CN114620736B - Compression-controllable SiO 2 Aerogel composite material preparation method - Google Patents
Compression-controllable SiO 2 Aerogel composite material preparation method Download PDFInfo
- Publication number
- CN114620736B CN114620736B CN202111533985.0A CN202111533985A CN114620736B CN 114620736 B CN114620736 B CN 114620736B CN 202111533985 A CN202111533985 A CN 202111533985A CN 114620736 B CN114620736 B CN 114620736B
- Authority
- CN
- China
- Prior art keywords
- sio
- aerogel composite
- hardness
- composite material
- aerogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a compression-controllable SiO 2 Aerogel compositeMethod for preparing composite material, siO by controlled preparation 2 Pure SiO in raw material for preparing aerogel composite material 2 Hardness and wet gel aging time to achieve controllable compression of the product; specifically including SiO as desired 2 Determination of the compressibility of the aerogel composite to be produced 2 Hardness and wet gel aging time of the aerogel composite; then determining the proportion of ethyl silicate, absolute ethyl alcohol and deionized materials according to a hardness formula and preparing SiO 2 Aerogel glue solution; finally, the sheet is dipped into gel, and then the SiO with the required hardness is obtained after wet gel aging, hydrophobic treatment and drying 2 An aerogel composite. The method realizes the controllable compression production of SiO 2 The aerogel composite material is simple and feasible in method and accurate in result, the hardness of the product can be adjusted according to different compression requirements among the battery units, accurate application of the aerogel composite material among the battery units is guaranteed, and the aerogel composite material has a good application prospect.
Description
Technical Field
The invention relates to SiO with controllable compression 2 A method for preparing aerogel composite material.
Background
SiO 2 The aerogel composite material has excellent performances of high porosity, high specific area, low volume density, extremely low thermal conductivity coefficient, low temperature and high temperature resistance, A-grade non-inflammability, environmental protection, no toxicity and the like, is regarded as the most promising material in the field of heat insulation, and is widely applied to the fields of aerospace and military affairs. In recent years, with the rapid development of new energy automobile technology, siO 2 The aerogel composite material is also applied to the field of new energy automobile manufacturing, and particularly applied to the manufacturing of batteries of new energy automobiles, and plays a role in heat insulation and fire prevention of battery pack units.
Since the gaps between the battery cells of the lithium ion battery pack of the new energy automobile are divided according to the shape of the battery, for example, the square lithium ion battery, the gaps between the battery cells are basically the same but different, therefore, the gaps between the cells are different for SiO 2 The thickness of the aerogel composite material has certain requirements, and the compression performance of the aerogel composite material is also required so as to ensure full adaptationThe gaps between the battery cells of the lithium ion battery pack ensure the heat-insulating and fireproof effects of the lithium ion battery pack.
SiO 2 The thickness of the aerogel composite material is mainly determined by the thickness of the base material, the compression performance of the base material is fixed according to the material of the base material, and the compression performance of certain base material is basically unchanged, so that the final SiO can be realized only by regulating and controlling the performance of the aerogel 2 The compression performance of the aerogel composite material product is controllable, and the application requirements of the aerogel composite material product in a lithium battery cell are met.
Disclosure of Invention
In view of the above-mentioned problems and in order to achieve the above-mentioned object, the present invention provides a SiO with controllable compression 2 The preparation method of the aerogel composite material is realized by controlling pure SiO 2 The hardness and the wet gel aging time of the product are controlled, and the prepared product has the advantages of good heat insulation performance, flame retardance, light weight, excellent compression performance, energy conservation, environmental protection and the like. The specific technical scheme is as follows:
compression-controllable SiO 2 Preparation method of aerogel composite material by controlling preparation of SiO 2 Pure SiO in raw material for preparing aerogel composite material 2 The method realizes the compression controllability of the product by hardness and wet gel aging time, and specifically comprises the following steps:
1) Determination of hardness and aging time: according to the SiO required 2 Determining the compression ratio of the aerogel composite material and determining the SiO to be prepared 2 Hardness and wet gel aging time of the aerogel composite;
2) Calculating the raw material ratio: according to the SiO to be prepared 2 The hardness of the aerogel composite material is determined by calculation of a hardness formula to prepare the SiO 2 The proportion of ethyl silicate, absolute ethyl alcohol and deionized water used by the aerogel composite material;
3) Preparing glue solution: weighing the materials according to the determined proportion among the ethyl silicate, the absolute ethyl alcohol and the deionized water, and preparing into SiO 2 Aerogel glue solution;
4) Gum dipping and aging: will be used to prepare the desired SiO 2 Placing the base material sheet of aerogel composite material on the surface of the aerogel composite materialIn the prepared container, the prepared SiO 2 Pouring the aerogel glue solution into a container, ensuring that each substrate sheet is soaked by the glue solution, and carrying out static gel aging according to the determined wet gel aging time;
5) Hydrophobic drying: taking out the base material sheet after the aging of the gel, performing surface hydrophobization treatment by using a hydrophobizing agent, and finally performing supercritical drying to obtain SiO with required hardness 2 An aerogel composite.
Compressive controlled SiO as described above 2 In the preparation method of the aerogel composite material, in the step 1) and the step 4), the determined hardness and the wet gel aging time are determined according to a compression ratio/gel hardness/wet gel aging time data table, and the compression ratio/gel hardness/wet gel aging time data table is determined according to a SiO 2 The compression ratio of the aerogel composite material is obtained through a plurality of tests, and comprises wet gel aging time, gel hardness value and SiO corresponding to the hardness value 2 Thickness of aerogel composite and its compressibility under 2MPa conditions.
Compressive controlled SiO as described above 2 A method for preparing the aerogel composite material, wherein in the step 2), the SiO is prepared by determining 2 The proportion of ethyl silicate, absolute ethyl alcohol and deionized water used by the aerogel composite material is as follows: according to the determined SiO 2 The hardness of the aerogel composite material is determined by calculation through a hardness formula to prepare SiO 2 The weight of the solvent absolute ethyl alcohol used for the aerogel; the hardness formula is as follows:
wherein the content of the first and second substances,
M silicon content Is M Ethyl silicate The content of medium silicon;
M ethyl silicate For preparing SiO 2 The weight of precursor ethyl silicate used for the aerogel;
M anhydrous ethanol For preparing SiO 2 The weight of the solvent absolute ethyl alcohol required by the aerogel;
M deionized water For preparing SiO 2 The weight of deionized water used for the aerogel;
H hardness of According to the required SiO 2 Gel hardness as determined by the compressibility of the aerogel composite.
Compressive controlled SiO as described above 2 The preparation method of the aerogel composite material comprises the step 4), wherein the specially-made container is a vessel box which is provided with a cover body and has the length of 450mm, the width of 250mm and the height of 100mm, and holes with the diameter of 20mm are formed in the surface of the vessel box.
Compressive controlled SiO as described above 2 Aerogel composite material preparation method for preparing required SiO 2 The base material sheet of the aerogel composite material is preferably any one of a pre-oxidized fiber base material, a glass fiber surface felt base material or a ceramic felt base material, and the thickness of the base material sheet is preferably 1-5 mm.
Compressive controlled SiO as described above 2 Aerogel composite material preparation method for preparing required SiO 2 When the base material sheet of the aerogel composite material is placed in a special container, the non-woven fabric with the thickness of 0.09mm is adopted for isolation between the sheets, and the sheets can be peeled.
Compressive controlled SiO as described above 2 In the step 5), the hydrophobizing agent is dimethyl diethoxy silane, the temperature of the hydrophobizing treatment is controlled to be 45-60 ℃, and the time of the hydrophobizing treatment is not less than 20 hours; the supercritical process is CO 2 Supercritical drying method, CO used therefor 2 Is food grade CO 2 。
The method has the beneficial effects that:
1) The method of the invention is realized by determining SiO 2 The hardness of the aerogel composite and the aging time of the wet gel to achieve controlled compression of the final product ensures accurate application of products of different thicknesses between cells.
2) The method prepares SiO by controlling 2 The weight of absolute ethyl alcohol as solvent for aerogel to control SiO 2 Hardness of aerogel so that SiO is controlled 2 The hardness of the aerogel becomes simpleAnd (4) single operation.
3) The method of the invention prepares SiO by calculation of a hardness formula 2 The weight of the solvent absolute ethyl alcohol required by the aerogel is simple and quick, and the prepared SiO is ensured 2 The hardness of the aerogel composite material reaches the required value, so that the compression ratio of the final product is ensured.
4) The method is established on SiO 2 Based on the data relationship between the compressibility of the aerogel composite material and the gel hardness and the wet gel aging time, the relationship between the compressibility/the gel hardness/the wet gel aging time is obtained by a great amount of experiments, so that the practice and the theory are combined, and the SiO is better controlled 2 The compression ratio of the aerogel composite material realizes controllable production of SiO according to requirements 2 An aerogel composite.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only preferred embodiments of the present invention, rather than all embodiments, and are not intended to limit the present invention in other forms, and any person skilled in the art may make changes or modifications equivalent to the technical solutions disclosed. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention. The contents of the examples are as follows:
example 1
This example is a process for preparing SiO with controlled compression 2 A method of aerogel composite. SiO2 2 The aerogel composite material comprises a base material and SiO solid-impregnated on the base material 2 The compressibility of the aerogel, substrate, is essentially unchanged, so this example is controlled by SiO 2 The properties of the aerogel to realize the prepared SiO 2 Controllability of the compression of the aerogel composite. In particular to the preparation of SiO by control 2 Pure SiO in raw material for preparing aerogel composite material 2 Preparation of SiO with controllable compression by hardness and gel aging time 2 A method of forming an aerogel composite. In particular toThe method comprises the following steps:
1) Determining the hardness: according to the required SiO 2 Compressibility and compressibility/gel hardness/Wet gel aging time data sheet for aerogel composites 2 Hardness and wet gel aging time of the aerogel composite; the compressibility/gel hardness/wet gel aging time data sheet is according to SiO 2 The compression ratio of the aerogel composite material is obtained through a plurality of tests and comprises the wet gel aging time, the gel hardness value and SiO corresponding to the hardness value 2 Thickness of aerogel composite and its compressibility under 2MPa conditions. The partial compressibility/gel hardness/wet gel aging time data table is shown in table 1:
TABLE 1 compressibility/gel hardness data Table (parts)
2) Calculating the raw material ratio: according to the SiO to be prepared 2 The hardness of the aerogel composite material is determined by calculation of a hardness formula to prepare the SiO 2 Ethyl silicate, absolute ethyl alcohol and deionized water are used in the aerogel composite material. Since the research finds that SiO 2 The hardness of the aerogel composite is primarily a function of the amount of solvent used. Under the condition of certain material and thickness of the base material, the proportion of the ethyl silicate to the deionized water is unchanged, and the smaller the proportion of the absolute ethyl alcohol is, the prepared SiO is 2 The greater the hardness of the aerogel composite; on the contrary, the larger the proportion of absolute ethyl alcohol is, the SiO prepared 2 The lower the hardness of the aerogel composite, i.e., by controlling the pure SiO in the feedstock 2 Hardness to control the SiO produced 2 Compressibility of the aerogel composite. Thus, the SiO to be prepared was determined 2 After the hardness of the aerogel composite material is kept constant, the proportion of ethyl silicate to deionized water is kept constant, and the dosage ratio of absolute ethyl alcohol is adjusted to obtain SiO with required hardness 2 An aerogel composite. In this embodiment, the hardness formula is:
wherein, the first and the second end of the pipe are connected with each other,
M silicon content Is M Ethyl silicate The content of medium silicon;
M ethyl silicate For preparing SiO 2 The weight of precursor tetraethoxysilane used for the aerogel;
M anhydrous ethanol For preparing SiO 2 The weight of the solvent absolute ethyl alcohol required by the aerogel;
M deionized water For preparing SiO 2 The weight of deionized water used for the aerogel;
H hardness of According to the required SiO 2 Gel hardness as determined by compressibility of the aerogel composite.
3) Preparing glue solution: weighing the materials according to the determined proportion among the ethyl silicate, the absolute ethyl alcohol and the deionized water, and preparing into SiO 2 And (4) aerogel glue solution.
4) Gum dipping and aging: will be used to prepare the desired SiO 2 Placing the base material sheet of aerogel composite material in a special container, and preparing SiO 2 Pouring the aerogel glue solution into a container, ensuring that each substrate sheet is soaked by the glue solution, and standing for gelation according to the determined wet gel aging time. The longer the gel aging time, the higher the strength of the skeleton generated inside the wet gel, and the SiO prepared thereby 2 Aerogel composites are not easily compressed, so the specific time for wet gel aging depends on the SiO being prepared 2 The desired compressibility of the aerogel composite is determined. In this embodiment, the specially-made container is a vessel box with a cover body and a length of 450mm, a width of 250mm and a height of 100mm, and the surface of the vessel box is provided with holes with a diameter of 20mm, so that glue can completely enter the vessel box. The substrate sheet is preferably any one of a pre-oxidized fiber substrate, a glass fiber surface felt substrate or a ceramic felt substrate, and the thickness of the substrate sheet is preferably 1-5 mm. When the substrate sheets are placed in a special container, the sheets need to be isolated from one another so as to ensure that the sheets can be separated from one anotherAnd (6) stripping. On the one hand, the preparation of SiO is ensured when the isolation material is selected 2 The aerogel composite material sheet can be peeled off from the sheet, and on the other hand, each base material sheet is ensured to be soaked by the glue solution, and the fact that too much container space is not occupied and too much glue solution is adsorbed is also considered, so that the non-woven fabric with the thickness of 0.09mm is preferably adopted to isolate the sheets in the embodiment.
5) Dewatering and drying: taking out the base material sheet after the gel aging, and performing surface hydrophobization by using dimethyl diethoxy silane as a hydrophobization reagent, wherein the temperature of the hydrophobization is controlled to be 45-60 ℃, and the time of the hydrophobization is not less than 20h; finally adopting the passage of CO 2 CO used for drying by supercritical drying 2 Is food grade CO 2 To obtain SiO with required hardness 2 An aerogel composite.
Example 2
This example prepared SiO with the specified thickness and compressibility according to the method described in example 1 2 An aerogel composite. In this example, siO to be prepared is required 2 The aerogel composite material is 3-3.5mm thick, and the adopted base material is a glass fiber surface felt; and the SiO is required to be 2 The compressibility of the aerogel composite material under the condition of 2MPa reaches 60-65%, and the SiO is determined by checking a compressibility/gel hardness/wet gel aging time data table 2 The hardness of the aerogel composite product was 6 and the wet gel aging time was 15h. In this embodiment, when the amount of ethyl silicate weighed is 100g and the amount of deionized water weighed is 24.6g, the weight of the required solvent, namely absolute ethyl alcohol, is calculated to be 558g. Pouring the weighed materials into a container, stirring, adding a catalyst after stirring for a certain time, and preparing into a glue solution. The prepared fiberglass surfacing mat is placed into a ware box. Pouring the prepared glue solution onto sheets to ensure that each sheet is soaked by the glue solution, covering an upper cover plate of a vessel box to wait for gelation, aging wet gel for 15h, taking out the sheets to perform surface hydrophobization treatment, wherein the temperature of the hydrophobization liquid is 45 ℃, the hydrophobization time is 35h, and performing CO (carbon monoxide) hydrophobization after hydrophobization 2 Supercritical drying to obtain SiO with required compression ratio 2 Aerogel composite products.
To ensure the final product is acceptable, the SiO is prepared 2 5 sheets are randomly drawn from the aerogel composite material to measure the thickness of the aerogel composite material and carry out compression performance test, and the specific test results are shown in table 2, and the results all meet the product requirements.
TABLE 2 hardness of 6 SiO 2 Aerogel composite compression performance test results
| Serial number | SiO2 aerogel composite thickness (mm) | Verification of the 2MPa compressibility (%) |
| 1 | 3.45 | 62.34 |
| 2 | 3.32 | 62.75 |
| 3 | 3.31 | 63.18 |
| 4 | 3.47 | 62.28 |
| 5 | 3.29 | 63.75 |
Example 3
This example also prepared SiO with the specified thickness and compressibility according to the method described in example 1 2 An aerogel composite. In this example, siO to be produced is required 2 The aerogel composite material is 3-3.5mm thick, and the adopted base material is a glass fiber surface felt; and the SiO is required to be 2 The compressibility of the aerogel composite material under the condition of 2MPa reaches 65-70%; the SiO is determined by looking up the compressibility/gel hardness/wet gel aging time data sheet 2 The hardness of the aerogel composite material product is 4, and the wet gel aging time is 10h; in this embodiment, when the weight of the ethyl silicate weighed is 100g and the weight of the deionized water weighed is 24.6g, the weight of the required solvent, namely the absolute ethyl alcohol, is determined to be 900g through calculation. Pouring the weighed materials into a container, stirring, adding a catalyst after stirring for a certain time, and preparing into a glue solution. Putting the prepared glass fiber surface felt into a vessel box, pouring the prepared glue solution onto the sheets to ensure that each sheet is soaked by the glue solution, covering an upper cover plate of the vessel box to wait for gelation, taking out the sheets after 10 hours of aging of the gelation, performing surface hydrophobization treatment, wherein the temperature of the hydrophobization liquid is 55 ℃, the hydrophobization time is 25 hours, and performing CO (carbon dioxide) hydrophobization after finishing hydrophobization 2 Supercritical drying to obtain SiO with required compression ratio 2 Aerogel composite products.
To ensure the final prepared product is acceptable, the SiO prepared 2 5 sheets are randomly drawn from the aerogel composite material to measure the thickness of the aerogel composite material and carry out compression performance test, and the specific test results are shown in table 3, so that the results all meet the product requirements.
TABLE 3 hardness of 4 SiO 2 Aerogel composite compression performance test results
| Serial number | SiO2 aerogel composite thickness (mm) | Verify the 2MPa compressibility (%) |
| 1 | 3.28 | 67.82 |
| 2 | 3.37 | 66.59 |
| 3 | 3.42 | 68.24 |
| 4 | 3.27 | 67.94 |
| 5 | 3.36 | 69.05 |
Example 4
This example also prepared SiO with the specified thickness and compressibility according to the method described in example 1 2 An aerogel composite. In this example, siO to be prepared is required 2 The aerogel composite material is 4.5-5mm thick, and the adopted base material is a glass fiber surface felt; and the SiO is required to be 2 The compressibility of the aerogel composite material under the condition of 2MPa reaches 45-50%, and the SiO is determined by checking a compressibility/gel hardness/wet gel aging data table 2 The hardness of the aerogel composite product was 12 and the wet gel aging time was 48h. In this embodiment, when the amount of ethyl silicate weighed is 100g and the amount of deionized water weighed is 24.6g, the weight of the required solvent, namely absolute ethyl alcohol, is determined by calculationThe amount was 217g. And pouring the weighed materials into a container, stirring for a certain time, and then adding a catalyst to prepare a glue solution. The prepared fiberglass surfacing mat is placed into a ware box. Pouring the prepared glue solution onto the sheets to ensure that each sheet is soaked by the glue solution, covering the upper cover plate of the vessel box to wait for gelation, taking out the sheets after the gelation is aged for 48h, performing surface hydrophobization treatment, wherein the temperature of the hydrophobization liquid is 60 ℃, the hydrophobization time is 20h, and performing CO (carbon monoxide) hydrophobization after the hydrophobization is finished 2 Supercritical drying to obtain SiO with hardness of 12 2 Aerogel composite products.
To ensure the final prepared product is acceptable, the SiO prepared 2 5 sheets are randomly drawn from the aerogel composite material to measure the thickness of the aerogel composite material and carry out compression performance test, and the specific test result is shown in table 4, and the result also meets the product requirement.
TABLE 4 hardness of 12 SiO 2 Aerogel composite compression performance test results
| Serial number | SiO2 aerogel composite thickness (mm) | Verification of the 2MPa compressibility (%) |
| 1 | 4.65 | 47.57 |
| 2 | 4.72 | 46.90 |
| 3 | 4.55 | 46.95 |
| 4 | 4.62 | 47.89 |
| 5 | 4.75 | 45.21 |
In summary, the process of the invention proceeds from defined SiO 2 The hardness of the aerogel composite and the wet gel aging time allow for controlled compression of the final product, ensuring accurate application of products of different thicknesses between cells. The method is established in SiO 2 Based on the relation between the compressibility of the aerogel composite material and the gel hardness data and the wet gel aging time, the relation between the compressibility/the gel hardness/the wet gel aging time is obtained by a great amount of experiments, so that the practice and the theory are combined, and the SiO is better controlled 2 The compression ratio of the aerogel composite material realizes controllable production of SiO according to requirements 2 An aerogel composite. And the method prepares SiO by controlling 2 The weight of the solvent absolute ethyl alcohol required by the aerogel is used for controlling SiO 2 Hardness of aerogel so that SiO is controlled 2 The hardness of the aerogel becomes simple and feasible, and the SiO is prepared by calculation of a hardness formula 2 The weight of the solvent absolute ethyl alcohol required by the aerogel is simple and quick, and the prepared SiO is ensured 2 The hardness of the aerogel composite material reaches a required value, so that the compression ratio of a final product is ensured, and the aerogel composite material has a good application prospect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (5)
1. Compression-controllable SiO 2 The preparation method of the aerogel composite material is characterized by comprising the following steps: preparation of SiO by controlled 2 Pure SiO in raw material for preparing aerogel composite material 2 Hardness of the wet gel and aging time of the wet gel to achieve controllable compression of the product; the method specifically comprises the following steps:
1) Determination of hardness and aging time: according to the SiO required 2 Determining the compression ratio of the aerogel composite material and determining the SiO to be prepared 2 Hardness and wet gel aging time of the aerogel composite; the determined hardness and the wet gel aging time are determined according to a compression rate/gel hardness data/gel aging time data table; the compression ratio/gel hardness/wet gel aging time data sheet is according to SiO 2 The compression ratio of the aerogel composite material is obtained through a plurality of tests, and comprises wet gel aging time, gel hardness value and SiO corresponding to the hardness value 2 The thickness of the aerogel composite material and the compressibility thereof under the condition of 2 MPa;
2) Calculating the raw material ratio: according to the SiO to be prepared 2 The hardness of the aerogel composite material is determined by calculation through a hardness formula to prepare the SiO 2 The proportion of ethyl silicate, absolute ethyl alcohol and deionized water used by the aerogel composite material; the determination prepares the SiO 2 The proportion of ethyl silicate, absolute ethyl alcohol and deionized water used by the aerogel composite material is determined according toSiO 2 The hardness of the aerogel composite material is determined by calculation through a hardness formula to prepare SiO 2 The weight of the solvent absolute ethyl alcohol used for the aerogel; the hardness formula is as follows:
wherein, the first and the second end of the pipe are connected with each other,
M silicon content Is M Ethyl silicate The content of medium silicon;
M ethyl silicate For preparing SiO 2 The weight of precursor ethyl silicate used for the aerogel;
M anhydrous ethanol For preparing SiO 2 The weight of the solvent absolute ethyl alcohol required by the aerogel;
M deionized water For preparing SiO 2 The weight of deionized water used for the aerogel;
H hardness of The gel hardness is determined according to the compression ratio of the required SiO2 aerogel composite material;
3) Preparing glue solution: weighing the materials according to the determined proportion among the ethyl silicate, the absolute ethyl alcohol and the deionized water, and preparing into SiO 2 Aerogel glue solution;
4) Gum dipping and aging: will be used to prepare the desired SiO 2 Placing the base material sheet of aerogel composite material in a special container, and preparing SiO 2 Pouring the aerogel glue solution into a container, ensuring that each substrate sheet is soaked by the glue solution, and standing for gelling according to the determined wet gelling aging time; the special container is a vessel box which is provided with a cover body and has the length of 450mm, the width of 250mm and the height of 100mm, and the surface of the vessel box is provided with a hole with the diameter of 20 mm;
5) Dewatering and drying: taking out the base material sheet after the aging of the gel, performing surface hydrophobization treatment by using a hydrophobizing agent, and finally performing supercritical drying to obtain SiO with required hardness 2 An aerogel composite.
2. Compression controllable SiO as claimed in claim 1 as required 2 The preparation method of the aerogel composite material is characterized by comprising the following steps: in step 4), the method is used for preparing the required SiO 2 The base material sheet of the aerogel composite material is any one of a pre-oxidized fiber base material, a glass fiber surface felt base material or a ceramic felt base material, and the thickness of the base material sheet is 1-5 mm.
3. Compression controllable SiO according to claim 1 or 2 2 The preparation method of the aerogel composite material is characterized by comprising the following steps: the method is used for preparing the required SiO 2 When the base material sheet of the aerogel composite material is placed in a special container, the non-woven fabric with the thickness of 0.09mm is adopted for isolation between the sheets, and the sheets can be peeled.
4. Compression controllable SiO as claimed in claim 1 2 The preparation method of the aerogel composite material is characterized by comprising the following steps: in the step 5), the hydrophobizing reagent is dimethyl diethoxy silane, the temperature of the hydrophobizing treatment is controlled to be 45-60 ℃, and the time of the hydrophobizing treatment is not less than 20 hours.
5. Compression controllable SiO as claimed in claim 1 2 The preparation method of the aerogel composite material is characterized by comprising the following steps: in step 5), the supercritical method is CO 2 Supercritical drying method, CO used therefor 2 Is food grade CO 2 。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111533985.0A CN114620736B (en) | 2021-12-15 | 2021-12-15 | Compression-controllable SiO 2 Aerogel composite material preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111533985.0A CN114620736B (en) | 2021-12-15 | 2021-12-15 | Compression-controllable SiO 2 Aerogel composite material preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114620736A CN114620736A (en) | 2022-06-14 |
| CN114620736B true CN114620736B (en) | 2023-04-18 |
Family
ID=81898420
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111533985.0A Active CN114620736B (en) | 2021-12-15 | 2021-12-15 | Compression-controllable SiO 2 Aerogel composite material preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114620736B (en) |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000034117A (en) * | 1998-07-16 | 2000-02-02 | Mitsui Chemicals Inc | Production of siliceous aerogel sphere |
| WO2007024925A2 (en) * | 2005-08-25 | 2007-03-01 | Keller Companies, Inc. | Aerogel and method of manufacturing same |
| US8596468B2 (en) * | 2007-06-27 | 2013-12-03 | J.M. Huber Corporation | Composite caustic silica gel manufacturing method and gels made thereby |
| PT107101A (en) * | 2013-08-02 | 2015-02-02 | Univ De Coimbra | FLEXIBLE HYDROFOVIC AEROGEL PANELS REINFORCED WITH FIBER FELT |
| CN105174274A (en) * | 2015-09-06 | 2015-12-23 | 广州大学 | Ambient preparation and control method of low-density SiO2 aerogel |
| KR101919121B1 (en) * | 2016-10-19 | 2018-11-16 | (주)대협테크 | Aerogel Composite and Preparation Method Thereof |
| CN107954687A (en) * | 2017-12-01 | 2018-04-24 | 四川科宁泰科技有限公司 | A kind of aerosil with ultralow thermal conductivity and preparation method thereof |
| CN108328620B (en) * | 2018-02-12 | 2021-08-24 | 南京工业大学 | Preparation method of hydrophobic foaming cement composite silicon aerogel material |
| CN110483004B (en) * | 2019-09-10 | 2022-03-29 | 航天海鹰(镇江)特种材料有限公司 | Aerogel preparation method for recycling glue solution |
| KR102403765B1 (en) * | 2019-12-10 | 2022-05-31 | 한국과학기술연구원 | Method of manufacturing superhydrophobic coating film coated with aerogel nanocomposite |
-
2021
- 2021-12-15 CN CN202111533985.0A patent/CN114620736B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 李威等.复合纤维增强疏水SiO_2气凝胶的制备及其性能.《材料导报B:研究篇》.2015,29(11),第72-74页，下转第95页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114620736A (en) | 2022-06-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11808032B2 (en) | Composite insulation including an inorganic aerogel and a melamine foam | |
| CN107140938B (en) | A kind of anti-shedding aeroge complex heat-preservation felt and preparation method thereof | |
| CN106189066B (en) | Phenolic resin/silicon dioxide composite aerogel material and preparation method thereof | |
| KR100710887B1 (en) | Method for manufacturing aerogel blanket | |
| US20220089503A1 (en) | Ceramic foams, methods of making same, and uses thereof | |
| KR20210014675A (en) | Fire Grade Reinforced Airgel Composition | |
| CN114634700B (en) | Aerogel modified polyurethane foam heat insulation board and preparation method thereof | |
| CN109336545A (en) | A kind of silicon dioxide silica aerogel composite material, preparation method and application | |
| CN105837244A (en) | Environment-friendly magnesium silicate fibrofelt-reinforced silica aerogel composite and preparation method thereof | |
| CN109053131A (en) | Oxidization fiber aerogel blanket and preparation method thereof | |
| JP2016540878A (en) | Benzimidazole airgel materials | |
| CN101698583A (en) | Multi-element aerogel composite material and preparation method thereof | |
| KR102666096B1 (en) | Continous manufacturing process for silica-aerogel adiabatic sheet having a continuous patterned insulation coating layer | |
| CN115710117A (en) | Aerogel composite material and preparation method and application thereof | |
| Gu et al. | Robust composite aerogel beads with pomegranate-like structure for water-based thermal insulation coating | |
| CN114620736B (en) | Compression-controllable SiO 2 Aerogel composite material preparation method | |
| CN114775298A (en) | Composite material containing graphene aerogel and preparation method and application thereof | |
| CN109626954A (en) | A kind of heatproof damp-proof silicon dioxide silica aerogel composite material and its preparation method and application | |
| CN111043450A (en) | Wave-transparent heat-insulation gas-barrier member and preparation method thereof | |
| CN115043408B (en) | Flexible silica aerogel, aerogel felt and preparation method thereof | |
| Shi et al. | A novel combustion drying technology for in-situ preparation of glass fiber composite SiO2 aerogel thin felt with excellent thermal insulation performance | |
| CN115772338A (en) | Heat-insulating flame-retardant nano composite sheet and preparation method thereof | |
| CN110407215A (en) | A kind of aerogel material heat-insulating composite panel and preparation method thereof | |
| CN110614691B (en) | Preparation method of densified wood-based graphene conductive composite material | |
| CN111943713A (en) | Environment-friendly heat-preservation and heat-insulation material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |