CN111302348A - Normal pressure preparation method of silicon dioxide aerogel spherical particles - Google Patents
Normal pressure preparation method of silicon dioxide aerogel spherical particles Download PDFInfo
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- CN111302348A CN111302348A CN202010269026.1A CN202010269026A CN111302348A CN 111302348 A CN111302348 A CN 111302348A CN 202010269026 A CN202010269026 A CN 202010269026A CN 111302348 A CN111302348 A CN 111302348A
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- 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
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- C01B33/1585—Dehydration into aerogels
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Abstract
An atmospheric pressure preparation method of silica aerogel spherical particles comprises the following steps: (1) preparing a sodium silicate aqueous solution and a sulfuric acid aqueous solution; (2) adding a sodium silicate aqueous solution into a surfactant, uniformly stirring, then adding the sodium silicate aqueous solution and a sulfuric acid aqueous solution into a mixer simultaneously by using a high-pressure pump, uniformly mixing, and spraying the mixture into air through a nozzle for granulation; (3) collecting the wet balls in water, heating, curing, and washing with tap water; (4) adding the generated material into a displacement kettle, adding n-butyl alcohol, heating to boil, forming an azeotrope by the n-butyl alcohol and water, carrying out organic solvent displacement on the azeotrope through oil-water separation, stopping heating, and discharging; (5) and (3) carrying out vacuum drying on the generated material by adopting a vacuum drying box, heating to raise the temperature, and drying to obtain the spherical silicon dioxide aerogel.
Description
Technical Field
The invention relates to the technical field of silica aerogel inorganic materials, in particular to a normal-pressure preparation method of spherical particles of silica aerogel.
Background
The silica-silica aerogel has specific optical property, dielectric property and optical property as a functional material, and is widely applied to various aspects of electronics, building heat preservation and the like. The silicon dioxide aerogel products which are in the market and are mature day by day comprise silicon dioxide aerogel powder materials, silicon dioxide aerogel heat preservation felts, silicon dioxide aerogel forming bodies, silicon dioxide aerogel coatings and the like. The silicon dioxide powder material only has powder with the granularity of about 10 microns at present, and needs multilayer hanging coating in thick paste heat-insulating putty, and the coating performance is reduced due to the multilayer hanging coating, so that the further application of the silicon dioxide coating market is influenced.
Some existing methods for preparing silica aerogel particles adopt sodium silicate as a raw material, firstly prepare silica sol through ion exchange, then drop the silica sol into an oil column, wash the gel with an organic solvent to remove oil, then prepare alcohol sol, and prepare the spherical silica aerogel through supercritical drying.
It can be seen that there is a need in the art for a method for preparing silica aerogel sphere-type particles that overcomes the above-mentioned drawbacks of the prior art.
Disclosure of Invention
According to an embodiment of the present invention, there is provided an atmospheric pressure preparation method of silica aerogel spherical particles, the method including the steps of:
(1) adding water into sodium silicate to prepare a sodium silicate aqueous solution, adding water into sulfuric acid to prepare a sulfuric acid aqueous solution, and settling the sulfuric acid aqueous solution and the sulfuric acid aqueous solution for later use;
(2) adding a surfactant into the sodium silicate aqueous solution, uniformly stirring, adding the sodium silicate aqueous solution and the sulfuric acid aqueous solution into a mixer simultaneously by using a high-pressure pump, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the pH value of an outlet of the nozzle to generate wet balls;
(3) collecting the wet balls in water, curing, and washing by using tap water;
(4) adding the material generated in the step (3) into a displacement kettle, adding n-butyl alcohol, heating until the n-butyl alcohol and water form an azeotrope when the n-butyl alcohol and the water are boiled, carrying out organic solvent displacement on the azeotrope through oil-water separation, and then discharging;
(5) and (5) carrying out vacuum drying on the material generated in the step (4) by adopting a vacuum drying oven, thereby preparing the spherical silicon dioxide aerogel.
According to the method for preparing the silica aerogel spherical particles under normal pressure, disclosed by the embodiment of the invention, industrial sodium silicate is used as a raw material, the process is simple, the cost is low, the industrialization is facilitated, and the particle size of the formed aerogel particles can reach 1-5 mm.
Drawings
FIG. 1 shows a flow diagram of silica aerogel ball-type particles according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below with reference to the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention to those skilled in the art. It will be apparent, however, to one skilled in the art that the present invention may be practiced without some of these specific details. Furthermore, it should be understood that the invention is not limited to the specific embodiments described. Rather, it is contemplated that the invention may be practiced with any combination of the following features and elements, whether or not they relate to different embodiments. Thus, the following aspects, features, embodiments and advantages are merely illustrative and should not be considered elements or limitations of the claims except where explicitly recited in a claim. The meaning of each term referred to in this specification is generally a meaning commonly understood in the art or a meaning normally understood by those skilled in the art after reading this specification. The terms "comprising" and "including" in this specification are open-ended, i.e., may include additional elements not already mentioned in addition to the elements already mentioned. The specific values of the contents of the components described in the present specification are only used to indicate a proportional relationship between the contents of the components, and are not used to limit the contents of the components to any absolute values. Specific values for the amounts of ingredients and specific values for the process parameters described in this specification are intended to be inclusive, e.g., 15% inclusive, and not intended to be limiting to a precise value.
Referring now to fig. 1, a method of atmospheric pressure preparation of silica aerogel sphere-type particles according to embodiments of the present invention is shown. As shown in fig. 1, the method comprises the steps of:
(1) adding water into sodium silicate to prepare a sodium silicate aqueous solution, adding water into sulfuric acid to prepare a sulfuric acid aqueous solution, and settling the sulfuric acid aqueous solution and the sulfuric acid aqueous solution for later use;
(2) adding a surfactant into the sodium silicate aqueous solution, uniformly stirring, adding the sodium silicate aqueous solution and the sulfuric acid aqueous solution into a mixer simultaneously by using a high-pressure pump, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the pH value of an outlet of the nozzle to generate wet balls;
(3) collecting the wet balls in water, curing, and washing by using tap water;
(4) adding the material generated in the step (3) into a displacement kettle, adding n-butyl alcohol, heating until the n-butyl alcohol and water form an azeotrope when the n-butyl alcohol and the water are boiled, carrying out organic solvent displacement on the azeotrope through oil-water separation, and then discharging;
(5) and (5) carrying out vacuum drying on the material generated in the step (4) by adopting a vacuum drying oven, thereby preparing the spherical silicon dioxide aerogel.
In some embodiments, in said step (1), the sodium silicate is added with water to prepare an aqueous sodium silicate solution of 15-20% wt on silica basis, and the sulfuric acid is added with water to prepare an aqueous sulfuric acid solution of 20-30% wt, both of which are settled for 48 hours for use.
In some embodiments, in the step (2), the surfactant is added in an amount of 0.5 to 1% of the silica, and then at 25 to 30 ℃ using a high pressure pump at 2 to 3kg/cm2Adding the sodium silicate aqueous solution and the sulfuric acid aqueous solution into a mixer at the same time under pressure, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controllingAnd (4) preparing a spray nozzle outlet PH8-9 to generate wet balls.
In some embodiments, in the step (3), the wet ball is collected in water with pH9-10, heated to 80-90 ℃, aged for 40-60 minutes, washed with tap water until the water resistivity is below 1000 Ω/cm.
In some embodiments, in the step (4), the material produced in the step (3) is added into a displacement kettle, after the n-butanol is added, the material is heated at a heating rate of 5-10 ℃/min, the n-butanol and water form an azeotrope when the material is heated to boiling, the azeotrope is subjected to organic solvent displacement through oil-water separation, and when the water content in the silica gel is less than 10 wt%, the heating is stopped and the material is discharged.
In some embodiments, in the step (5), the material produced in the step (4) is vacuum-dried by using a vacuum drying oven, heated to 180-.
In some embodiments, in step (2), the size of the silica particle size is controlled using the pore size of the nozzle.
In some embodiments, the surfactant is selected from one or both of JFC, peregal o pi-10.
The atmospheric pressure preparation method of silica aerogel spherical particles according to the embodiments of the present invention has been described above with reference to the accompanying drawings, and it should be noted that the above description is only an example and not a limitation of the present invention. In other embodiments of the invention, the method may include more, fewer, or different process steps, and the ingredients, proportions, and process conditions and parameters in the various process steps may differ from those described and illustrated.
Several specific embodiments of the invention are described below:
example one
1. Preparing 1000g of sodium silicate aqueous solution with 15 percent of silicon dioxide content by weight, and preparing 30 percent of aqueous solution by sulfuric acid; settling the two for 48 hours for later use;
2. adding 7.5g of surfactant into the sodium silicate aqueous solution-JFC was stirred well and then at 25 ℃ 2kg/cm2Adding sodium silicate and sulfuric acid into a high-efficiency mixer at the same time under pressure, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the PH8 at the outlet of the nozzle, wherein the aperture of the nozzle is 0.5 mm;
3. collecting the water with PH9 from the wet bulb in the step 2, heating to 80 ℃, curing for 60 minutes, then washing with tap water until the water resistivity is 1000 omega/cm;
4. adding the material obtained in the step (3) into a displacement kettle, adding n-butyl alcohol, heating at a heating rate of 5 ℃/min, forming an azeotrope with water when the material is heated to be boiling, carrying out organic solvent displacement on the azeotrope through oil-water separation, and stopping heating and discharging when the water content in silica gel is 9%;
5. vacuum drying the materials by a vacuum drying oven, heating to 200 ℃ at a heating rate of 10 ℃/min, and drying for 2 hours; spherical silica aerogel of 1.5mm was obtained.
Example two
1. Preparing 1000g of sodium silicate aqueous solution with the silicon dioxide content of 18 wt%, and preparing 25 wt% of aqueous solution with sulfuric acid; settling the two for 48 hours for later use;
2. adding 10.8g of surfactant-JFC into the sodium silicate aqueous solution, uniformly stirring, and then stirring at 25 ℃ and 2.2kg/cm2Adding sodium silicate and sulfuric acid into a high-efficiency mixer at the same time under pressure, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the pH of an outlet of the nozzle to be 8.5 and the aperture of the nozzle to be 0.8 mm;
3. collecting the water with PH9 from the wet bulb in the step 2, heating to 82 ℃, curing for 50 minutes, then washing with tap water until the water resistivity is 950 omega/cm;
4. adding the material obtained in the step (3) into a displacement kettle, adding n-butyl alcohol, heating at the heating rate of 6 ℃/min, forming an azeotrope with water when the material is heated to be boiling, carrying out organic solvent displacement on the azeotrope through oil-water separation, and stopping heating and discharging when the water content in silica gel is 5%;
5. vacuum drying the materials by a vacuum drying oven, heating to 190 ℃ at a heating rate of 15 ℃/min, and drying for 2 hours; spherical silica aerogel of 2.2mm was obtained.
EXAMPLE III
1. Preparing 1000g of sodium silicate aqueous solution with 20 wt% of silicon dioxide content, and preparing 20 wt% of sulfuric acid aqueous solution by using sulfuric acid; settling the two for 48 hours for later use;
2. adding 10.8g of surfactant o pi-10 into sodium silicate aqueous solution, stirring uniformly, and then at 30 ℃ and 2.8kg/cm2Adding sodium silicate and sulfuric acid into a high-efficiency mixer at the same time under pressure, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the pH of an outlet of the nozzle to be 8.5 and the aperture of the nozzle to be 1.0 mm;
3. collecting the water with the pH value of 9.5 by the wet bulb in the step 2, heating to 90 ℃, curing for 40 minutes, then washing by using tap water until the water resistivity is 850 omega/cm;
4. adding the material obtained in the step (3) into a displacement kettle, adding n-butyl alcohol, heating at a heating rate of 10 ℃/min, forming an azeotrope with water when the material is heated to be boiling, carrying out organic solvent displacement on the azeotrope through oil-water separation, and stopping heating and discharging when the water content in silica gel is 5%;
5. vacuum drying the materials by a vacuum drying oven, heating to 200 ℃ at a heating rate of 20 ℃/min, and drying for 2 hours; spherical silica aerogel of 3.0mm was obtained.
Example four
1. Preparing 1000g of sodium silicate aqueous solution with 20 wt% of silicon dioxide content, and preparing 25 wt% of sulfuric acid aqueous solution; settling the two for 48 hours for later use;
2. adding 6g of surfactant JFC and 6g of surfactant o pi-10 into sodium silicate aqueous solution, uniformly stirring, and then stirring at 30 ℃ and 2.5kg/cm2Adding sodium silicate and sulfuric acid into a high-efficiency mixer at the same time under pressure, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the pH of an outlet of the nozzle to be 8.5 and the aperture of the nozzle to be 1.2 mm;
3. collecting the water with the pH value of 9.0 by the wet bulb in the step 2, heating to 90 ℃, curing for 50 minutes, then washing by using tap water until the water resistivity is 900 omega/cm;
4. adding the material obtained in the step (3) into a displacement kettle, adding n-butyl alcohol, heating at a heating rate of 10 ℃/min, forming an azeotrope with water when the material is heated to be boiling, carrying out organic solvent displacement on the azeotrope through oil-water separation, and stopping heating and discharging when the water content in silica gel is 8%;
5. vacuum drying the materials by a vacuum drying oven, heating to 200 ℃ at a heating rate of 20 ℃/min, and drying for 2 hours; spherical silica aerogel of 3.8mm was obtained.
Determination of physicochemical Properties of silica aerogel
| Pore volume ml/g | Specific surface area m2/g | |
| Example one | 2.0 | 500 |
| Example two | 2.2 | 450 |
| EXAMPLE III | 2.1 | 475 |
| Example four | 2.4 | 400 |
According to the method for preparing the silica aerogel spherical particles under normal pressure, disclosed by the embodiment of the invention, industrial sodium silicate is used as a raw material, the process is simple, the cost is low, the industrialization is facilitated, and the particle size of the formed aerogel particles can reach 1-5 mm.
Although the present invention has been disclosed above by way of examples, the present invention is not limited thereto. Various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this disclosure, and the scope of the invention should be determined only by the language of the claims and the equivalents thereof.
Claims (8)
1. A normal pressure preparation method of silica aerogel spherical particles comprises the following steps:
(1) adding water into sodium silicate to prepare a sodium silicate aqueous solution, adding water into sulfuric acid to prepare a sulfuric acid aqueous solution, and settling the sulfuric acid aqueous solution and the sulfuric acid aqueous solution for later use;
(2) adding a surfactant into the sodium silicate aqueous solution, uniformly stirring, adding the sodium silicate aqueous solution and the sulfuric acid aqueous solution into a mixer simultaneously by using a high-pressure pump, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the pH value of an outlet of the nozzle to generate wet balls;
(3) collecting the wet balls in water, curing, and washing by using tap water;
(4) adding the material generated in the step (3) into a displacement kettle, adding n-butyl alcohol, heating until the n-butyl alcohol and water form an azeotrope when the n-butyl alcohol and the water are boiled, carrying out organic solvent displacement on the azeotrope through oil-water separation, and then discharging;
(5) and (5) carrying out vacuum drying on the material generated in the step (4) by adopting a vacuum drying oven, thereby preparing the spherical silicon dioxide aerogel.
2. The method as claimed in claim 1, wherein, in the step (1), the sodium silicate is added with water to prepare an aqueous sodium silicate solution of 15-20% wt in terms of silica, and the sulfuric acid is added with water to prepare an aqueous sulfuric acid solution of 20-30% wt, and the two are settled for 48 hours for use.
3. The method as claimed in claim 1, wherein, in the step (2), the surfactant is added in an amount of 0.5-1% of silica, and then at 25-30 ℃ using a high pressure pump at 2-3kg/cm2Adding the sodium silicate aqueous solution and the sulfuric acid aqueous solution into a mixer at the same time under the pressure, uniformly mixing, spraying the mixture into air through a nozzle for granulation, and controlling the PH8-9 of an outlet of the nozzle to generate a wet ball.
4. The method according to claim 1, wherein, in the step (3), the wet bulb is collected in water with pH9-10, heated to 80-90 ℃, aged for 40-60 minutes, and then washed with tap water until the water resistivity is below 1000 Ω/cm.
5. The method according to claim 1, wherein in the step (4), the material produced in the step (3) is added into a displacement kettle, after the n-butanol is added, the material is heated at a heating rate of 5-10 ℃/min, when the material is heated to boiling, the n-butanol and water form an azeotrope, the azeotrope is subjected to oil-water separation for organic solvent displacement, and when the water content in the silica gel is less than 10% by weight, the heating is stopped and the material is discharged.
6. The method as claimed in claim 1, wherein, in the step (5), the material produced in the step (4) is vacuum-dried by using a vacuum drying oven, heated to 180 ℃ at a heating rate of 10-20 ℃/min and dried for 2 hours, thereby obtaining the spherical silica aerogel.
7. The method according to claim 1, wherein in the step (2), the size of the silica particle size is controlled by using the pore size of the nozzle.
8. The method of claim 1, wherein the surfactant is selected from one or two of JFC, pinggai-o pi-10.
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| CN114149010A (en) * | 2021-12-15 | 2022-03-08 | 河北三棵树涂料有限公司 | Silicon dioxide aerogel ball and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114149010A (en) * | 2021-12-15 | 2022-03-08 | 河北三棵树涂料有限公司 | Silicon dioxide aerogel ball and preparation method thereof |
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