, 2mol of formaldehyde and 2mol of network forming agent anhydrous citric acid into the solution, and uniformly stirring to obtain a solution B. Pouring the solution B into the solution A, fully mixing, and continuously stirring for 30min until the solution is completely uniform, thereby obtaining C-Al2O3-B4And C, pouring the composite aerogel sol solution into a mold, and waiting for gelation. The gel time is about 8h at room temperature, the gel is put into a 70 ℃ oven for high-temperature aging for 1d after being gelled, and then the gel is fully reactedThen, ethanol is used as an aging solution to replace impurity ions in the wet gel for 4 times, and each time lasts for 12 hours. Then adding C-Al2O3-B4Placing the C composite wet gel into a high-temperature high-pressure kettle, and utilizing CO2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 12MPa, the temperature is controlled at 50 ℃, and the supercritical drying time is 2 d. Finally, heating the sample to 1400 ℃ at a heating rate of 3 ℃/min under the protection of argon atmosphere, keeping the temperature for 6 hours, and cooling to room temperature to obtain C-Al2O3-B4C, composite aerogel. The characterization shows that: the prepared C-Al2O3-B4The specific surface area of the C composite aerogel is 375m2(iv)/g, compressive strength is calculated as 25% thickness deflection, compressive strength is 2142 kPa.
Example 3
2mol of aluminum chloride crystal, 20mol of deionized water and 16mol of absolute ethyl alcohol are fully and uniformly stirred until the solution is a faint yellow clear aluminum chloride crystal hydrolysis solution with the mass concentration of 16.87%. Then, 1mol of resorcinol, 2mol of formaldehyde, 0.002mol of anhydrous sodium carbonate as a reaction catalyst and 7mol of propylene oxide as a network forming agent are added into the hydrolysis solution, and the mixture is fully and uniformly stirred to obtain a solution A. 1mol of boric acid, 0.005mol of anhydrous sodium carbonate serving as a reaction catalyst, 20mol of deionized water and 8mol of anhydrous ethanol are ultrasonically dispersed uniformly, and the mixture is heated and stirred at 40 ℃ to obtain a clear solution. Then adding 1mol of resorcinol, 2mol of formaldehyde and 1mol of network forming agent anhydrous citric acid into the solution, and uniformly stirring to obtain a solution B. Pouring the solution B into the solution A, fully mixing, and continuously stirring for 30min until the solution is completely uniform, thereby obtaining C-Al2O3-B4And C, pouring the composite aerogel sol solution into a mold, and waiting for gelation. The gel time is about 8h at room temperature, the gel is put into a 50 ℃ oven for high-temperature aging for 2d after being gelled, so as to be fully reacted, and then the ethanol is used as an aging liquid to replace the impurity ions in the wet gel for 5 times, and each time is 12 h. Then adding C-Al2O3-B4Placing the C composite wet gel into a high-temperature high-pressure kettle, and utilizing CO2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 11MPa, and the temperature is controlled at 50 DEG CThe supercritical drying time was 1 d. Finally, heating the sample to 1450 ℃ at the heating rate of 4 ℃/min under the protection of argon atmosphere, keeping the temperature for 7 hours, and cooling to room temperature to obtain C-Al2O3-B4C, composite aerogel. The characterization shows that: the prepared C-Al2O3-B4The specific surface area of the C composite aerogel is 309m2(iv)/g, compressive strength is calculated as 25% thickness deflection, compressive strength is 2890 kPa.
Example 4
2mol of aluminum chloride crystal, 24mol of deionized water and 18mol of absolute ethyl alcohol are fully and uniformly stirred until the solution is a faint yellow clear aluminum chloride crystal hydrolysis solution with the mass concentration of 15.29%. Then, 1mol of resorcinol, 2mol of formaldehyde, 0.02mol of anhydrous sodium carbonate as a reaction catalyst and 15mol of propylene oxide as a network forming agent are added into the hydrolysis solution, and the mixture is fully and uniformly stirred to obtain a solution A. 2mol of boric acid, 0.06mol of reaction catalyst anhydrous sodium carbonate, 120mol of deionized water and 50mol of anhydrous ethanol are ultrasonically dispersed uniformly, and the clear solution is obtained by heating and stirring at 40 ℃. Then, 1mol of resorcinol, 2mol of formaldehyde and 2mol of sodium citrate as a network forming agent are added into the solution and stirred uniformly to obtain a solution B. Pouring the solution B into the solution A, fully mixing, and continuously stirring for 30min until the solution is completely uniform, thereby obtaining C-Al2O3-B4And C, pouring the composite aerogel sol solution into a mold, and waiting for gelation. The gel time is about 8h at room temperature, the gel is put into a 60 ℃ oven for high-temperature aging for 1d after being gelled, so that the gel is fully reacted, and then the ethanol is used as an aging liquid to replace impurity ions in the wet gel for 6 times, and each time is 12 h. Then adding C-Al2O3-B4Placing the C composite wet gel into a high-temperature high-pressure kettle, and utilizing CO2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 12MPa, the temperature is controlled at 50 ℃, and the supercritical drying time is 2 d. Finally, heating the sample to 1600 ℃ at a heating rate of 4 ℃/min under the protection of argon atmosphere, keeping the temperature for 10 hours, and cooling to room temperature to obtain C-Al2O3-B4C, composite aerogel. The characterization shows that: the prepared C-Al2O3-B4C compositeThe aerogel specific surface area is 218m2(iv)/g, compressive strength is calculated as 25% thickness deflection, and compressive strength is 3489 kPa.
Example 5
1mol of aluminum chloride crystal, 12mol of deionized water and 8mol of absolute ethyl alcohol are fully and uniformly stirred until the solution is a faint yellow clear aluminum chloride crystal hydrolysis solution with the mass concentration of 16.14%. Then, 1mol of resorcinol, 2mol of formaldehyde, 0.01mol of reaction catalyst sodium hydroxide and 10mol of network forming agent propylene oxide are added into the hydrolysis solution, and the mixture is fully and uniformly stirred to obtain solution A. 1.5mol of boric acid, 0.03mol of reaction catalyst sodium hydroxide, 60mol of deionized water and 25mol of absolute ethyl alcohol are ultrasonically dispersed uniformly, and are heated and stirred at 50 ℃ to obtain a clear solution. Then adding 1mol of resorcinol, 2mol of formaldehyde and 1.5mol of network forming agent citric acid monohydrate into the solution, and uniformly stirring to obtain a solution B. Pouring the solution B into the solution A, fully mixing, and continuously stirring for 30min until the solution is completely uniform, thereby obtaining C-Al2O3-B4And C, pouring the composite aerogel sol solution into a mold, and waiting for gelation. The gel time is about 8h at room temperature, the gel is put into a 70 ℃ oven for high-temperature aging for 1d after being gelled, so as to be fully reacted, and then the ethanol is used as an aging liquid to replace the impurity ions in the wet gel for 5 times, and each time is 10 h. Then adding C-Al2O3-B4Placing the C composite wet gel into a high-temperature high-pressure kettle, and utilizing CO2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 12MPa, the temperature is controlled at 47 ℃, and the supercritical drying time is 36 h. Finally, heating the sample to 1500 ℃ at the heating rate of 3 ℃/min under the protection of argon atmosphere, keeping the temperature for 8 hours, and cooling to room temperature to obtain C-Al2O3-B4C, composite aerogel. The characterization shows that: the prepared C-Al2O3-B4The specific surface area of the C composite aerogel is 296m2(iv)/g, compressive strength is calculated as 25% thickness deflection, and the compressive strength is 3008 kPa.
Claims (6)
1. C-Al2O3-B4The preparation method of the C composite aerogel comprises the following specific stepsThe following:
(1) uniformly stirring the aluminum chloride crystal, water and ethanol to obtain a clear aluminum chloride crystal hydrolysis solution;
(2) adding formaldehyde, resorcinol, propylene oxide and a reaction catalyst into the aluminum chloride crystal hydrolysis solution, and uniformly stirring to obtain a solution A; wherein the resorcinol: formaldehyde: aluminum chloride crystal: propylene oxide: the molar ratio of the reaction catalyst is 1: 2: (1-2): (7-15): (0.002-0.02);
(3) a boron source, a reaction catalyst, deionized water and absolute ethyl alcohol are mixed according to a molar ratio of 1: (0.005-0.03): (20-60): (8-25) after ultrasonic dispersion, heating and uniformly stirring to obtain a boron source hydrolysis solution;
(4) adding formaldehyde, resorcinol and a network forming agent into the boron source hydrolysis solution, and uniformly stirring to obtain a solution B; wherein the ratio of resorcinol to formaldehyde: a boron source: the molar ratio of the network former is 1: 2: (0.5-2): (0.5 to 2);
(5) adding the solution B into the solution A in the step (2), and continuously stirring to obtain C-Al2O3-B4C, compounding aerogel sol solution; wherein the molar ratio of the aluminum chloride of the solution A to the boron source of the solution B is 1: (0.5 to 2);
(6) the C-Al obtained in the step (5)2O3-B4Pouring the composite aerogel sol solution into a mold to react until gel is formed, and putting the gel into an oven for aging treatment;
(7) adding absolute ethyl alcohol into the gel obtained in the step (6) for solvent replacement;
(8) performing CO treatment on the composite wet gel subjected to solvent replacement in the step (7)2Supercritical drying treatment in which CO2Supercritical drying method using CO2Under the protection of gas, controlling the reaction temperature to be 45-50 ℃, the pressure of a high-pressure reaction kettle to be 10-12 MPa, and the reaction time to be 1-2 d;
(9) heating the sample treated in the step (8) to 1350-1600 ℃ at a heating rate of 2-4 ℃/min under the protection of inert atmosphere, and carrying out heat treatment for 5-10 hours to finally obtain C-Al2O3-B4C, compounding aerogel;
wherein, the reaction catalyst in the step (2) and the step (3) is one of anhydrous sodium carbonate or sodium hydroxide; the boron source in the step (2) is boric acid.
2. The method according to claim 1, wherein the molar ratio of water to ethanol in step (1) is 1: (0.2-5), and controlling the mass concentration of the aluminum chloride crystal hydrolysis solution to be 15-20%.
3. The method according to claim 1, wherein the heating and stirring temperature in the step (3) is 40 ℃ to 50 ℃.
4. The method of claim 1, wherein the network forming agent in the step (4) is one of anhydrous citric acid, citric acid monohydrate or sodium citrate.
5. The preparation method according to claim 1, wherein the oven temperature in the step (6) is 40 ℃ to 70 ℃, and the aging is carried out for 1 to 2 days; and (4) replacing the solvent in the step (7) once every 10-12 h, wherein the replacement is performed 3-6 times in total.
6. The method according to claim 1, wherein the inert gas atmosphere in the step (9) is one of helium gas and argon gas.
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| CN110711543A (en) * | 2019-11-07 | 2020-01-21 | 南京工业大学 | Preparation method of fiber composite boron carbide-alumina aerogel material |
| CN111848140B (en) * | 2020-07-13 | 2022-04-29 | 航天特种材料及工艺技术研究所 | Alumina nanowire aerogel thermal insulation material and preparation method thereof |
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