CN115490239A - Organic silicon hydrophobic modifier, preparation method and application thereof, and preparation method of silicon dioxide aerogel - Google Patents
Organic silicon hydrophobic modifier, preparation method and application thereof, and preparation method of silicon dioxide aerogel Download PDFInfo
- Publication number
- CN115490239A CN115490239A CN202211245516.3A CN202211245516A CN115490239A CN 115490239 A CN115490239 A CN 115490239A CN 202211245516 A CN202211245516 A CN 202211245516A CN 115490239 A CN115490239 A CN 115490239A
- Authority
- CN
- China
- Prior art keywords
- silicic acid
- solution
- nitrogen
- acid gel
- modifier
- 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.)
- Granted
Links
Images
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
-
- 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
-
- 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
-
- 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
- C01B33/159—Coating or hydrophobisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2006/10—Solid density
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides an organosilicon hydrophobic modifier, a preparation method and application thereof, and a preparation method of silicon dioxide aerogel.
Description
Technical Field
The invention belongs to the technical field of new material preparation, and particularly relates to an organic silicon hydrophobic modifier, a preparation method and application thereof, and a preparation method of silicon dioxide aerogel.
Background
The silica aerogel is a novel thermal insulation material with excellent performance, has many superior characteristics of low heat transfer coefficient, light volume weight, non-combustibility, water resistance, moisture resistance, wide applicable temperature range and the like, and has wide application prospect. In the preparation process of the silica aerogel, hydrophobic modification of materials by using a hydrophobic modifier is involved. Because residual hydrogen chloride exists in the preparation process of the existing organosilicon hydrophobic modifier, when the aerogel is prepared, the material is subjected to hydrophobic modification, a hydrogen chloride gas byproduct is generated, the production equipment is easily corroded, and the possibility that residual hydrogen chloride components are attached to products exists, so that the application occasions of the products are limited.
Disclosure of Invention
In view of the above, in order to solve the above problems, the present invention provides an organosilicon hydrophobic modifier, a preparation method and an application thereof, and a preparation method of silica aerogel. According to the invention, cheap trimethylchlorosilane is used as a raw material, and is converted into trimethylethoxysilane through steps of alcoholysis, displacement dechlorination, neutralization and the like, and the trimethylethoxysilane is used as a modifier for preparing the silica aerogel.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention provides a preparation method of an organic silicon hydrophobic modifier, which comprises the following steps:
s1, preparing a trimethylchlorosilane solution with the concentration of 25-35 wt%, wherein the solvent is n-hexane;
s2, preparing an ethanol-n-hexane mixed solution, wherein the molar ratio of ethanol to n-hexane is preferably 1:1, and the molar ratio of ethanol to trimethylchlorosilane in S1 is 1.05-1.3: 1;
s3, slowly dripping ethanol-normal hexane mixed solution into the reaction container containing the trimethylchlorosilane solution under the condition of stirring at the temperature of 50-65 ℃; introducing nitrogen or mixed gas of nitrogen and ammonia into the reaction container during the adding process, condensing the overflowed gas, sending the condensate back into the reaction container, and sending out and eluting the gas; the condensation temperature is controlled to be 5-10 ℃, so that other components volatilized with the nitrogen flow back to the reaction vessel, and the hydrogen chloride is sent out along with the nitrogen and eluted;
s4, after the dropwise addition is finished, continuously introducing nitrogen or mixed gas of nitrogen and ammonia, and preserving heat;
s5, cooling to room temperature after heat preservation is finished; when the introduced nitrogen is nitrogen, cooling to room temperature, stopping introducing the nitrogen, starting introducing dried ammonia until the gas flowing out of the reaction vessel is alkaline, and stopping introducing the ammonia; when the mixed gas of nitrogen and ammonia is introduced, the mixed gas of nitrogen and ammonia is stopped after the temperature is reduced to the room temperature;
s6, standing and layering, and taking supernatant to obtain a mixed solution of an organic silicon hydrophobic modifier with a main component of trimethylethoxysilane and n-hexane;
s7, removing n-hexane to obtain the target product, namely the organic silicon hydrophobic modifier of the trimethylethoxysilane.
Wherein, ethanol and normal hexane in S1 and S2 are dehydrated in advance;
furthermore, in the step S3, the dripping time is controlled to be 3-4 h.
Further, in the step S4, the heat preservation time is 36-48 h.
The invention also provides an organic silicon hydrophobic modifier prepared by the preparation method.
The invention also provides application of the organosilicon hydrophobic modifier in preparing silica aerogel.
In another aspect, the present invention provides a method for preparing a silica aerogel, comprising the steps of:
step one, preparing silicic acid sol;
step two, removing salt contained in the silicic acid sol and adjusting the pH value to obtain silicic acid gel;
step three, carrying out solvent replacement on the silicic acid gel, removing water contained in the silicic acid gel, and converting the silicic acid gel into a non-hydrogel system;
step four, adopting the organic silicon hydrophobic modifier in claim 4 to carry out hydrophobic modification on the silicic acid gel after solvent replacement;
step five, performing solvent replacement on the hydrophobically modified silicic acid gel, and eluting impurities;
and step six, drying the silicic acid gel subjected to solvent replacement in the step five to obtain the silicon dioxide aerogel.
Further, in the first step, under the condition of stirring at the temperature of not higher than 12 ℃, dropwise adding 25wt% -35 wt% of sodium silicate solution into 18wt% -25 wt% of sulfuric acid solution, wherein the dropwise adding time can be controlled within 3-5 h, and when the pH value reaches 5.6-5.7, the dropwise adding is stopped, so that the solution containing the silicic acid sol is obtained.
Further, in the second step, the solution containing the silicic acid sol is filtered, filtrate is taken, and 25wt% -35 wt% of water in the filtrate can be removed by adopting a reduced pressure distillation mode at 55 ℃ -65 ℃; dropwise adding 2-3.5 wt% of sodium hydroxide solution, measuring the pH value, adjusting the pH value of the residual filtrate to 6.2-6.3, adding ethanol with the same volume as the filtrate, and standing; and (3) filtering to remove precipitated solids, adjusting the pH value of the filtrate to 6.7-6.9 by dripping 0.8wt% of ammonia water and measuring the pH value, standing for 20-30 min to obtain the silicic acid gel.
Further, in the third step, the silicic acid gel is subjected to solvent replacement by absolute ethyl alcohol (or n-hexane), absolute ethyl alcohol with the same volume as the silicic acid gel is added, the mixture is kept stand for more than 12 hours at room temperature, ethyl alcohol is poured out, a new batch of absolute ethyl alcohol is added, the mixture is kept stand for more than 12 hours, and the solvent replacement is completed by repeating the steps twice.
Further, in the fourth step, silicic acid gel is soaked in a modifier solution; the concentration of the modifier solution is 8-15 wt%; the molar ratio of the modifier to the silicon of the silica gel is 0.3-0.7: 1.
further, in the fourth step, the length of time for soaking the silicic acid gel in the modifier solution is more than 24 hours.
Further, in the fifth step, absolute ethyl alcohol, absolute isopropanol, absolute methanol, absolute acetone, n-hexane, n-heptane or 2-isooctane is adopted to carry out solvent replacement on the hydrophobically modified silicic acid gel for multiple times.
Soaking the hydrophobically modified silicic acid gel for more than 12 hours by using absolute ethyl alcohol, absolute isopropanol, absolute methanol, absolute acetone, normal hexane, normal heptane or 2-isooctane as a solvent to complete one-time solvent replacement; pouring out the solvent, adding a new batch of solvent, standing for more than 12h, and repeating twice to complete solvent replacement.
Further, in the sixth step, the drying mode is normal pressure heating drying or high temperature and high pressure supercritical drying.
Heating and drying under normal pressure: and (3) transferring the silicic acid gel to a flat tray, spreading the silicic acid gel, placing the silicic acid gel in an electric heating air blast drying box, gradually heating the silicic acid gel to 150 ℃ from room temperature at normal pressure, keeping the temperature for a period of time, stopping heating and preserving the heat, and taking out the tray when the temperature is reduced to be close to the room temperature to obtain the silicon dioxide aerogel particles dried at normal pressure.
High-temperature high-pressure supercritical drying: and (3) putting the silicic acid gel into a high-pressure kettle, and performing supercritical drying by using carbon dioxide gas or ethanol gas as a mobile phase to obtain silicon dioxide aerogel particles.
Compared with the prior art, the organosilicon hydrophobic modifier, the preparation method and the application thereof, and the preparation method of the silicon dioxide aerogel have the following advantages:
according to the invention, trimethylchlorosilane with lower price is used as a raw material to prepare the trimethylethoxysilane hydrophobizing agent, dechlorination is carried out in the preparation process, hydrogen chloride is removed, the condition that hydrogen chloride gas byproducts are generated in the aerogel preparation process to corrode production equipment is avoided, and the application occasion limitation caused by the residual components of hydrogen chloride attached in the product is avoided.
Drawings
FIG. 1 is a scanning electron micrograph of the silica aerogel obtained in example 1;
FIG. 2 is a scanning electron micrograph of the silica aerogel obtained in example 2.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are all conventional methods unless otherwise specified.
The present invention will be described in detail below with reference to the following examples and the accompanying drawings.
Example 1
1. Preparation of an organosilicon hydrophobic modifier
1) Adding 0.5mol of trimethylchlorosilane and 1.5mol of dehydrated normal hexane into a 500ml four-mouth bottle, and installing a stirrer, an aeration conduit, a condenser tube and a dropping funnel;
2) 0.55mol of dehydrated absolute ethyl alcohol is taken to be uniformly mixed with 0.55mol of dehydrated normal hexane and added into a dropping funnel;
3) Immersing the four-mouth bottle in a temperature-controlled oil bath, heating to 55 ℃, and starting stirring; opening a nitrogen bottle, adjusting the flow rate to 10 ml/min-15 ml/min, blowing nitrogen into the four-mouth bottle, simultaneously leading out overflowed gas from the outlet end of a condenser to a gas washing bottle, and circularly introducing refrigerating fluid at 5-10 ℃ into the condenser; opening a dropping funnel, dropwise adding an ethanol-n-hexane solution into the four-mouth bottle, and finishing dropping within 3 hours;
4) After the dropwise addition is finished, keeping the temperature of ventilation and oil bath for 40h;
5) After the heat preservation is finished, cooling to room temperature, switching nitrogen gas into dried ammonia gas for 10min, and stopping introducing ammonia gas;
6) Standing for layering, and taking supernatant to obtain a mixed solution of an organic silicon hydrophobic modifier with a main component of trimethylethoxysilane and n-hexane;
7) And removing the normal hexane to obtain the target product, namely the organic silicon hydrophobic modifier of the trimethylethoxysilane.
2. Preparation of silica aerogels
1) Adding 2L of 25wt% sulfuric acid solution into a 5L sandwich glass kettle, and introducing 5-10 ℃ refrigerating fluid into a jacket to reduce the temperature of the sulfuric acid solution in the kettle to below 12 ℃;
2) Slowly dripping 35% sodium silicate solution into the kettle under the condition of stirring, controlling the temperature in the kettle to be not higher than 12 ℃, measuring the pH value, and stopping dripping the sodium silicate solution when the pH value reaches 5.6-5.7;
3) Discharging the materials in the kettle, filtering, and distilling the filtrate at 60 ℃ under reduced pressure to remove 30wt% of water; cooling the dehydrated solution to room temperature, adjusting the pH value to 6.2 by using a 3% sodium hydroxide solution, adding 95% ethanol with the same volume as the solution, and standing; filtering to remove precipitated solid, adjusting pH of the filtrate to 6.8 with 0.2M ammonia water, and standing at room temperature for about 30min to obtain silicic acid gel;
4) Carrying out solvent replacement on the silicic acid gel by using absolute ethyl alcohol, adding the absolute ethyl alcohol with the same volume as the silicic acid gel, standing at room temperature for more than 12h, pouring out the ethyl alcohol, adding a new batch of absolute ethyl alcohol, standing for more than 12h, and repeating twice to finish the solvent replacement;
5) Soaking the replaced silica gel for more than 24 hours at 50 ℃ by using the prepared organic silicon hydrophobic modifier solution of trimethylethoxysilane, wherein the silicon molar ratio of the modifier to the silica gel is 0.7:1;
6) Filtering out the modifier solution, eluting the hydrophobically modified silicic acid gel by using a normal hexane solvent, and staying for more than 12 hours each time; after twice elution, the solvent is filtered off;
7) And transferring the silicic acid gel to a flat tray, spreading the silicic acid gel, placing the silicic acid gel in an electric heating air blowing drying box, heating the silicic acid gel to 150 ℃ from room temperature at the speed of 1 ℃/min under normal pressure, keeping the temperature for 2 hours, and cooling to obtain the silicon dioxide aerogel.
As shown in fig. 1, a scanning electron micrograph of the resulting silica aerogel;
the bulk density of the resulting silica aerogel was determined to be 70kg/m 3 The thermal conductivity coefficient is 0.017W/m.K.
Example 2
1. Preparation of an organosilicon hydrophobic modifier
1) Adding 1mol of trimethylchlorosilane and 2.5mol of dehydrated normal hexane into a 1000ml four-mouth bottle, and installing a stirrer, an aeration conduit, a condenser tube and a dropping funnel;
2) Taking 1.2mol of dehydrated absolute ethyl alcohol, mixing with 1.2mol of dehydrated normal hexane uniformly, and adding into a dropping funnel;
3) Immersing the four-mouth bottle in a temperature-controlled oil bath, heating to 55 ℃, and starting stirring; opening a nitrogen gas bottle and an ammonia gas bottle, regulating the introduction ratio of ammonia gas and nitrogen gas to 1:4 through an air flow mixing valve, setting the total flow rate of mixed gas at 10 ml/min-15 ml/min, blowing the mixed gas into the four-mouth bottle, simultaneously leading out overflowed gas from the outlet end of a condenser to a gas washing bottle, and circularly introducing refrigerating fluid at 5-10 ℃ into the condenser; opening a dropping funnel, and dropwise adding an ethanol-n-hexane solution into the four-mouth bottle for 4 hours;
4) After the dropwise addition is finished, keeping the temperature of ventilation and oil bath for 36h;
5) After the heat preservation is finished, cooling to room temperature, and stopping introducing the mixed gas;
6) Standing for layering, and taking supernatant to obtain a mixed solution of an organic silicon hydrophobic modifier with a main component of trimethylethoxysilane and n-hexane;
7) And removing the normal hexane to obtain the target product, namely the organic silicon hydrophobic modifier of the trimethylethoxysilane.
2. Preparation of silica aerogels
1) Adding 2L of 25wt% sulfuric acid solution into a 5L sandwich glass kettle, and introducing 5-10 ℃ refrigerating fluid into a jacket to reduce the temperature of the sulfuric acid solution in the kettle to below 12 ℃;
2) Slowly dripping 35% sodium silicate solution into the kettle under the condition of stirring, controlling the temperature in the kettle to be not higher than 12 ℃, measuring the pH value, and stopping dripping the sodium silicate solution when the pH value reaches 5.6-5.7;
3) Discharging the materials in the kettle, filtering, and distilling the filtrate at 60 ℃ under reduced pressure to remove 30wt% of water; cooling the dehydrated solution to room temperature, adjusting the pH value to 6.2 by using a 3% sodium hydroxide solution, adding 95% ethanol with the same volume as the solution, and standing; filtering to remove precipitated solid, adjusting pH of the filtrate to 6.8 with 0.2M ammonia water, and standing at room temperature for about 30min to obtain silicic acid gel;
4) Performing solvent replacement on the silicic acid gel by using absolute ethyl alcohol, adding the absolute ethyl alcohol with the same volume as the silicic acid gel, standing at room temperature for more than 12h, pouring out the ethyl alcohol, adding a new batch of absolute ethyl alcohol, standing for more than 12h, and repeating twice to complete solvent replacement;
5) Soaking the replaced silica gel for more than 24 hours at 50 ℃ by using the prepared organic silicon hydrophobic modifier solution of trimethylethoxysilane, wherein the silicon molar ratio of the modifier to the silica gel is 0.5:1;
6) Filtering out the modifier solution, eluting the hydrophobically modified silicic acid gel with a normal hexane solvent, and staying for more than 12 hours each time; after twice elution, the solvent is filtered off;
7) Transferring the silicic acid gel into a high-pressure kettle, taking carbon dioxide as a mobile phase, performing supercritical drying at 120 ℃ and 30MPa until the partial pressure of distilled carbon dioxide is constant, reducing pressure and cooling, and taking the material out of the kettle to obtain the silicon dioxide aerogel.
As shown in fig. 2, a scanning electron micrograph of the obtained silica aerogel;
the bulk density of the obtained silica aerogel was determined to be 58kg/m 3 The thermal conductivity coefficient is 0.016W/m.K.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of an organosilicon hydrophobic modifier is characterized by comprising the following steps:
s1, preparing a trimethylchlorosilane solution with the concentration of 25-35 wt%, wherein a solvent is n-hexane;
s2, preparing an ethanol-n-hexane mixed solution, wherein the molar ratio of ethanol to trimethylchlorosilane in the S1 is 1.05-1.3: 1;
s3, slowly dripping an ethanol-n-hexane mixed solution into a reaction container containing a trimethylchlorosilane solution under the condition of stirring at the temperature of 50-65 ℃; introducing nitrogen or mixed gas of nitrogen and ammonia into the reaction container during the adding process, condensing the overflowed gas, sending the condensate back into the reaction container, and sending out and eluting the gas; the condensation temperature is controlled to be 5-10 ℃;
s4, after the dropwise addition is finished, continuously introducing nitrogen or mixed gas of nitrogen and ammonia, and preserving heat;
s5, cooling to room temperature after heat preservation is finished; when the introduced nitrogen is nitrogen, cooling to room temperature, stopping introducing the nitrogen, starting introducing dried ammonia until the gas flowing out of the reaction vessel is alkaline, and stopping introducing the ammonia; when the mixed gas of nitrogen and ammonia is introduced, the mixed gas of nitrogen and ammonia is stopped after the temperature is reduced to the room temperature;
s6, standing and layering, and taking supernatant to obtain a mixed solution of an organic silicon hydrophobic modifier with a main component of trimethylethoxysilane and n-hexane;
s7, removing n-hexane to obtain the target product, namely the organic silicon hydrophobic modifier of the trimethylethoxysilane.
2. The method of preparing the organosilicon hydrophobic modifier of claim 1, characterized in that: and in the S3, the dripping time is controlled to be 3-4 h.
3. The method of preparing the organosilicon hydrophobic modifier of claim 1, characterized in that: in the step S4, the heat preservation time is 36-48 h.
4. An organosilicon hydrophobic modifier prepared by the preparation method of any one of claims 1 to 3.
5. Use of the silicone hydrophobic modifier of claim 4, characterized in that: application in preparing silica aerogel.
6. The preparation method of the silicon dioxide aerogel is characterized by comprising the following steps:
step one, preparing silicic acid sol;
step two, removing salt contained in the silicic acid sol and adjusting the pH value to obtain silicic acid gel;
step three, carrying out solvent replacement on the silicic acid gel, removing water contained in the silicic acid gel, and converting the silicic acid gel into a non-hydrogel system;
step four, adopting the organic silicon hydrophobic modifier in claim 4 to carry out hydrophobic modification on the silicic acid gel after solvent replacement;
step five, performing solvent replacement on the hydrophobically modified silicic acid gel, and eluting impurities;
and step six, drying the silicic acid gel subjected to solvent replacement in the step five to obtain the silicon dioxide aerogel.
7. The method for preparing silica aerogel according to claim 6, characterized in that: in the first step, under the condition of stirring at the temperature of not higher than 12 ℃, 25-35 wt% of sodium silicate solution is dripped into 18-25 wt% of sulfuric acid solution, and when the pH value reaches 5.6-5.7, the dripping is stopped, so that the solution containing silicic acid sol is obtained.
8. The method for preparing silica aerogel according to claim 6, characterized in that: in the second step, filtering the solution containing the silicic acid sol, taking filtrate, and removing 25-35 wt% of water in the filtrate; adjusting the pH value of the residual filtrate to 6.2-6.3, adding ethanol, and standing; filtering to remove precipitated solids, adjusting the pH value of the filtrate to 6.7-6.9, and standing to obtain the silicic acid gel.
9. The method for preparing silica aerogel according to claim 6, characterized in that: in the fourth step, silicic acid gel is soaked in a modifier solution; the concentration of the modifier solution is 8-15 wt%; the molar ratio of the modifier to the silicon of the silica gel is 0.3-0.7: 1.
10. the method for preparing silica aerogel according to claim 6, characterized in that: in the sixth step, the drying mode is normal pressure heating drying or high temperature high pressure supercritical drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211245516.3A CN115490239B (en) | 2022-10-12 | 2022-10-12 | Organosilicon hydrophobic modifier, preparation method and application thereof, and preparation method of silica aerogel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211245516.3A CN115490239B (en) | 2022-10-12 | 2022-10-12 | Organosilicon hydrophobic modifier, preparation method and application thereof, and preparation method of silica aerogel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115490239A true CN115490239A (en) | 2022-12-20 |
| CN115490239B CN115490239B (en) | 2023-10-13 |
Family
ID=84474449
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211245516.3A Active CN115490239B (en) | 2022-10-12 | 2022-10-12 | Organosilicon hydrophobic modifier, preparation method and application thereof, and preparation method of silica aerogel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115490239B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613367A (en) * | 2009-07-22 | 2009-12-30 | 吉林新亚强生物化工有限公司 | The preparation method of trimethylethoxysilane |
| CN102020285A (en) * | 2009-09-16 | 2011-04-20 | 深圳大学 | Preparation method for hydrophobic silica aerogel |
| CN102219802A (en) * | 2011-04-15 | 2011-10-19 | 北京秀珀科技发展有限公司 | Method for preparing novel isobutyl triethoxy silane |
| CN102718791A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation process of trimethylethoxysilane |
| CN104262380A (en) * | 2014-08-21 | 2015-01-07 | 湖北兴发化工集团股份有限公司 | Preparation method of methyltrialkoxysilane |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| CN109232633A (en) * | 2018-11-16 | 2019-01-18 | 江西晨光新材料股份有限公司 | A kind of one methoxy silane of trimethyl-hexamethyldisilazane combined preparation process |
| CN109650396A (en) * | 2019-01-28 | 2019-04-19 | 安徽科昂纳米科技有限公司 | A kind of preparation method of aerosil and aerosil obtained |
-
2022
- 2022-10-12 CN CN202211245516.3A patent/CN115490239B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613367A (en) * | 2009-07-22 | 2009-12-30 | 吉林新亚强生物化工有限公司 | The preparation method of trimethylethoxysilane |
| CN102020285A (en) * | 2009-09-16 | 2011-04-20 | 深圳大学 | Preparation method for hydrophobic silica aerogel |
| CN102219802A (en) * | 2011-04-15 | 2011-10-19 | 北京秀珀科技发展有限公司 | Method for preparing novel isobutyl triethoxy silane |
| CN102718791A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation process of trimethylethoxysilane |
| CN104262380A (en) * | 2014-08-21 | 2015-01-07 | 湖北兴发化工集团股份有限公司 | Preparation method of methyltrialkoxysilane |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| CN109232633A (en) * | 2018-11-16 | 2019-01-18 | 江西晨光新材料股份有限公司 | A kind of one methoxy silane of trimethyl-hexamethyldisilazane combined preparation process |
| CN109650396A (en) * | 2019-01-28 | 2019-04-19 | 安徽科昂纳米科技有限公司 | A kind of preparation method of aerosil and aerosil obtained |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115490239B (en) | 2023-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101187568B1 (en) | Preparation method of silica aerogel granules | |
| CN106747541B (en) | Method for in-situ synthesis of mullite whisker self-toughened mullite ceramic | |
| US20080081014A1 (en) | Rapid preparation process of aerogel | |
| CN109734412B (en) | Secondary drying method for preparing hydrophobic aluminum-silicon aerogel heat insulation material | |
| CN112174144A (en) | Ultrahigh-transparency large-size block silica aerogel and preparation method and application thereof | |
| WO2019075793A1 (en) | Method for continuously preparing boron-doped sio2 aerogel | |
| KR20110125773A (en) | Manufacturing method of hydrophobic silica aerogel and hydrophobic silica aerogel manufactured therefrom | |
| CN110723738B (en) | Preparation method of enhanced silica aerogel, enhanced silica aerogel and application thereof | |
| CN115448719B (en) | High-entropy block ceramic aerogel with high-temperature stability and preparation method and application thereof | |
| KR100867466B1 (en) | Method for Preparing Permanently Hydrophobic Aerogel Powder Having Increased Particle Size and Density And Aerogel Powder Therefrom | |
| WO2009038393A2 (en) | Method for preparing surface-modified transparent bead type aerogel and aerogel prepared therefrom | |
| WO2008038935A1 (en) | Method of fabricating superhydrophobic silica chain powders | |
| CN110615663A (en) | Solid wood fiber/SiO2Aerogel composite thermal insulation material and preparation method thereof | |
| CN101638237B (en) | Method for quickly preparing silicondioxlde aerogel | |
| WO2013189247A1 (en) | Method for preparing bulk c-aln composite aerogel with high strength and high temperature resistance | |
| CN106366315A (en) | Powder silicon resin and preparation method thereof | |
| CN115490239A (en) | Organic silicon hydrophobic modifier, preparation method and application thereof, and preparation method of silicon dioxide aerogel | |
| KR100729947B1 (en) | Sol-gel process for the production of glassy articles | |
| CN102198943A (en) | Method for preparing silicon-based aerogel with different contact angles by drying with low cost under normal pressure | |
| CN109679588B (en) | Method for preparing polyethylene glycol phase change heat conduction composite material by controllable sol-gel method and application | |
| CN115806427A (en) | Low-cost SiO 2 Method for producing aerogels | |
| CN113735148B (en) | Preparation method of high-temperature-resistant massive alumina aerogel | |
| CN110627977A (en) | Preparation method of graphene oxide grafted styrene | |
| CN115583656B (en) | Method for preparing silicon dioxide aerogel through carbon dioxide aqueous solution conversion | |
| CN110498418A (en) | A kind of preparation method being alkylated large aperture capacity silicon oxide aeroge |
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 |