CN114149010B - Silica aerogel ball and preparation method thereof - Google Patents
Silica aerogel ball and preparation method thereof Download PDFInfo
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- CN114149010B CN114149010B CN202111538444.7A CN202111538444A CN114149010B CN 114149010 B CN114149010 B CN 114149010B CN 202111538444 A CN202111538444 A CN 202111538444A CN 114149010 B CN114149010 B CN 114149010B
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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
- 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
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention relates to a silica aerogel ball and a preparation method thereof, wherein the preparation method comprises the following steps of preparing a precursor and preparing acid liquor; mixing the prepared precursor and the prepared acid aqueous solution in a mass ratio of 1-3:1 in a pipeline mixer to form mixed solution, then spraying the mixed solution downwards from the top of a curing tower through a nozzle connected with the pipeline mixer, forming spherical gel by the sprayed liquid under the action of bottom-up wind sprayed from an air outlet pipe in the curing tower, and finally falling into water positioned at the bottom of the curing tower; the wind speed of the wind is 1-8 m/s and the temperature is 60-90 ℃; washing with water, soaking for replacement, and then modifying and drying to obtain the silica aerogel balls. According to the invention, a sol system is optimized, the gelation time is precisely controlled, circular liquid drops are formed in a free falling mode, the spherical gel is quickly solidified by controlling the countercurrent hot air of a curing tower, and finally, the spherical aerogel particles are prepared through water washing, modification and drying.
Description
Technical Field
The invention relates to an aerogel material and a preparation method thereof, in particular to a silicon dioxide aerogel ball and a preparation method thereof.
Background
The silica aerogel is a light nano-porous amorphous solid material with a space network structure, wherein the structure of the light nano-porous amorphous solid material is formed by cross-linking colloid particles or high polymer molecules. The porosity is up to 80% -99.8%, the pore size is 1-100 nm, and the specific surface area is up to 200-1000 m 2 The density variation range of the catalyst can reach 3-500 kg/m 3 . Aerogel has the characteristics of temperature resistance, heat insulation, extremely low heat conductivity and the like, is a solid material with the best heat insulation performance at present, and has unique characteristics in various aspects such as mechanics, acoustics, thermal and optics. Therefore, the material has wide application prospect in the fields of military industry, aerospace, medical use, high-speed trains, petrochemical industry, building materials and the like, and is called as a magic material for changing the world.
Aerogel products currently on the market are mainly composite materials of aerogel and fiber mats. The size of the uncomplexed aerogel is not easy to control due to structural brittleness, and the uncomplexed aerogel is usually in irregular particles or powder, so that the problem of stress concentration exists as a filling material, and the application scene of the silica aerogel is limited. The spherical aerogel particles have the characteristics of easy filling and difficult breaking, and have unique advantages as fillers. Therefore, how to obtain spherical aerogels is a hotspot in this field.
Patent CN 103787343a discloses a method for preparing microsphere aerogel based on super-hydrophobic surface, the product obtained by the method and its application, the method uses silica sol aqueous solution to gel on the super-hydrophobic surface to form microsphere, and prepares micron-sized aerogel pellets through aging, solvent replacement, surface modification, surface cleaning and drying treatment, and is characterized in that the water-soluble silica sol forms microsphere on the super-hydrophobic surface through the action of surface tension to gradually gel to form solidified spheres, the method has the defects of lower efficiency, long waiting time, unable continuous production, low utilization rate of special super-hydrophobic surface, and unsuitability for industrialized production.
Patent CN 101164881 discloses a method for preparing millimeter-sized silica aerogel balls, which is characterized in that spherical liquid drops are formed by the surface tension of an alcohol sol in soybean oil, gel is gradually formed in the rising process, and finally spherical alcohol gel is suspended at the interface between the soybean oil and ethanol and enters a supercritical system for drying after being cleaned and aged to prepare spherical aerogel, the method has particularly high production control requirement, the spherical gel needs to be cleaned to treat the soybean oil remained on the surface, and the flow is complex; secondly, the spherical alcogel avoids the unorganized diffusion of the organic solvent in the transfer process, brings hidden danger to the production safety and is not suitable for mass production.
Patent CN106422998 discloses a method for preparing aerogel microspheres, in which sol formed by water glass after being treated by ion exchange resin is dropped onto a platform containing aerogel powder, sol liquid beads coated by the aerogel powder are formed by means of large surface tension, and then Ph value is regulated by a method of injecting ammonia water through a needle tube.
The above-disclosed patents all use a precursor of silicon to form a sol, then in a nonpolar medium, spherical droplets are formed by spontaneous high surface tension, and then gel is gradually solidified. The formation and solidification efficiency of the liquid drops directly affect the production efficiency, and the method has the defects of complex solidification mode or long solidification waiting time, so that the industrial mass production is difficult to realize.
Disclosure of Invention
The invention provides a silicon dioxide aerogel ball and a preparation method thereof, and the method can prepare SiO 2 Spherical aerogel, whileThe method is simple, does not need other auxiliary media, has high production efficiency, and is suitable for industrial production.
The invention is realized by the following technical scheme:
the preparation method of the silica aerogel ball comprises the following steps:
1. and (3) configuring a precursor: the method comprises the steps of mixing potassium methyl silicate, silica sol, hydroxypropyl methylcellulose and water according to a mass ratio of 1: :0.01:4, mixing;
2. preparing acid liquor: preparing an acid water solution with the mass concentration of 20-40%;
3. mixing the precursor prepared in the first step and the acid aqueous solution prepared in the second step in a mass ratio of 1-3:1 in a pipeline mixer to form a mixed solution, then spraying the mixed solution downwards from the top of a curing tower through a nozzle connected with the pipeline mixer, forming spherical gel under the action of bottom-up wind sprayed from an air outlet pipe in the curing tower, and finally falling into water positioned at the bottom of the curing tower; the wind speed of the wind is 1-8 m/s and the temperature is 60-90 ℃;
4. washing gel balls obtained at the bottom of the curing tower in the step three with water, soaking and replacing the gel balls with ethanol aqueous solution, and then placing the gel balls in a modifier with the temperature of 60-75 ℃ for modification for 4-8 hours;
5. and finally, drying the gel ball modified in the step four at 70 ℃ for 2 hours, and drying the gel ball at 150 ℃ for 2 hours to obtain the silica aerogel ball.
Further, in the step one, the solid content of the potassium methyl silicate is 30-42%; the solid content of the silica sol is 25-30%.
Further, the acid in the second step is sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, acetic acid or oxalic acid.
Further, in the third step, the diameter of the nozzle is 0.5-2 mm.
Further, the temperature of the water at the bottom of the curing tower in the step three is 50-80 ℃.
Further, the height of the inner cavity of the curing tower in the third step is 5-20 m.
Further, the modifier in the fourth step comprises the following components in percentage by mass: 5 to 10 percent of trimethylchlorosilane and n-hexane.
Further, the water washing temperature in the fourth step is 50-80 ℃ for 2 times; soaking and replacing once by using an ethanol water solution with the temperature of 50-80 ℃ and the mass concentration of 75-95%.
Further, the curing tower include outer tower body, outer tower body top interval set up a plurality of first through-holes that are used for wearing to establish the nozzle and are used for the air-out of surface about being equipped with of outer tower body top, tower body lateral wall bottom be equipped with the second through-hole, the tuber pipe including be responsible for and a plurality of interval setting be responsible for the top and with be responsible for the branch pipe of intercommunication, be responsible for outside port connection air-blower and penetrate to the inner chamber of outer tower body from the second through-hole, the vertical upwards extension of branch pipe, bottom mouth of pipe and be responsible for the intercommunication, the top port is exposed above the surface of water of curing tower intussuseption packing.
The silica aerogel balls are prepared by the preparation method.
And (3) curing: the precursor prepared in the first step is firstly mixed in a pipeline mixer to form sol, the sol is connected to the top of a curing tower through a pipeline, hot water is filled at the bottom of the curing tower, a large number of branch pipes are distributed at the bottom of the curing tower, the pipe orifices of the branch pipes are exposed out of the water surface, and hot air from bottom to top is generated; the top of the curing tower is provided with an air outlet, a plurality of nozzles are uniformly distributed at the top of the curing tower, sol freely falls through the nozzles in the form of liquid drops, the liquid drops can roll under the action of hot air from bottom to top to quickly become spherical liquid beads in regular form, the liquid beads are quickly solidified by gel under the condition of hot air heating, and meanwhile, the falling speed of the liquid beads can be slowed down by hot air, so that the liquid beads are fully solidified by gel, and the solidified gel beads fall into hot water.
When the gel balls reach a certain quantity, the gel balls can be discharged together with hot water to enter the next procedure, and then new hot water is supplemented to the bottom of the tower at the same time.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, a sol system is optimized, the gelation time is precisely controlled, circular liquid drops are formed in a free falling mode, the spherical gel is quickly solidified by controlling the countercurrent hot air of a curing tower, and finally, the spherical aerogel particles are prepared through water washing, modification and drying. The invention has simple curing mode, does not need other auxiliary media, has high production efficiency and is suitable for industrial production.
Drawings
FIG. 1 is a schematic view of the structure and connection of the curing tower, the pipe mixer, the nozzle and the air outlet pipe of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings and detailed description.
Example 1
The preparation method of the silica aerogel ball comprises the following steps:
1. and (3) configuring a precursor: the method comprises the steps of mixing potassium methyl silicate, silica sol, hydroxypropyl methylcellulose and water according to a mass ratio of 1:0.5:0.01:4, mixing;
2. preparing acid liquor: preparing an acid aqueous solution with the mass concentration of 30%;
3. mixing the precursor prepared in the first step and the acid aqueous solution prepared in the second step in a mass ratio of 3:1 in a pipeline mixer 1 to form a mixed solution, then spraying the mixed solution downwards from the top of a curing tower 3 through a nozzle 2 connected with the pipeline mixer 1, forming spherical gel under the action of bottom-up wind sprayed from an air outlet pipe 4 in the curing tower, and finally falling into water positioned at the bottom of the curing tower; the wind speed of the wind is 4m/s and the temperature is 75 ℃;
4. washing and replacing the gel balls obtained at the bottom of the curing tower in the step three, and then placing the gel balls in a modifier with the temperature of 70 ℃ for modification for 6 hours;
5. and finally, drying the gel ball modified in the step four at 70 ℃ for 2 hours, and drying the gel ball at 150 ℃ for 2 hours to obtain the silica aerogel ball.
Step one, the solid content of the methyl potassium silicate is 35%; the solids content of the silica sol was 28%.
The acid in the second step is sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, acetic acid or oxalic acid.
And step three, the pH value of the sol discharged from the pipeline mixer is 7.
Step three the diameter of the nozzle 2 is 1mm.
And step three, the temperature of water at the bottom of the curing tower 3 is 65 ℃.
And step three, the height of the internal cavity of the curing tower 3 is 10m.
The mass ratio of the modifier in the fourth step is 1: and 8, mixing the trimethylchlorosilane with n-hexane.
Step four, washing with water at 65 ℃ for 2 times; the mixture was immersed in an aqueous ethanol solution at 65℃and a mass concentration of 85% for one time. The water washing is to remove salt in the gel ball, the volume ratio of water to the gel ball is 3:1, the replacement is to replace water in the gel ball with ethanol solution, and the volume ratio of the ethanol solution to the gel ball is 3:1.
The curing tower 3 comprises an outer tower body 3-1, a plurality of first through holes 3-2 penetrating through the upper surface and the lower surface of the top of the outer tower body 3-1 and an air outlet 3-3 used for air outlet are formed in the top of the outer tower body 3-1 at intervals, a second through hole 3-4 is formed in the bottom of the side wall of the tower body 1, the air outlet pipe 4 comprises a main pipe 4-1 and a plurality of branch pipes 4-2 which are arranged above the main pipe 4-1 at intervals and are communicated with the main pipe 4-1, external ports of the main pipe 4-1 are connected with a blower and penetrate into an inner cavity of the outer tower body 3-1 from the second through holes 3-4, the branch pipes 4-2 extend vertically upwards, bottom pipe orifices are communicated with the main pipe 4-1, and top ports are exposed above water surfaces filled in the curing tower 3.
Example 2
The preparation method of the silica aerogel ball comprises the following steps:
1. and (3) configuring a precursor: the method comprises the steps of mixing potassium methyl silicate, silica sol, hydroxypropyl methylcellulose and water according to a mass ratio of 1:1:0.01:4, mixing;
2. preparing acid liquor: preparing an acid aqueous solution with the mass concentration of 40%;
3. mixing the precursor prepared in the first step and the acid aqueous solution prepared in the second step in a mass ratio of 3:1 in a pipeline mixer 1 to form a mixed solution, then spraying the mixed solution downwards from the top of a curing tower 3 through a nozzle 2 connected with the pipeline mixer 1, forming spherical gel under the action of bottom-up wind sprayed from an air outlet pipe 4 in the curing tower, and finally falling into water positioned at the bottom of the curing tower; the wind speed of the wind is 8m/s and the temperature is 90 ℃;
4. washing and replacing the gel balls obtained at the bottom of the curing tower in the step three, and then placing the gel balls in a modifier with the temperature of 75 ℃ for modification for 8 hours;
5. and finally, drying the gel ball modified in the step four at 70 ℃ for 2 hours, and drying the gel ball at 150 ℃ for 2 hours to obtain the silica aerogel ball.
Step one, the solid content of the methyl potassium silicate is 42%; the solids content of the silica sol was 30%.
The acid in the second step is sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, acetic acid or oxalic acid.
And step three, the pH value of the sol discharged from the pipeline mixer is 8.
Step three the diameter of the nozzle 2 is 2mm.
And step three, the temperature of water at the bottom of the curing tower 3 is 80 ℃.
And step three, the height of the internal cavity of the curing tower 3 is 20m.
The mass ratio of the modifier in the fourth step is 1:10 and n-hexane.
Step four, washing with water at 80 ℃ for 2 times; the mixture was immersed in an aqueous ethanol solution having a mass concentration of 95% at 80℃for one time. The water washing is to remove salt in the gel ball, the volume ratio of water to the gel ball is 5:1, the replacement is to replace water in the gel ball with ethanol solution, and the volume ratio of the ethanol solution to the gel ball is 5:1.
The curing tower 3 comprises an outer tower body 3-1, a plurality of first through holes 3-2 penetrating through the upper surface and the lower surface of the top of the outer tower body 3-1 and an air outlet 3-3 used for air outlet are formed in the top of the outer tower body 3-1 at intervals, a second through hole 3-4 is formed in the bottom of the side wall of the tower body 1, the air outlet pipe 4 comprises a main pipe 4-1 and a plurality of branch pipes 4-2 which are arranged above the main pipe 4-1 at intervals and are communicated with the main pipe 4-1, external ports of the main pipe 4-1 are connected with a blower and penetrate into an inner cavity of the outer tower body 3-1 from the second through holes 3-4, the branch pipes 4-2 extend vertically upwards, bottom pipe orifices are communicated with the main pipe 4-1, and top ports are exposed above water surfaces filled in the curing tower 3.
Example 3
The preparation method of the silica aerogel ball comprises the following steps:
1. and (3) configuring a precursor: the method comprises the steps of mixing potassium methyl silicate, silica sol, hydroxypropyl methylcellulose and water according to a mass ratio of 1:0.8:0.01:4, mixing;
2. preparing acid liquor: preparing an acid aqueous solution with the mass concentration of 20%;
3. mixing the precursor prepared in the first step and the acid aqueous solution prepared in the second step in a mass ratio of 1:1 in a pipeline mixer 1 to form a mixed solution, then spraying the mixed solution downwards from the top of a curing tower 3 through a nozzle 2 connected with the pipeline mixer 1, forming spherical gel under the action of bottom-up wind sprayed from an air outlet pipe 4 in the curing tower, and finally falling into water positioned at the bottom of the curing tower; the wind speed of the wind is 1m/s and the temperature is 60 ℃;
4. washing and replacing the gel balls obtained at the bottom of the curing tower in the step three, and then placing the gel balls in a modifier with the temperature of 60 ℃ for modification for 4 hours;
5. and finally, drying the gel ball modified in the step four at 70 ℃ for 2 hours, and drying the gel ball at 150 ℃ for 2 hours to obtain the silica aerogel ball.
Step one, the solid content of the methyl potassium silicate is 30%; the solids content of the silica sol was 25%.
The acid in the second step is sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, acetic acid or oxalic acid.
And step three, the pH value of the sol discharged from the pipeline mixer is 5.
Step three the diameter of the nozzle 2 is 0.5mm.
And step three, the temperature of water at the bottom of the curing tower 3 is 50 ℃.
And step three, the height of the inner cavity of the curing tower 3 is 5m.
The mass ratio of the modifier in the fourth step is 1:5, and mixing the trimethylchlorosilane with n-hexane.
Step four, washing with water at 50 ℃ for 2 times; the mixture was immersed in an aqueous ethanol solution having a mass concentration of 75% at a temperature of 50℃for one time. The water washing is to remove salt in the gel ball, the volume ratio of water to the gel ball is 2:1, the replacement is to replace water in the gel ball with ethanol solution, and the volume ratio of the ethanol solution to the gel ball is 2:1.
The curing tower 3 comprises an outer tower body 3-1, a plurality of first through holes 3-2 penetrating through the upper surface and the lower surface of the top of the outer tower body 3-1 and an air outlet 3-3 used for air outlet are formed in the top of the outer tower body 3-1 at intervals, a second through hole 3-4 is formed in the bottom of the side wall of the tower body 1, the air outlet pipe 4 comprises a main pipe 4-1 and a plurality of branch pipes 4-2 which are arranged above the main pipe 4-1 at intervals and are communicated with the main pipe 4-1, external ports of the main pipe 4-1 are connected with a blower and penetrate into an inner cavity of the outer tower body 3-1 from the second through holes 3-4, the branch pipes 4-2 extend vertically upwards, bottom pipe orifices are communicated with the main pipe 4-1, and top ports are exposed above water surfaces filled in the curing tower 3.
Example 4
The preparation method of the silica aerogel ball comprises the following steps:
1. and (3) configuring a precursor: the method comprises the steps of mixing potassium methyl silicate, silica sol, hydroxypropyl methylcellulose and water according to a mass ratio of 1:0.8:0.01:4, mixing;
2. preparing acid liquor: preparing an acid aqueous solution with the mass concentration of 30%;
3. mixing the precursor prepared in the first step and the acid aqueous solution prepared in the second step in a mass ratio of 2:1 in a pipeline mixer 1 to form a mixed solution, then spraying the mixed solution downwards from the top of a curing tower 3 through a nozzle 2 connected with the pipeline mixer 1, forming spherical gel under the action of bottom-up wind sprayed from an air outlet pipe 4 in the curing tower, and finally falling into water positioned at the bottom of the curing tower; the wind speed of the wind is 5m/s and the temperature is 80 ℃;
4. washing and replacing the gel balls obtained at the bottom of the curing tower in the step three, and then placing the gel balls in a modifier with the temperature of 60 ℃ for modification for 8 hours;
5. and finally, drying the gel ball modified in the step four at 70 ℃ for 2 hours, and drying the gel ball at 150 ℃ for 2 hours to obtain the silica aerogel ball.
Step one, the solid content of the methyl potassium silicate is 30%; the solids content of the silica sol was 30%.
The acid in the second step is sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, acetic acid or oxalic acid.
And step three, the pH value of the sol discharged from the pipeline mixer is 6.
Step three the diameter of the nozzle 2 is 1mm.
And step three, the temperature of water at the bottom of the curing tower 3 is 60 ℃.
And step three, the height of the internal cavity of the curing tower 3 is 10m.
The mass ratio of the modifier in the fourth step is 1:5, and mixing the trimethylchlorosilane with n-hexane.
Step four, washing with water at 60 ℃ for 2 times; the mixture was immersed in an aqueous ethanol solution having a mass concentration of 92% at 60℃for one time. The water washing is to remove salt in the gel ball, the volume ratio of water to the gel ball is 5:1, the replacement is to replace water in the gel ball with ethanol solution, and the volume ratio of the ethanol solution to the gel ball is 5:1.
The curing tower 3 comprises an outer tower body 3-1, a plurality of first through holes 3-2 penetrating through the upper surface and the lower surface of the top of the outer tower body 3-1 and an air outlet 3-3 used for air outlet are formed in the top of the outer tower body 3-1 at intervals, a second through hole 3-4 is formed in the bottom of the side wall of the tower body 1, the air outlet pipe 4 comprises a main pipe 4-1 and a plurality of branch pipes 4-2 which are arranged above the main pipe 4-1 at intervals and are communicated with the main pipe 4-1, external ports of the main pipe 4-1 are connected with a blower and penetrate into an inner cavity of the outer tower body 3-1 from the second through holes 3-4, the branch pipes 4-2 extend vertically upwards, bottom pipe orifices are communicated with the main pipe 4-1, and top ports are exposed above water surfaces filled in the curing tower 3.
The present invention has been described above by way of example, but the present invention is not limited to the above specific embodiments, and many modifications are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (9)
1. A preparation method of silica aerogel balls is characterized by comprising the following steps: the method comprises the following steps:
1. and (3) configuring a precursor: the method comprises the steps of mixing potassium methyl silicate, silica sol, hydroxypropyl methylcellulose and water according to a mass ratio of 1: (0.5-1): 0.01:4, mixing;
2. preparing acid liquor: preparing an acid water solution with the mass concentration of 20-40%;
3. mixing the precursor prepared in the first step and the acid aqueous solution prepared in the second step in a mass ratio of 1-3:1 in a pipeline mixer (1) to form mixed liquid, then spraying the mixed liquid downwards from the top of a curing tower (3) through a nozzle (2) connected with the pipeline mixer (1), forming spherical gel under the action of air sprayed from an air outlet pipe (4) in the curing tower from bottom to top, and finally falling into water positioned at the bottom of the curing tower; the wind speed of the wind is 1-8 m/s and the temperature is 60-90 ℃;
4. washing gel balls obtained at the bottom of the curing tower in the step three with water, soaking and replacing the gel balls with an ethanol aqueous solution, and then placing the gel balls in a modifier with the temperature of 60-75 ℃ for modification for 4-8 hours;
5. finally, drying the gel ball modified in the step four at 70 ℃ for 2 hours, and drying the gel ball at 150 ℃ for 2 hours to obtain a silicon dioxide aerogel ball;
the mass ratio of the modifier in the fourth step is 1: 5-10 parts of trimethylchlorosilane and n-hexane.
2. The method for preparing silica aerogel balls according to claim 1, wherein: step one, the solid content of the methyl potassium silicate is 30-42%; the solid content of the silica sol is 25-30%.
3. The method for preparing silica aerogel balls according to claim 1, wherein: the acid in the second step is sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, acetic acid or oxalic acid.
4. The method for preparing silica aerogel balls according to claim 1, wherein: and step three, the diameter of the nozzle (2) is 0.5-2 mm.
5. The method for preparing silica aerogel balls according to claim 1, wherein: and thirdly, the temperature of water at the bottom of the curing tower (3) is 50-80 ℃.
6. The method for preparing silica aerogel balls according to claim 1, wherein: and thirdly, the height of the inner cavity of the curing tower (3) is 5-20 m.
7. The method for preparing silica aerogel balls according to claim 1, wherein: step four, washing with water at 50-80 ℃ for 2 times; soaking and replacing once by using an ethanol water solution with the temperature of 50-80 ℃ and the mass concentration of 75-95%.
8. The method for preparing silica aerogel balls according to claim 1, wherein: the solidifying tower (3) comprises an outer tower body (3-1), a plurality of first through holes (3-2) penetrating through the upper surface and the lower surface of the top of the outer tower body (3-1) and an air outlet (3-3) used for air outlet are formed in the top of the outer tower body (3-1) at intervals, second through holes (3-4) are formed in the bottom of the side wall of the outer tower body (3-1), the air outlet pipe (4) comprises a main pipe (4-1) and a plurality of branch pipes (4-2) which are arranged above the main pipe (4-1) at intervals and are communicated with the main pipe (4-1), external ports of the main pipe (4-1) are connected with a blower and penetrate into an inner cavity of the outer tower body (3-1) from the second through holes (3-4), the branch pipes (4-2) vertically extend upwards, bottom pipe orifices are communicated with the main pipe (4-1), and the top ports are exposed above water surfaces filled in the solidifying tower (3).
9. A silica aerogel sphere characterized by: prepared by the preparation method of any one of claims 1 to 8.
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| DE19722738A1 (en) * | 1997-05-30 | 1998-12-03 | Hoechst Ag | Process for the production of essentially spherical lyogels and aerogels |
| CN103073008A (en) * | 2013-01-31 | 2013-05-01 | 中国科学技术大学 | Preparation method of silicon dioxide aerogel |
| CN106185959B (en) * | 2016-09-14 | 2018-04-06 | 纳诺科技有限公司 | A kind of method that aeroge is quickly prepared using microemulsion as precursor |
| WO2018170772A1 (en) * | 2017-03-22 | 2018-09-27 | 伊科纳诺（北京）科技发展有限公司 | Method for preparing silicon dioxide aerogel at atmospheric pressure and prepared silicon dioxide aerogel |
| CN111302348B (en) * | 2020-04-08 | 2022-01-18 | 天津纳科世纪新材料有限公司 | Normal pressure preparation method of silicon dioxide aerogel spherical particles |
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