CN115304066A - Preparation method of high-temperature-resistant aerogel powder - Google Patents
Preparation method of high-temperature-resistant aerogel powder Download PDFInfo
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- CN115304066A CN115304066A CN202211008548.1A CN202211008548A CN115304066A CN 115304066 A CN115304066 A CN 115304066A CN 202211008548 A CN202211008548 A CN 202211008548A CN 115304066 A CN115304066 A CN 115304066A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/152—Preparation of hydrogels
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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Abstract
The invention provides a preparation method of high-temperature resistant aerogel powder, which comprises the following steps: s1, adding an aqueous silicon source into water, adjusting the pH value to 0.5-5 by using a chlorine-free acid, standing for 2-3 hours at the temperature of-2 to-3 ℃ for desalting, adding an opacifier, and uniformly stirring to obtain sol; s2, adjusting the pH value of the sol obtained in the step S1 to 5-6, heating to 40-60 ℃, and curing to obtain gel; s3, placing the gel obtained in the step S2 in an environment with the temperature of 10-60 ℃, standing and aging for 12-24 hours to obtain aged gel; s4, crushing the aged gel obtained in the step S3 to obtain gel powder, and modifying the gel powder by using a chlorine-free alcohol-free surface modifier at the temperature of 40-70 ℃ to obtain modified gel; and S5, drying the modified gel obtained in the step S4 by using drying equipment, cooling by using a cooling system, and collecting by using a collecting system to obtain the high-temperature resistant aerogel powder. The high-temperature resistant aerogel powder prepared by the invention has better high-temperature resistance.
Description
Technical Field
The invention relates to a preparation method of high-temperature resistant aerogel powder.
Background
The silicon dioxide aerogel is a novel nano, porous, low-density and amorphous material and has a continuous three-dimensional network structure. The porosity of the silicon dioxide aerogel is as high as 80-99%, the typical size of the pores is 1-100mm, and the silicon dioxide aerogel has the advantages of low refractive index, small Young modulus, low acoustic impedance, low thermal conductivity, strong adsorption performance and the like, and has unique properties in the aspects of chemistry, thermal, optics, acoustics, electricity and the like. The silicon dioxide aerogel is put into production and use at home and abroad, has a fast speed increase in domestic industrial scale, is put into use in various fields such as petrochemical industry, heating power pipe networks, new energy automobiles and the like, and shows excellent performance.
The aerogel can be made of various materials such as inorganic materials, organic materials and the like, wherein the technology of the silica aerogel is the most mature, the production cost is the lowest, and the silica aerogel is applied to the fields of petrochemical pipeline heat preservation and the like in the form of a heat preservation felt. However, the nanometer pore channel of the existing silicon dioxide aerogel begins to collapse when the temperature is over 800 ℃, and the heat preservation effect is basically lost when the temperature is over 1000 ℃, so that the existing silicon dioxide aerogel cannot be used in the field of high-temperature-resistant heat preservation and heat insulation.
Disclosure of Invention
The invention aims to provide a preparation method of high-temperature resistant aerogel powder, and the prepared high-temperature resistant aerogel powder has better high-temperature resistance.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of high-temperature resistant aerogel powder comprises the following steps:
s1, adding an aqueous silicon source into water, adjusting the pH value to 0.5-5 by using acid without chlorine, standing for 2-3 hours at the temperature of-2 to-3 ℃ for desalting, adding an opacifier, and uniformly stirring to obtain sol;
s2, adjusting the pH value of the sol obtained in the step S1 to 5-6, heating to 40-60 ℃, and curing to obtain gel;
s3, placing the gel obtained in the step S2 in an environment with the temperature of 10-60 ℃, standing and aging for 12-24 hours to obtain aged gel;
s4, crushing the aged gel obtained in the step S3 to obtain gel powder, and modifying the gel powder by using a chlorine-free alcohol-free surface modifier at the temperature of 40-70 ℃ to obtain modified gel;
and S5, drying the modified gel obtained in the step S4 by using drying equipment, cooling by using a cooling system, and collecting by using a collecting system to obtain the high-temperature resistant aerogel powder.
In step S1 of the present invention, 30 to 40 parts by weight of an aqueous silicon source, 30 to 40 parts by weight of water, 10 to 20 parts by weight of a chlorine-free acid, and 0.1 to 0.5 part by weight of an opacifying agent are further included.
Further, in step S1 of the present invention, the aqueous silicon source is one of water glass and sodium metasilicate.
Further, in step S1 of the present invention, the acid not containing chlorine is one of sulfuric acid, phosphoric acid, citric acid, and oxalic acid.
In step S1 of the present invention, the light-shading agent is one of ferrous oxide, carbon black, titanium dioxide, potassium hexatitanate whisker, zinc oxide, aluminum oxide, magnesium oxide, and aluminum silicate.
Further, in step S4 of the present invention, the specific process of modification is: mixing the chlorine-free and alcohol-free surface modifier with the gel powder according to the weight ratio of 1 (1-2), and stirring for 60-100min at the stirring speed of 10-50 r/min.
Further, in step S4 of the present invention, the chlorine-free and alcohol-free surface modifier is hexamethyldisiloxane, methyltrimethoxysilane, bistrimethylsiloxysilyl silane, or hexamethyldisilazane.
Furthermore, in the step S5 of the invention, the feeding temperature of the drying system is 120-150 ℃, the discharging temperature is 90-105 ℃, and the temperature of the cooling system is 0-2 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1) The heat transfer paths in the aerogel include solid-phase heat transfer, gas-phase heat transfer and radiation heat transfer, the heat transfer is mainly realized by radiation in a high-temperature environment, an object transfers energy by electromagnetic waves and is called as radiation, and theoretically, any substance above absolute zero can carry out heat radiation, but the heat radiation only plays a determining role at high temperature. Thermal radiation, like visible light, also has reflective, refractive and absorptive properties, subject to the laws of reflection and refraction of light. The opacifier has strong absorption and scattering performance on heat radiation, and can effectively inhibit the proportion of radiation heat transfer in the aerogel.
2) The high-temperature resistant gel powder disclosed by the invention belongs to a general material in the field of high-temperature heat insulation, solves the problem that high-efficiency nano heat insulation materials in the field of high-temperature heat insulation are extremely deficient, can be used for high-temperature industrial equipment such as high-temperature industrial kilns, smelting furnaces, petrochemical cracking furnaces and the like and materials such as wood, steel and the like which need high-temperature fire protection, has very wide application scenes and has great potential market value.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
Preparing high-temperature resistant aerogel powder according to the following steps:
s1, adding 30 parts of water glass into 40 parts of water, adjusting the pH value to 3 by using 10 parts of sulfuric acid, standing in an environment at the temperature of-2 ℃ for 2.5 hours to remove salt, adding 0.1 part of carbon black and 0.2 part of potassium hexatitanate whiskers, and uniformly stirring to obtain sol;
s2, adjusting the pH value of the sol obtained in the step S1 to 5.5, heating to 45 ℃, and curing to obtain gel;
s3, placing the gel obtained in the step S2 in an environment of 45 ℃ for standing and aging for 18 hours to obtain aged gel;
s4, crushing the aged gel obtained in the step S3 to obtain gel powder, mixing hexamethyldisilazane with the weight ratio of 1:1 and the gel powder at 60 ℃, and stirring at the stirring speed of 30r/min for 80min to obtain modified gel;
s5, drying the modified gel obtained in the step S4 by using drying equipment, cooling the dried modified gel by using a cooling system, and collecting the modified gel by using a collecting system to obtain high-temperature-resistant aerogel powder, wherein the feeding temperature of the drying system is 135 ℃, the discharging temperature of the drying system is 100 ℃, and the temperature of the cooling system is 1 ℃.
Example 2
Preparing high-temperature resistant aerogel powder according to the following steps:
s1, adding 30 parts of water glass into 30 parts of water, adjusting the pH value to 3.5 by using 10 parts of sulfuric acid, standing in an environment at the temperature of-3 ℃ for 2.4 hours to remove salt, then adding 0.4 part of titanium dioxide, and uniformly stirring to obtain sol;
s2, adjusting the pH value of the sol obtained in the step S1 to 5, heating to 50 ℃, and curing to obtain gel;
s3, placing the gel obtained in the step S2 in an environment of 50 ℃, standing and aging for 12 hours to obtain aged gel;
s4, crushing the aged gel obtained in the step S3 to obtain gel powder, mixing hexamethyldisilazane with the weight ratio of 1:2 and the gel powder at 60 ℃, and stirring at a stirring speed of 20r/min for 90min to obtain modified gel;
s5, drying the modified gel obtained in the step S4 by using drying equipment, cooling the dried modified gel by using a cooling system, and collecting the modified gel by using a collecting system to obtain high-temperature-resistant aerogel powder, wherein the feeding temperature of the drying system is 120 ℃, the discharging temperature of the drying system is 90 ℃, and the temperature of the cooling system is 0 ℃.
Example 3
Preparing high-temperature resistant aerogel powder according to the following steps:
s1, adding 35 parts of water glass into 36 parts of water, adjusting the pH value to 5 by using 15 parts of phosphoric acid, standing for 2 hours in an environment at the temperature of-3 ℃ for desalting, then adding 0.2 part of ferrous oxide and 0.3 part of zinc oxide, and uniformly stirring to obtain sol;
s2, adjusting the pH value of the sol obtained in the step S1 to 5.1, and heating to 40 ℃ to solidify to obtain gel;
s3, placing the gel obtained in the step S2 in an environment of 10 ℃, standing and aging for 24 hours to obtain aged gel;
s4, crushing the aged gel obtained in the step S3 to obtain gel powder, mixing hexamethyldisiloxane and the gel powder in a weight ratio of 1.5 at 70 ℃, and stirring at a stirring speed of 10r/min for 100min to obtain modified gel;
s5, drying the modified gel obtained in the step S4 by using drying equipment, cooling the dried modified gel by using a cooling system, and collecting the modified gel by using a collecting system to obtain high-temperature-resistant aerogel powder, wherein the feeding temperature of the drying system is 140 ℃, the discharging temperature of the drying system is 100 ℃, and the temperature of the cooling system is 1 ℃.
Example 4
Preparing high-temperature resistant aerogel powder according to the following steps:
s1, adding 40 parts of sodium metasilicate into 35 parts of water, adjusting the pH value to 1 by using 20 parts of citric acid, standing for 3 hours at the temperature of minus 2 ℃ for desalting, adding 0.1 part of aluminum silicate, and uniformly stirring to obtain sol;
s2, adjusting the pH value of the sol obtained in the step S1 to 6, heating to 60 ℃, and curing to obtain gel;
s3, placing the gel obtained in the step S2 in an environment of 60 ℃ for standing and aging for 15 hours to obtain aged gel;
s4, crushing the aged gel obtained in the step S3 to obtain gel powder, mixing methyltrimethoxysilane with the weight ratio of 1.5 to the gel powder at 50 ℃, and stirring at the stirring speed of 50r/min for 60min to obtain modified gel;
s5, drying the modified gel obtained in the step S4 by using drying equipment, cooling the dried modified gel by using a cooling system, and collecting the modified gel by using a collecting system to obtain high-temperature-resistant aerogel powder, wherein the feeding temperature of the drying system is 150 ℃, the discharging temperature of the drying system is 105 ℃, and the temperature of the cooling system is 2 ℃.
Example 5
Preparing high-temperature resistant aerogel powder according to the following steps:
s1, adding 35 parts of sodium metasilicate into 36 parts of water, adjusting the pH value to 5 by using 15 parts of oxalic acid, standing in an environment at the temperature of-3 ℃ for 2 hours to remove salt, then adding 0.2 part of aluminum oxide and 0.2 part of magnesium oxide, and uniformly stirring to obtain sol;
s2, adjusting the pH value of the sol obtained in the step S1 to 5.1, and heating to 40 ℃ to solidify to obtain gel;
s3, placing the gel obtained in the step S2 in an environment of 10 ℃ for standing and aging for 24 hours to obtain aged gel;
s4, crushing the aged gel obtained in the step S3 to obtain gel powder, mixing bis (trimethylsilyloxy) methylsilane with the gel powder in a weight ratio of 1.5 at 70 ℃, and stirring at a stirring speed of 10r/min for 100min to obtain modified gel;
s5, drying the modified gel obtained in the step S4 by using drying equipment, cooling the dried modified gel by using a cooling system, and collecting the modified gel by using a collecting system to obtain high-temperature-resistant aerogel powder, wherein the feeding temperature of the drying system is 140 ℃, the discharging temperature of the drying system is 100 ℃, and the temperature of the cooling system is 1 ℃.
Experimental example: thermal conductivity test
The high temperature resistant aerogel powders prepared in examples 1 to 5 and the comparative example (a conventional silica aerogel powder prepared from pure silica, excluding other components) were each tested for thermal conductivity at 1000 ℃ by the unsteady planar heat source method.
The test results are shown in table 1:
TABLE 1
| Coefficient of thermal conductivity (W/m. K) | |
| Example 1 | 0.034 |
| Example 2 | 0.035 |
| Example 3 | 0.037 |
| Example 4 | 0.036 |
| Example 5 | 0.038 |
| Comparative example | 0.102 |
As can be seen from Table 1, the thermal conductivity coefficients at 1000 ℃ of the samples 1 to 5 are obviously lower than those of the comparative samples, which shows that the high temperature resistant aerogel powder prepared by the invention has better high temperature resistance.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. A preparation method of high-temperature resistant aerogel powder is characterized by comprising the following steps: the method comprises the following steps:
s1, adding an aqueous silicon source into water, adjusting the pH value to 0.5-5 by using a chlorine-free acid, standing for 2-3 hours at the temperature of-2 to-3 ℃ for desalting, adding an opacifier, and uniformly stirring to obtain sol;
s2, adjusting the pH value of the sol obtained in the step S1 to 5-6, heating to 40-60 ℃, and curing to obtain gel;
s3, placing the gel obtained in the step S2 in an environment with the temperature of 10-60 ℃ for standing and aging for 12-24 hours to obtain aged gel;
s4, crushing the aged gel obtained in the step S3 to obtain gel powder, and modifying the gel powder by using a chlorine-free alcohol-free surface modifier at the temperature of 40-70 ℃ to obtain modified gel;
and S5, drying the modified gel obtained in the step S4 by using drying equipment, cooling by using a cooling system, and collecting by using a collecting system to obtain the high-temperature resistant aerogel powder.
2. The method for preparing high-temperature-resistant aerogel powder according to claim 1, wherein the method comprises the following steps: in the step S1, 30-40 parts of aqueous silicon source, 30-40 parts of water, 10-20 parts of chlorine-free acid and 0.1-0.5 part of opacifier by weight.
3. The method for preparing high-temperature-resistant aerogel powder according to claim 1, wherein the method comprises the following steps: in the step S1, the aqueous silicon source is one of water glass and sodium metasilicate.
4. The method for preparing high-temperature-resistant aerogel powder according to claim 1, wherein the method comprises the following steps: in the step S1, the acid not containing chlorine is one of sulfuric acid, phosphoric acid, citric acid, and oxalic acid.
5. The method for preparing high-temperature-resistant aerogel powder according to claim 1, wherein the method comprises the following steps: in the step S1, the opacifier is one of ferrous oxide, carbon black, titanium dioxide, potassium hexatitanate whisker, zinc oxide, aluminum oxide, magnesium oxide, and aluminum silicate.
6. The method for preparing high-temperature-resistant aerogel powder according to claim 1, wherein the method comprises the following steps: in the step S4, the specific process of modification is as follows: mixing the chlorine-free and alcohol-free surface modifier with the gel powder according to the weight ratio of 1 (1-2), and stirring for 60-100min at the stirring speed of 10-50 r/min.
7. The method for preparing high-temperature-resistant aerogel powder according to claim 1, wherein the method comprises the following steps: in the step S4, the chlorine-free and alcohol-free surface modifier is hexamethyldisiloxane, methyltrimethoxysilane, bistrimethylsiloxymethylsilane, or hexamethyldisilazane.
8. The method for preparing high-temperature-resistant aerogel powder according to claim 1, wherein the method comprises the following steps: in the step S5, the feeding temperature of the drying system is 120-150 ℃, the discharging temperature is 90-105 ℃, and the temperature of the cooling system is 0-2 ℃.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6210751B1 (en) * | 1995-11-09 | 2001-04-03 | Cabot Corporation | Process for preparing organically modified aerogels in which the salts formed are precipitated out |
| CN104030301A (en) * | 2014-06-18 | 2014-09-10 | 金承黎 | Silicon dioxide aerogel material and preparation method thereof |
| CN107098352A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method of high temperature resistant aeroge and aerogel type porous ceramics |
| CN108314411A (en) * | 2018-01-03 | 2018-07-24 | 深圳中凝科技有限公司 | The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine |
| CN109734101A (en) * | 2019-03-12 | 2019-05-10 | 江苏脒诺甫纳米材料有限公司 | A kind of high temperature resistant silicon substrate aerogel powder and preparation method thereof |
| CN112592149A (en) * | 2020-12-31 | 2021-04-02 | 山东大学 | Method for rapidly preparing silicon dioxide aerogel composite material by taking water glass as raw material through single solvent exchange |
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- 2022-08-22 CN CN202211008548.1A patent/CN115304066A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6210751B1 (en) * | 1995-11-09 | 2001-04-03 | Cabot Corporation | Process for preparing organically modified aerogels in which the salts formed are precipitated out |
| CN104030301A (en) * | 2014-06-18 | 2014-09-10 | 金承黎 | Silicon dioxide aerogel material and preparation method thereof |
| CN107098352A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method of high temperature resistant aeroge and aerogel type porous ceramics |
| CN108314411A (en) * | 2018-01-03 | 2018-07-24 | 深圳中凝科技有限公司 | The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine |
| CN109734101A (en) * | 2019-03-12 | 2019-05-10 | 江苏脒诺甫纳米材料有限公司 | A kind of high temperature resistant silicon substrate aerogel powder and preparation method thereof |
| CN112592149A (en) * | 2020-12-31 | 2021-04-02 | 山东大学 | Method for rapidly preparing silicon dioxide aerogel composite material by taking water glass as raw material through single solvent exchange |
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