CN111348888A - High-temperature-resistant aerogel fiber composite material and preparation method thereof - Google Patents
High-temperature-resistant aerogel fiber composite material and preparation method thereof Download PDFInfo
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- CN111348888A CN111348888A CN202010268429.4A CN202010268429A CN111348888A CN 111348888 A CN111348888 A CN 111348888A CN 202010268429 A CN202010268429 A CN 202010268429A CN 111348888 A CN111348888 A CN 111348888A
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- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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Abstract
Disclosed are a high temperature resistant aerogel fiber composite material and a preparation method thereof, the method comprising: (1) prehydrolysis is carried out on tetramethyl orthosilicate to form silica sol; (2) dissolving a zirconium source in a mixed solvent of ethanol and deionized water; (3) adding formamide into the solution in the step (2) and stirring; (4) adding the silica sol obtained in the step (1) into the solution obtained in the step (3) to generate a mixed sol system; (5) adding a gel initiator into the mixed sol system to form a wet gel block; (6) carrying out solvent replacement on the wet gel block and ethanol; (7) carrying out surface silanization on the displaced wet gel block in an ethanol/tetraethyl orthosilicate solution; (8) immersing basalt fibers in the wet gel block with the silanized surface, standing for aging, rolling and placing in a supercritical reaction kettle; and (9) performing supercritical drying by adopting carbon dioxide to obtain the aerogel composite fiber block.
Description
Technical Field
The invention relates to the technical field of hybrid aerogel inorganic materials, in particular to a high-temperature-resistant aerogel fiber composite material and a preparation method thereof.
Background
Silica aerogel felt is widely accepted and favored by the industry of thermal insulation materials due to good physical and chemical properties and ultralow thermal conductivity as a thermal insulation material. But the application range of the material is greatly limited because the temperature resistance of the material can only reach 600 ℃.
Accordingly, there is a need in the art for a solution for preparing high temperature resistant aerogel composites.
Disclosure of Invention
In one aspect of the present invention, a method for preparing a high temperature resistant aerogel fiber composite is provided, comprising the steps of:
(1) prehydrolysis of tetra-methyl orthosilicate (TEOS) to form Silica (SiO)2) Sol;
(2) dissolving a zirconium source in a mixed solvent of ethanol (EtOH) and deionized water;
(3) adding Formamide (FA) into the solution generated in the step (2) and stirring;
(4) adding the silica sol generated in the step (1) into the solution generated in the step (3) to generate a mixed sol system;
(5) adding a gel initiator into the mixed sol system generated in the step (4) to generate sol-gel transformation to form a wet gel block;
(6) carrying out solvent replacement on the wet gel block generated in the step (5) and ethanol;
(7) carrying out surface silanization on the wet gel block subjected to solvent replacement in the step (6) in an ethanol/tetraethyl orthosilicate (EtOH/TEOS) solution;
(8) immersing basalt fibers into the wet gel block subjected to surface silanization in the step (7), standing for aging, then rolling and placing in a supercritical reaction kettle; and
(9) and (3) performing supercritical drying on the material in the supercritical reaction kettle by adopting carbon dioxide to obtain the aerogel composite fiber block.
In another aspect of the present invention, there is provided a high temperature resistant aerogel fiber composite, which is prepared according to the preparation method of the high temperature resistant aerogel fiber composite of any one embodiment of the present invention.
The novel hybrid aerogel material formed by doping zirconium dioxide (ZrO 2) and silicon dioxide (SiO 2), sol-gel and compounding with basalt fibers can resist the high temperature of 1100 ℃, and the application of the aerogel material is greatly expanded.
Drawings
FIG. 1 illustrates a method of making a high temperature resistant aerogel fiber composite according to embodiments of the present disclosure.
Detailed Description
Embodiments of the present invention are described in detail below with reference to the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention to those skilled in the art. It will be apparent, however, to one skilled in the art that the present invention may be practiced without some of these specific details. Furthermore, it should be understood that the invention is not limited to the specific embodiments described. Rather, it is contemplated that the invention may be practiced with any combination of the following features and elements, whether or not they relate to different embodiments. Thus, the following aspects, features, embodiments and advantages are merely illustrative and should not be considered elements or limitations of the claims except where explicitly recited in a claim. The meaning of each term referred to in this specification is generally a meaning commonly understood in the art or a meaning normally understood by those skilled in the art after reading this specification. The terms "comprising" and "including" in this specification are open-ended, i.e., may include additional elements not already mentioned in addition to the elements already mentioned. The specific values of the contents of the components described in the present specification are only used to indicate a proportional relationship between the contents of the components, and are not used to limit the contents of the components to any absolute values. Specific values for the amounts of ingredients and specific values for process conditions described in this specification are intended to be inclusive of one another, e.g., 15% inclusive, and are not intended to be limiting to a precise value.
Referring now to fig. 1, a method of making a high temperature resistant aerogel fiber composite is shown, according to an embodiment of the present disclosure. As shown in fig. 1, the method comprises the steps of:
(1) prehydrolysis is carried out on tetramethyl orthosilicate to form silica sol;
(2) dissolving a zirconium source in a mixed solvent of ethanol and deionized water;
(3) adding formamide into the solution generated in the step (2) and stirring;
(4) adding the silica sol generated in the step (1) into the solution generated in the step (3) to generate a mixed sol system;
(5) adding a gel initiator into the mixed sol system generated in the step (4) to generate sol-gel transformation to form a wet gel block;
(6) carrying out solvent replacement on the wet gel block generated in the step (5) and ethanol;
(7) carrying out surface silanization on the wet gel block subjected to solvent replacement in the step (6) in an ethanol/tetraethyl orthosilicate solution;
(8) immersing basalt fibers into the wet gel block subjected to surface silanization in the step (7), standing for aging, then rolling and placing in a supercritical reaction kettle; and
(9) and (3) performing supercritical drying on the material in the supercritical reaction kettle by adopting carbon dioxide to obtain the aerogel composite fiber block.
In some embodiments, in the step (1), tetraethyl orthosilicate is prehydrolyzed at a water to silicon ratio (r) =1, pH =3, 50 ℃ for 60 minutes to form a silica sol. For example, 38mL of tetraethoxysilane can be dissolved in 140mL of ethanol, 12mL of deionized water is added, 0.5mL of 1 mol/L hydrochloric acid is added as a catalyst, and prehydrolysis is carried out for 60 minutes under the condition of heating in a water bath.
In some embodiments, in step (2), the zirconium source is Zirconium Oxychloride (ZOC). In other embodiments, in step (2), the zirconium source is zirconium polyacetylacetonate (C)20H28O8Zr)。
In some embodiments, in step (3), formamide is added to the solution produced in step (2) and stirred for 30 minutes.
In some embodiments, in the step (4), the mass fraction of the silicon dioxide in the zirconium dioxide is 12.4% to 16.8%, for example, about 14.6%.
In some embodiments, in the step (5), a gel initiator is added to the mixed sol system generated in the step (4), and a sol-gel transition occurs within about 5 minutes to form a wet gel mass.
In some embodiments, in step (5), the gel initiator is Propylene Oxide (PO). In other embodiments, in step (5), the gel initiator is ammonia (NH4 · OH).
In some embodiments, in the steps (2) to (5), the ratio of the components and the process parameters are as follows:
in the step (2), 1.75g of the zirconium source is dissolved in 20mL of the mixed solvent of ethanol and deionized water with the volume ratio of 3;
in the step (3), 200uL of formamide is added into the solution generated in the step (2) and stirred for 30 minutes;
in the step (4), 1.86mL of the silica sol generated in the step (1) is added into the solution generated in the step (3) so that the mass fraction of the silica in the zirconium dioxide is 14.6%;
in the step (5), 3.8mL of propylene oxide or 200uL of ammonia water is added into the mixed sol system generated in the step (4),
wherein, the numerical values of the above-mentioned component proportions and process parameters represent the range of 15% above and below the numerical values.
In some embodiments, in said (6), the wet gel mass produced in step (5) is subjected to solvent displacement with ethanol, 3 times within 24 hours, for example 1 time every 8 hours.
In some embodiments, in the step (7), the wet gel mass after solvent replacement in the step (6) is mixed in a volume ratio of 1: 1 in ethanol/tetraethyl orthosilicate solution, 3 times in 24 hours, for example 1 time every 8 hours.
In some embodiments, in the step (8), the wet gel block after surface silanization in the step (7) is immersed in basalt fiber, left to stand for aging for 24 hours, and then wound up and placed in a supercritical reaction kettle.
The method for preparing the high temperature resistant aerogel fiber composite according to the embodiments of the present invention is described above with reference to the accompanying drawings, and it should be noted that the above description is only an example and not a limitation of the present invention. In other embodiments of the invention, the method may include more, fewer, or different process steps, and the ingredients, proportions, and process conditions and parameters in the various process steps may differ from those described and illustrated.
In another aspect of the present invention, there is also provided a high temperature resistant aerogel fiber composite prepared according to the preparation method of the high temperature resistant aerogel fiber composite of any one embodiment of the present invention.
Several specific exemplary embodiments of the method of making the high temperature resistant aerogel fiber composite of the present invention are described below:
the first embodiment is as follows: ZOC is taken as a zirconium source, PO is taken as a gel initiator
Preparing materials:
1. zirconium oxychloride (ZOC, 99%),
2. tetraethoxysilane (TEOS, >99%),
3. ethanol (EtOH ≧ 99.5%),
4. hydrochloric acid (HC1, 36.0% -38.0%),
5. formamide (FA, 99%),
6. propylene oxide (PO ≧ 99.5%),
preparation process
TEOS prehydrolysis
TEOS was prehydrolyzed for 60 minutes at a water to silicon ratio (r) =1, pH =3, 50 ℃, the specific procedure was as follows:
38mL of TEOS is dissolved in 140mL of ethanol, 12mL of deionized water is added, and 0.5mL of 1 mol/L hydrochloric acid is added as a catalyst, and prehydrolysis is carried out for 60 minutes under the condition of heating in a water bath.
2. ZrO2/SiO2Preparation of hybrid aerogels
2.1 g and 1.75g of ZOC are dissolved in 20mL of a mixed solvent of ethanol and deionized water with the volume ratio of 3,
2.2, adding 200uL of FA and stirring for 30 minutes;
2.3, 1.86mL of SiO2Sol (corresponding to SiO)2At ZrO2The mass fraction in (1) is 14.6%);
2.4, adding 3.8mL of PO gel initiator into each mixed sol system, wherein the mixed sol system can generate sol-gel transformation within 5 minutes to form a gel block;
2.5, the wet gel block is subjected to solvent replacement (3 times/24 hours);
2.6, mixing the components in a volume ratio of 1: 1 EtOH/TEOS (3 times/24 hours);
2.7, immersing the basalt fiber felt, standing, aging for 24 hours, rolling and placing in a supercritical reaction kettle;
2.8, using CO2And (4) performing supercritical drying to obtain the aerogel composite fiber block.
Example two: taking zirconium polyacetylacetonate as a zirconium source and PO as a gel initiator
Preparing materials:
1. zirconium polyacetylacetonate (C)20H28O8Zr)，
2. Tetraethoxysilane (TEOS, >99%),
3. ethanol (EtOH ≧ 99.5%),
4. hydrochloric acid (HC1, 36.0% -38.0%),
5. formamide (FA ≧ 99%),
6. propylene oxide (PO ≧ 99.5%),
preparation process
TEOS prehydrolysis
Prehydrolysis of TEOS at a water to silicon ratio (r) =1, pH =3, 50 ℃ for 60 minutes,
the specific operation process is that 38mL TEOS is dissolved in 140mL ethanol, 12mL deionized water is added, 0.5mL 1 mol/L hydrochloric acid is added as a catalyst, and prehydrolysis is carried out for 60 minutes under the condition of water bath heating.
2. ZrO2/SiO2Preparation of hybrid aerogels
Dissolving 2.1 g and 1.75g of zirconium polyacetylacetonate in 20mL of ethanol deionized water mixed solvent with the volume ratio of 3;
2.2, adding 200uL of FA and stirring for 30 minutes;
2.3, 1.86mL of SiO2Sol (corresponding to SiO)2At ZrO2The mass fraction in (1) is 14.6%);
2.4, adding 3.8mL of PO gel initiator into the mixed sol system, wherein the mixed sol system can generate sol-gel transformation within 5 minutes to form a gel block;
2.5, the wet gel block is subjected to solvent replacement (3 times/24 hours);
2.6, mixing the components in a volume ratio of 1: 1 EtOH/TEOS (3 times/24 hours);
2.7, immersing the basalt fiber felt, standing, aging for 24 hours, and then placing the soaked basalt fiber felt in a supercritical reaction kettle;
2.8, performing supercritical drying by using CO2 to obtain the aerogel composite fiber block.
Example three: zirconium polyacetylacetonate as zirconium source and NH4 & OH as gel initiator
Preparing materials:
1. zirconium polyacetylacetonate (C)20H28O8Zr)，
2. Tetraethoxysilane (TEOS, >99%),
3. ethanol (EtOH ≧ 99.5%),
4. hydrochloric acid (HC1, 36.0% -38.0%),
5. formamide (FA ≧ 99%),
6. ammonia (NH 4. OH, 25% -28%)
Preparation process
TEOS prehydrolysis
TEOS was prehydrolyzed for 60 minutes at a water to silicon ratio (r) =1, pH =3, 50 ℃, the specific procedure was as follows:
38mL of TEOS is dissolved in 140mL of ethanol, 12mL of deionized water is added, and 0.5mL of 1 mol/L hydrochloric acid is added as a catalyst, and prehydrolysis is carried out for 60 minutes under the condition of heating in a water bath.
2. ZrO2/SiO2Preparation of hybrid aerogels
Dissolving 2.1 g and 1.75g of zirconium polyacetylacetonate in 20mL of ethanol deionized water mixed solvent with the volume ratio of 3;
2.2, adding 200uL of FA and stirring for 30 minutes;
2.3, 1.86mL of SiO2Sol (corresponding to SiO)2At ZrO2The mass fraction in (1) is 14.6%);
2.4, adding 200uL of NH4 & OH gel initiator into each mixed sol system, wherein the mixed sol system can generate sol-gel transformation within 5 minutes to form a gel block;
2.5, the wet gel block is subjected to solvent replacement (3 times/24 hours);
2.6, mixing the components in a volume ratio of 1: 1 EtOH/TEOS (3 times/24 hours);
2.7, immersing the basalt fiber felt, standing, aging for 24 hours, and then placing the soaked basalt fiber felt in a supercritical reaction kettle;
2.8, performing supercritical drying by using CO2 to obtain the aerogel composite fiber block.
The hybrid aerogel obtained according to the embodiment of the invention can be used in an environment at the temperature of less than 1100 ℃, has the thermal shrinkage rate of less than 25%, and has the thermal conductivity of 0.026, 0.037 and 0.058W/m.K at the temperature of 600 ℃, 800 ℃ and 1000 ℃, respectively, thereby indicating the potential application of the hybrid aerogel in the field of high-temperature-resistant heat insulation. In addition, the composite material has better cutting processing performance, can be cut in any shape by a cutter, has simple and easy preparation process and good repeatability, and can obtain aerogel composite heat insulation plates in batches.
Although the present invention has been disclosed above by way of examples, the present invention is not limited thereto. Various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this disclosure, and the scope of the invention should be determined only by the language of the claims and the equivalents thereof.
Claims (6)
1. A preparation method of a high-temperature resistant aerogel fiber composite material comprises the following steps:
(1) prehydrolysis is carried out on tetramethyl orthosilicate to form silica sol;
(2) dissolving a zirconium source in a mixed solvent of ethanol and deionized water;
(3) adding formamide into the solution generated in the step (2) and stirring;
(4) adding the silica sol generated in the step (1) into the solution generated in the step (3) to generate a mixed sol system;
(5) adding a gel initiator into the mixed sol system generated in the step (4) to generate sol-gel transformation to form a wet gel block;
(6) carrying out solvent replacement on the wet gel block generated in the step (5) and ethanol;
(7) carrying out surface silanization on the wet gel block subjected to solvent replacement in the step (6) in an ethanol/tetraethyl orthosilicate solution;
(8) immersing basalt fibers into the wet gel block subjected to surface silanization in the step (7), standing for aging, then rolling and placing in a supercritical reaction kettle; and
(9) and (3) performing supercritical drying on the material in the supercritical reaction kettle by adopting carbon dioxide to obtain the aerogel composite fiber block.
2. The method of claim 1, wherein the zirconium source is zirconium oxychloride or zirconium polyacetylacetonate.
3. The method of claim 1, wherein the gel initiator is propylene oxide or ammonia.
4. The method according to claim 1, wherein in the step (4), the mass fraction of silicon dioxide in zirconium dioxide is made to be 12.4% -16.8%.
5. The method of claim 1, wherein in the steps (2) to (5), the component ratios and the process parameters are as follows:
in the step (2), 1.75g of the zirconium source is dissolved in 20mL of the mixed solvent of ethanol and deionized water with the volume ratio of 3;
in the step (3), 200uL of formamide is added into the solution generated in the step (2) and stirred for 30 minutes;
in the step (4), 1.86mL of the silica sol generated in the step (1) is added into the solution generated in the step (3) so that the mass fraction of the silica in the zirconium dioxide is 14.6%;
in the step (5), 3.8mL of propylene oxide or 200uL of ammonia water is added into the mixed sol system generated in the step (4),
wherein, the numerical values of the above-mentioned component proportions and process parameters represent the range of 15% above and below the numerical values.
6. A high temperature resistant aerogel fiber composite prepared according to the method of any of claims 1-5.
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| CN112079618A (en) * | 2020-09-14 | 2020-12-15 | 南京工业大学 | Preparation method of modified silica aerogel heat insulation sheet |
| CN112625288A (en) * | 2020-12-08 | 2021-04-09 | 苏州启创新材料科技有限公司 | Organic-inorganic hybrid heat insulation film based on MOF/aerogel composite modification and preparation method thereof |
| CN114621016A (en) * | 2022-03-18 | 2022-06-14 | 安徽碳鑫科技有限公司 | Preparation process of refractory heat-insulating material |
| CN114790004A (en) * | 2022-04-19 | 2022-07-26 | 江苏安珈新材料科技有限公司 | Preparation of high-temperature-resistant SiO by using metal inorganic salt 2 Method for producing AxOy aerogels |
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| CN114790004A (en) * | 2022-04-19 | 2022-07-26 | 江苏安珈新材料科技有限公司 | Preparation of high-temperature-resistant SiO by using metal inorganic salt 2 Method for producing AxOy aerogels |
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