CN110981409A - Low-heat-radiation silicon dioxide aerogel and preparation method thereof - Google Patents
Low-heat-radiation silicon dioxide aerogel and preparation method thereof Download PDFInfo
- Publication number
- CN110981409A CN110981409A CN202010064014.5A CN202010064014A CN110981409A CN 110981409 A CN110981409 A CN 110981409A CN 202010064014 A CN202010064014 A CN 202010064014A CN 110981409 A CN110981409 A CN 110981409A
- Authority
- CN
- China
- Prior art keywords
- aerogel
- silicon dioxide
- heat radiation
- silica
- lead sulfide
- 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.)
- Withdrawn
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a low-heat radiation silicon dioxide aerogel and a preparation method thereof. According to the invention, nano lead sulfide and silica aerogel are compounded, the nano lead sulfide quantum dots have a high infrared heat radiation absorption effect, so that the silica aerogel with low heat radiation is obtained, nano lead sulfide particles grow up through annealing treatment to reduce the infrared heat radiation permeability of the silica aerogel, and the thickness of the aerogel material can be reduced by loading the nano lead sulfide into nano holes of the silica aerogel.
Description
Technical Field
The invention relates to the technical field of silicon dioxide modification, in particular to a low-heat-radiation silicon dioxide aerogel and a preparation method thereof.
Background
The silica aerogel is a nano porous material with low density, high porosity and low heat conductivity coefficient, and has open pores and a space continuous structure. As a light high-efficiency heat-insulating material, the silicon dioxide aerogel has wide application prospect in various fields such as aerospace, energy, building, traffic, industry and the like. The thermal radiation conduction of the aerogel is almost transparent in a 3-8 mu m area, the aerogel can effectively block infrared thermal radiation at normal temperature, but the thermal conductivity of the silica aerogel sharply rises along with the rise of temperature, the permeability of the infrared thermal radiation is enhanced, and the thermal insulation performance of the material is seriously reduced, so that the application of the aerogel under the high-temperature condition is limited.
To reduce high temperature infrared radiation, opacifiers, such as carbon black, titanium dioxide, and the like, are often added to aerogels, and the use of opacifiers can greatly reduce the infrared radiation at high temperatures. The size of the opacifier is generally equal to that of infrared radiation light waves, is about 3-5 mu m, is difficult to compound with aerogel, and is usually matched with aerogel in a mode of adding an interlayer for use, so that the high-temperature infrared radiation is reduced, and the thickness of the material is increased. Since carbon black is poor in temperature resistance and easily oxidized at about 500 ℃, it is usually necessary to use a mixture of several light-shading agents in order to obtain a better heat-radiation-proof material. For the thermal radiation resistant material which requires thin thermal insulation material and good effect, the opacifier interlayer is difficult to meet the requirement. Meanwhile, different sunscreen materials are needed to be used for obtaining a wider range of heat radiation resistant materials due to different temperature resistance of various opacifiers.
The Chinese patent application No. 201711397334.7 discloses a preparation method of titanium dioxide/silicon dioxide composite aerogel, which comprises the steps of adding a titanium source into deionized water, stirring in an ice-water bath, adding an alkaline solution to adjust the pH value of the solution to 7-11, generating a white precipitate after reaction, centrifuging to remove supernatant, washing until no chloride ions or sulfate ions exist, dispersing in 50-200ml of deionized water, adding hydrogen peroxide until the solution is yellow and transparent, and adding deionized water to dilute to the concentration of 5-20mg/ml to obtain a titanium peroxide complex aqueous solution; diluting a silicon source with deionized water to obtain a solution A with the concentration of 5-100 mg/ml; mixing the obtained titanium peroxide complex water solution with the obtained solution A under the condition of ice-water bath to obtain a mixed solution, and standing and aging; and (3) freezing the mixed solution after standing and aging, drying to remove water to obtain a blocky dried titanium dioxide/silicon dioxide composite aerogel precursor, and calcining to obtain the blocky dried titanium dioxide/silicon dioxide composite aerogel. The Chinese invention patent application number 201910148217.X discloses a silicon dioxide aerogel and a preparation method thereof, wherein a precursor is obtained by mixing a uniformly mixed A system and gel core particles in a sealed state, and the precursor is dried. The system A comprises silicon phosphate, sodium silicate and water; the gel core particles comprise one or two of white carbon black and silicon micropowder. After the precursor is dried, silicic acid is shrunk to form silicon dioxide, and simultaneously, the white carbon black and the silicon micropowder are used as gel core particles to adsorb the silicon dioxide obtained after shrinkage, so that the silicon dioxide aerogel with a pompon-shaped porous structure is formed. The silicon dioxide aerogel has the advantages of excellent performance, small heat conductivity coefficient and larger specific surface area, and the method also has the defect that the visible size of the material is difficult to reduce and has poor high-temperature resistance.
In order to reduce the infrared heat radiation of silica aerogel at high temperature and obtain aerogel materials with thin thickness and good heat insulation effect, it is necessary to provide a novel silica composite aerogel and a preparation method thereof, so as to expand the application of silica aerogel at high temperature.
Disclosure of Invention
Aiming at the problem that the thickness of the material is increased by adding composite opacifiers such as carbon black, titanium dioxide and the like to reduce the infrared heat radiation of the silicon dioxide aerogel at present, the invention provides the silicon dioxide aerogel with low heat radiation and the preparation method thereof.
In order to solve the problems, the invention adopts the following technical scheme:
the invention provides a low-heat radiation silicon dioxide aerogel which is prepared by firstly preparing silicon dioxide wet gel by a sol-gel method, then preparing lead sulfide colloid by the reaction of lead nitrate and sodium sulfide, then adding the silicon dioxide wet gel into the lead sulfide colloid for soaking and supercritical drying, and then annealing the obtained composite aerogel.
The invention also provides a preparation method of the low-heat-radiation silicon dioxide aerogel, which comprises the following steps:
(1) adding 60L of tetraethoxysilane into a reaction kettle filled with 200L of ethanol, stirring for 30min at the rotating speed of 200rpm, and then slowly adding a hydrochloric acid solution to adjust the pH value to about 3.5; continuously stirring for 30min, then heating to 45 ℃ and keeping the temperature for 24 h; adding ammonia water solution under stirring at 200rpm to adjust pH to about 7.5, stirring for 15min, and keeping constant temperature at 45 deg.C for 4 h; adding an aqueous solution of gamma-glycidyl ether propyl trimethoxy silane under stirring at 200rpm, heating to 60 ℃, and keeping the temperature for 2 hours to obtain silica wet gel;
(2) adding an aqueous solution of lead nitrate into an acetonitrile solution of polyethylene glycol, carrying out ice-water bath for 1-1.5h, taking out and recovering to room temperature, and then adding an acetonitrile solution of sodium sulfide to obtain lead sulfide colloid;
(3) adding the silica wet gel into lead sulfide colloid, soaking for 12-15h, and then performing supercritical drying to obtain nano lead sulfide composite silica aerogel;
(4) and (3) annealing the nano lead sulfide composite silicon dioxide aerogel to prepare the low-heat radiation silicon dioxide aerogel.
The preparation process flow is shown in figure 1.
Preferably, the molar concentration of the hydrochloric acid solution in the step (1) is 2.5 mol/L; the molar concentration of the ammonia water solution is 3 mol/L; the mass concentration of the aqueous solution of the gamma-glycidyl ether propyl trimethoxy silane is 30 percent.
Preferably, the gamma-glycidyl ether propyl trimethoxy silane stabilizer added in the step (1) accounts for 5-10% of the mass of the silicon dioxide.
Preferably, the mass concentration of the aqueous solution of lead nitrate in the step (2) is 3-5%; the mass concentration of the acetonitrile solution of the polyethylene glycol is 0.1%; the mass concentration of the acetonitrile solution of sodium sulfide is 10-15%.
Preferably, the mass ratio of the aqueous solution of lead nitrate, the acetonitrile solution of polyethylene glycol and the acetonitrile solution of sodium sulfide in the step (2) is 20-30:100: 4-8.
Preferably, the mass ratio of the silica wet gel to the lead sulfide colloid in the step (3) is 10-20: 100.
Preferably, the pre-pressurizing of the supercritical drying in the step (3) is 8-10MPa, the supercritical pressure is 12-15MPa, and the supercritical temperature is 250-300 ℃.
Preferably, the temperature of the annealing treatment in the step (4) is 500-600 ℃, and the time is 4-6 h.
It is known that, for nano materials, the particle diameter is small and is between 10 nm and 100nm, the infrared absorption band is wide, and the absorption of infrared light is obvious. Lead sulfide is an important semiconductor material, has a forbidden band width of 0.41eV at normal temperature, and can be observed at 18nm due to a quantization effect. The nano lead sulfide has stronger absorption to infrared band light, so the nano lead sulfide can be used as an additive material for preventing infrared radiation of silicon dioxide aerogel.
Furthermore, the nanocrystalline lead sulfide has an obvious quantum confinement effect, and the size of the nanocrystalline can be adjusted by controlling the preparation conditions of the lead sulfide nanocrystalline, so that the photoelectric property of the lead sulfide nanocrystalline can be regulated and controlled. The annealing treatment refers to a method of heating the material to a certain temperature in a certain atmosphere, keeping for a period of time, and then cooling at a proper rate, wherein the annealing treatment is carried out after the crystal grows, so that the defects in the crystal can be reduced, the stress is eliminated, and the crystallization quality is improved.
Furthermore, the size of the conventional opacifier is usually selected to be equivalent to that of infrared radiation light waves, and is difficult to be compounded with the aerogel, and the conventional opacifier is usually used together with the aerogel in a mode of adding a barrier layer, so that the thickness of the material per se is increased, and particularly when several opacifiers are mixed for use, the composite material with proper thickness and good heat insulation effect is more difficult to obtain. According to the preparation method, the silica wet gel is added into the lead sulfide colloid for soaking for a long time, and then supercritical drying is carried out, so that the nano lead sulfide is loaded into nano holes of the silica aerogel, and the obtained infrared and thermal radiation resistant composite aerogel material can be thinner.
The existing composite sunscreen agent can reduce the infrared radiation of the silica aerogel, but the thickness of the material is increased, so that the application of the silica aerogel is limited. In view of the above, the invention provides a low-heat radiation silica aerogel, which is prepared by a sol-gel method by using tetraethoxysilane as a raw material, ethanol as a solvent and gamma-glycidyl ether propyl trimethoxy silane as a surfactant to obtain a silica wet gel; then, preparing lead sulfide colloid by using an aqueous solution of lead nitrate and an acetonitrile solution of sodium sulfide as raw materials through an ice-water bath; then adding the silicon dioxide wet gel into lead sulfide colloid, soaking for 12-15h, and performing supercritical drying under the conditions of pressure of 12-15MPa and temperature of 250-300 ℃ to prepare the nano lead sulfide composite silicon dioxide aerogel; and finally, annealing the aerogel at the temperature of 500-600 ℃ for 4-6h to obtain the low-heat-radiation silicon dioxide aerogel. According to the invention, the silicon dioxide aerogel is compounded by adopting the nano lead sulfide and is subjected to annealing treatment, so that the heat radiation and the permeability of the silicon dioxide aerogel are reduced, the thickness of the material is reduced by loading the nano lead sulfide into nano holes of the silicon dioxide aerogel, and the obtained silicon dioxide aerogel material with thin thickness and good heat insulation effect has wider application space.
Compared with the prior art, the invention provides the low-heat-radiation silicon dioxide aerogel and the preparation method thereof, and the outstanding characteristics and excellent effects are as follows:
1. according to the silicon dioxide aerogel prepared by the invention, nano lead sulfide and the silicon dioxide aerogel are compounded, and the nano lead sulfide quantum dots have a high absorption effect on infrared heat radiation, so that the heat radiation of the silicon dioxide aerogel is reduced.
2. According to the preparation method, the nano lead sulfide particles grow up by annealing treatment, so that the absorption effect on infrared heat radiation is further improved, and the permeability of the silica aerogel on infrared heat radiation is reduced.
3. The silica aerogel material prepared by the invention can reduce the thickness of the aerogel material because the nano lead sulfide is loaded in the nano holes of the silica aerogel.
Drawings
FIG. 1: the invention relates to a preparation process flow chart of low-heat radiation silicon dioxide aerogel;
FIG. 2: test temperature of the low-emissivity silica aerogel of example 1;
FIG. 3: test temperature of silica aerogel of comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Adding 60L of tetraethoxysilane into a reaction kettle filled with 200L of ethanol, stirring for 30min at the rotating speed of 200rpm, and then slowly adding hydrochloric acid solution with the molar concentration of 2.5mol/L to adjust the pH value to about 3.5; continuously stirring for 30min, then heating to 45 ℃ and keeping the temperature for 24 h; adding ammonia water solution with the molar concentration of 3mol/L under stirring at 200rpm, adjusting the pH to about 7.5, continuously stirring for 15min, and keeping the temperature at 45 ℃ for 4 h; adding an aqueous solution of gamma-glycidyl ether propyl trimethoxy silane with the mass concentration of 30% while stirring at 200rpm, wherein the addition amount of a gamma-glycidyl ether propyl trimethoxy silane stabilizer is 10% of the mass of silicon dioxide, then heating to 60 ℃ and keeping the temperature for 2 hours to obtain silicon dioxide wet gel;
(2) adding an aqueous solution of lead nitrate with the mass concentration of 3% into an acetonitrile solution of polyethylene glycol with the mass concentration of 0.1%, carrying out ice-water bath for 1.5h, taking out and recovering to room temperature, then adding an acetonitrile solution of sodium sulfide with the mass concentration of 15% to obtain lead sulfide colloid, wherein the adding mass ratio of the aqueous solution of lead nitrate, the acetonitrile solution of polyethylene glycol and the acetonitrile solution of sodium sulfide is 30:100: 8;
(3) adding the silicon dioxide wet gel into lead sulfide colloid, wherein the adding mass ratio of the silicon dioxide wet gel to the lead sulfide colloid is 20:100, soaking for 12h, and then performing supercritical drying, wherein the pre-pressurization is 10MPa, the supercritical pressure is 15MPa, and the supercritical temperature is 250 ℃ to obtain the nano lead sulfide composite silicon dioxide aerogel;
(4) and (3) annealing the nano lead sulfide composite silicon dioxide aerogel at 600 ℃ for 6 hours to prepare the low-heat radiation silicon dioxide aerogel.
Example 2
(1) Adding 60L of tetraethoxysilane into a reaction kettle filled with 200L of ethanol, stirring for 30min at the rotating speed of 200rpm, and then slowly adding hydrochloric acid solution with the molar concentration of 2.5mol/L to adjust the pH value to about 3.5; continuously stirring for 30min, then heating to 45 ℃ and keeping the temperature for 24 h; adding ammonia water solution with the molar concentration of 3mol/L under stirring at 200rpm, adjusting the pH to about 7.5, continuously stirring for 15min, and keeping the temperature at 45 ℃ for 4 h; adding an aqueous solution of gamma-glycidyl ether propyl trimethoxy silane with the mass concentration of 30% while stirring at 200rpm, wherein the addition amount of a gamma-glycidyl ether propyl trimethoxy silane stabilizer is 5% of the mass of silicon dioxide, then heating to 60 ℃ and keeping the temperature for 2 hours to obtain silicon dioxide wet gel;
(2) adding an aqueous solution of lead nitrate with the mass concentration of 5% into an acetonitrile solution of polyethylene glycol with the mass concentration of 0.1%, carrying out ice-water bath for 1h, taking out and recovering to room temperature, then adding an acetonitrile solution of sodium sulfide with the mass concentration of 10% to obtain lead sulfide colloid, wherein the adding mass ratio of the aqueous solution of lead nitrate, the acetonitrile solution of polyethylene glycol and the acetonitrile solution of sodium sulfide is 20:100: 4;
(3) adding the silicon dioxide wet gel into lead sulfide colloid, wherein the adding mass ratio of the silicon dioxide wet gel to the lead sulfide colloid is 10-20:100, soaking for 15h, and then performing supercritical drying, wherein the pre-pressurization is 8MPa, the supercritical pressure is 12MPa, and the supercritical temperature is 300 ℃ to obtain the nano lead sulfide composite silicon dioxide aerogel;
(4) and (3) annealing the nano lead sulfide composite silicon dioxide aerogel at 500 ℃ for 4h to prepare the low-heat radiation silicon dioxide aerogel.
Example 3
(1) Adding 60L of tetraethoxysilane into a reaction kettle filled with 200L of ethanol, stirring for 30min at the rotating speed of 200rpm, and then slowly adding hydrochloric acid solution with the molar concentration of 2.5mol/L to adjust the pH value to about 3.5; continuously stirring for 30min, then heating to 45 ℃ and keeping the temperature for 24 h; adding ammonia water solution with the molar concentration of 3mol/L under stirring at 200rpm, adjusting the pH to about 7.5, continuously stirring for 15min, and keeping the temperature at 45 ℃ for 4 h; adding an aqueous solution of gamma-glycidyl ether propyl trimethoxy silane with the mass concentration of 30% while stirring at 200rpm, wherein the addition amount of a gamma-glycidyl ether propyl trimethoxy silane stabilizer is 8% of the mass of silicon dioxide, then heating to 60 ℃ and keeping the temperature for 2 hours to obtain silicon dioxide wet gel;
(2) adding an aqueous solution of lead nitrate with the mass concentration of 4% into an acetonitrile solution of polyethylene glycol with the mass concentration of 0.1%, carrying out ice-water bath for 1.5h, taking out and recovering to room temperature, then adding an acetonitrile solution of sodium sulfide with the mass concentration of 12% to obtain lead sulfide colloid, wherein the adding mass ratio of the aqueous solution of lead nitrate, the acetonitrile solution of polyethylene glycol and the acetonitrile solution of sodium sulfide is 25:100: 6;
(3) adding the silicon dioxide wet gel into lead sulfide colloid, wherein the adding mass ratio of the silicon dioxide wet gel to the lead sulfide colloid is 15:100, soaking for 13h, and then performing supercritical drying, wherein the pre-pressurization is 9MPa, the supercritical pressure is 14MPa, and the supercritical temperature is 280 ℃ to obtain the nano lead sulfide composite silicon dioxide aerogel;
(4) and (3) annealing the nano lead sulfide composite silicon dioxide aerogel at 550 ℃ for 5 hours to prepare the low-heat radiation silicon dioxide aerogel.
Example 4
(1) Adding 60L of tetraethoxysilane into a reaction kettle filled with 200L of ethanol, stirring for 30min at the rotating speed of 200rpm, and then slowly adding hydrochloric acid solution with the molar concentration of 2.5mol/L to adjust the pH value to about 3.5; continuously stirring for 30min, then heating to 45 ℃ and keeping the temperature for 24 h; adding ammonia water solution with the molar concentration of 3mol/L under stirring at 200rpm, adjusting the pH to about 7.5, continuously stirring for 15min, and keeping the temperature at 45 ℃ for 4 h; adding an aqueous solution of gamma-glycidyl ether propyl trimethoxy silane with the mass concentration of 30% while stirring at 200rpm, wherein the addition amount of a gamma-glycidyl ether propyl trimethoxy silane stabilizer is 6% of the mass of silicon dioxide, then heating to 60 ℃ and keeping the temperature for 2 hours to obtain silicon dioxide wet gel;
(2) adding an aqueous solution of lead nitrate with the mass concentration of 5% into an acetonitrile solution of polyethylene glycol with the mass concentration of 0.1%, carrying out ice-water bath for 1h, taking out and recovering to room temperature, then adding an acetonitrile solution of sodium sulfide with the mass concentration of 10% to obtain lead sulfide colloid, wherein the adding mass ratio of the aqueous solution of lead nitrate, the acetonitrile solution of polyethylene glycol and the acetonitrile solution of sodium sulfide is 22:100: 7;
(3) adding the silicon dioxide wet gel into lead sulfide colloid, wherein the adding mass ratio of the silicon dioxide wet gel to the lead sulfide colloid is 18:100, soaking for 15h, and then performing supercritical drying, wherein the pre-pressurization is 8MPa, the supercritical pressure is 12MPa, and the supercritical temperature is 280 ℃ to obtain the nano lead sulfide composite silicon dioxide aerogel;
(4) and (3) annealing the nano lead sulfide composite silicon dioxide aerogel at 520 ℃ for 6 hours to prepare the low-heat radiation silicon dioxide aerogel.
Example 5
(1) Adding 60L of tetraethoxysilane into a reaction kettle filled with 200L of ethanol, stirring for 30min at the rotating speed of 200rpm, and then slowly adding hydrochloric acid solution with the molar concentration of 2.5mol/L to adjust the pH value to about 3.5; continuously stirring for 30min, then heating to 45 ℃ and keeping the temperature for 24 h; adding ammonia water solution with the molar concentration of 3mol/L under stirring at 200rpm, adjusting the pH to about 7.5, continuously stirring for 15min, and keeping the temperature at 45 ℃ for 4 h; adding an aqueous solution of gamma-glycidyl ether propyl trimethoxy silane with the mass concentration of 30% while stirring at 200rpm, wherein the addition amount of a gamma-glycidyl ether propyl trimethoxy silane stabilizer is 9% of the mass of silicon dioxide, then heating to 60 ℃ and keeping the temperature for 2 hours to obtain silicon dioxide wet gel;
(2) adding an aqueous solution of lead nitrate with the mass concentration of 3% into an acetonitrile solution of polyethylene glycol with the mass concentration of 0.1%, carrying out ice-water bath for 1h, taking out and recovering to room temperature, then adding an acetonitrile solution of sodium sulfide with the mass concentration of 13% to obtain lead sulfide colloid, wherein the adding mass ratio of the aqueous solution of lead nitrate, the acetonitrile solution of polyethylene glycol and the acetonitrile solution of sodium sulfide is 28:100: 5;
(3) adding the silicon dioxide wet gel into lead sulfide colloid, wherein the adding mass ratio of the silicon dioxide wet gel to the lead sulfide colloid is 15:100, soaking for 12h, and then performing supercritical drying, wherein the pre-pressurization is 10MPa, the supercritical pressure is 12MPa, and the supercritical temperature is 250 ℃ to obtain the nano lead sulfide composite silicon dioxide aerogel;
(4) and (3) annealing the nano lead sulfide composite silicon dioxide aerogel at 500 ℃ for 6h to prepare the low-heat radiation silicon dioxide aerogel.
Comparative example 1
Comparative example 1 is silica aerogel containing no nano lead sulfide, and the process for preparing silica aerogel is the same as example 1.
The test method comprises the following steps:
the silica aerogel of example 1 and comparative example 1 was dispersed in ethanol in a mass ratio of 1:8 to form a slurry, and an asbestos mesh having a thickness of 3mm was used as a base material, and the slurry was immersed in the slurry to allow the asbestos mesh base material to adsorb the silica aerogel, and the dried product was used as a test sample. The sample is cut into plates with the length and the width of 6 multiplied by 4cm respectively, the plates are baked for 3min by an alcohol lamp, the height of a lamp wick of the alcohol lamp from the sample is 10cm, then the temperature of the other side of the sample is tested by using an infrared thermometer at a fixed point and a line, and the room temperature environment is 18 ℃. Example 1 testing is shown in figure 2 and comparative example 1 testing is shown in figure 3.
As can be seen from fig. 2 and 3, the test temperature of the low-emissivity silica aerogel of example 1 is 25.5 ℃, the test temperature of the silica aerogel of comparative example 1 is 39 ℃, and the temperature of the aerogel of example 1 is much lower than that of the aerogel of comparative example 1, which indicates that the nano lead sulfide quantum dots in the present invention have a high absorption effect on infrared heat radiation, and the low-emissivity silica aerogel can be obtained by compounding with silica, so that the temperature is lower.
Claims (9)
1. The low-heat-radiation silicon dioxide aerogel is characterized by being prepared by firstly preparing silicon dioxide wet gel by a sol-gel method, then preparing lead sulfide colloid by reacting lead nitrate with sodium sulfide, then adding the silicon dioxide wet gel into the lead sulfide colloid for soaking and supercritical drying, and then annealing the obtained composite aerogel.
2. A preparation method of low-heat-radiation silicon dioxide aerogel is characterized by comprising the following steps of:
(1) adding 60L of tetraethoxysilane into a reaction kettle filled with 200L of ethanol, stirring for 30min at the rotating speed of 200rpm, and then slowly adding a hydrochloric acid solution to adjust the pH value to about 3.5; continuously stirring for 30min, then heating to 45 ℃ and keeping the temperature for 24 h; adding ammonia water solution under stirring at 200rpm to adjust pH to about 7.5, stirring for 15min, and keeping constant temperature at 45 deg.C for 4 h; adding an aqueous solution of gamma-glycidyl ether propyl trimethoxy silane under stirring at 200rpm, heating to 60 ℃, and keeping the temperature for 2 hours to obtain silica wet gel;
(2) adding an aqueous solution of lead nitrate into an acetonitrile solution of polyethylene glycol, carrying out ice-water bath for 1-1.5h, taking out and recovering to room temperature, and then adding an acetonitrile solution of sodium sulfide to obtain lead sulfide colloid;
(3) adding the silica wet gel into lead sulfide colloid, soaking for 12-15h, and then performing supercritical drying to obtain nano lead sulfide composite silica aerogel;
(4) and (3) annealing the nano lead sulfide composite silicon dioxide aerogel to prepare the low-heat radiation silicon dioxide aerogel.
3. The method for preparing a silica aerogel with low heat radiation according to claim 2, wherein the hydrochloric acid solution in the step (1) has a molar concentration of 2.5 mol/L; the molar concentration of the ammonia water solution is 3 mol/L; the mass concentration of the aqueous solution of the gamma-glycidyl ether propyl trimethoxy silane is 30 percent.
4. The method for preparing a silica aerogel with low heat radiation according to claim 2, wherein the gamma-glycidoxypropyltrimethoxysilane stabilizer is added in the amount of 5 to 10% by mass of silica in step (1).
5. The method for preparing a silica aerogel with low heat radiation according to claim 2, wherein the mass concentration of the aqueous solution of lead nitrate in the step (2) is 3 to 5%; the mass concentration of the acetonitrile solution of the polyethylene glycol is 0.1%; the mass concentration of the acetonitrile solution of sodium sulfide is 10-15%.
6. The method for preparing silica aerogel with low heat radiation according to claim 2, wherein the aqueous solution of lead nitrate, the acetonitrile solution of polyethylene glycol and the acetonitrile solution of sodium sulfide are added in the step (2) in a mass ratio of 20-30:100: 4-8.
7. The method for preparing silica aerogel with low heat radiation according to claim 2, wherein the silica wet gel and the lead sulfide colloid are added in the step (3) in a mass ratio of 10-20: 100.
8. The method for preparing a silica aerogel with low heat radiation according to claim 2, wherein the pre-pressurization of the supercritical drying in the step (3) is 8 to 10MPa, the supercritical pressure is 12 to 15MPa, and the supercritical temperature is 250-300 ℃.
9. The method for preparing a silica aerogel having low heat radiation according to claim 2, wherein the temperature of the annealing treatment in the step (4) is 500-600 ℃ and the time is 4-6 h.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010064014.5A CN110981409A (en) | 2020-01-20 | 2020-01-20 | Low-heat-radiation silicon dioxide aerogel and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010064014.5A CN110981409A (en) | 2020-01-20 | 2020-01-20 | Low-heat-radiation silicon dioxide aerogel and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110981409A true CN110981409A (en) | 2020-04-10 |
Family
ID=70081324
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010064014.5A Withdrawn CN110981409A (en) | 2020-01-20 | 2020-01-20 | Low-heat-radiation silicon dioxide aerogel and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110981409A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114471387A (en) * | 2021-08-13 | 2022-05-13 | 松山湖材料实验室 | Aerogel containing quantum dots and preparation method thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1480569A (en) * | 2002-06-27 | 2004-03-10 | ͨ�õ�����˾ | Method of reducing crystal defect density |
CN1504826A (en) * | 2002-12-04 | 2004-06-16 | 中国科学院理化技术研究所 | Lead sulfide nano particle sensitizer and preparation method and application thereof |
WO2012177097A2 (en) * | 2011-06-24 | 2012-12-27 | Lg Innotek Co., Ltd. | Method of fabricating silicon carbide powder |
CN103877575A (en) * | 2014-04-02 | 2014-06-25 | 大连工业大学 | Light-weight mesoporous composite aerogel material and preparation method thereof |
CN105036143A (en) * | 2015-08-06 | 2015-11-11 | 江苏德威节能有限公司 | Preparation method for nanosilicon dioxide aerogel |
CN106732212A (en) * | 2016-12-09 | 2017-05-31 | 天长市天龙泵阀成套设备厂 | A kind of silica gold nano star composite aerogel and preparation method thereof |
-
2020
- 2020-01-20 CN CN202010064014.5A patent/CN110981409A/en not_active Withdrawn
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1480569A (en) * | 2002-06-27 | 2004-03-10 | ͨ�õ�����˾ | Method of reducing crystal defect density |
CN1504826A (en) * | 2002-12-04 | 2004-06-16 | 中国科学院理化技术研究所 | Lead sulfide nano particle sensitizer and preparation method and application thereof |
WO2012177097A2 (en) * | 2011-06-24 | 2012-12-27 | Lg Innotek Co., Ltd. | Method of fabricating silicon carbide powder |
CN103877575A (en) * | 2014-04-02 | 2014-06-25 | 大连工业大学 | Light-weight mesoporous composite aerogel material and preparation method thereof |
CN105036143A (en) * | 2015-08-06 | 2015-11-11 | 江苏德威节能有限公司 | Preparation method for nanosilicon dioxide aerogel |
CN106732212A (en) * | 2016-12-09 | 2017-05-31 | 天长市天龙泵阀成套设备厂 | A kind of silica gold nano star composite aerogel and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
杨立稳 等: "硫化铅红外吸收纳米材料的制备及其性能研究", 《全国第十四届红外加热暨红外医学发展研讨会论文及论文摘要集》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114471387A (en) * | 2021-08-13 | 2022-05-13 | 松山湖材料实验室 | Aerogel containing quantum dots and preparation method thereof |
CN114471387B (en) * | 2021-08-13 | 2022-12-23 | 松山湖材料实验室 | Aerogel containing quantum dots and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR101409884B1 (en) | Preparation method of hydrophobic monolith type silica aerogel | |
CN110563435B (en) | Rare earth-based aerogel material with radiation shielding effect and heat insulation performance as well as preparation and application thereof | |
CN103086692B (en) | Blocky SiO2-Y2O3Preparation method of composite aerogel | |
CN108383487B (en) | PAN pre-oxidized fiber felt/silicon dioxide aerogel composite material and preparation method thereof | |
CN108751969B (en) | High-temperature-resistant, heat-insulating and wave-transmitting ceramic matrix composite and preparation method thereof | |
CN108249901B (en) | Preparation method of high-temperature-resistant aerogel material | |
CN113716572A (en) | Preparation method of alumina-silica aerogel composite material | |
TW200835648A (en) | Porous material and method for preparing the same | |
CN105036143B (en) | Preparation method of nano silicon dioxide aerogel | |
CN106854086B (en) | High-temperature-resistant mullite aerogel composite material and preparation method thereof | |
CN115073981B (en) | Preparation method of water-based nano heat-preservation heat-insulation coating | |
CN110510617B (en) | Normal-pressure drying preparation method of large-size alumina-silica aerogel | |
CN109251005A (en) | A kind of preparation method enhancing silica aerogel material | |
CN104446305A (en) | Calcium sulphate whisker aerogel heat-insulating composite material and preparation method thereof | |
CN110282947A (en) | A kind of high-strength composite aeroge thermal insulation material and preparation method thereof | |
CN106186035A (en) | Preparation method of blocky La 2O 3-SiO 2 composite aerogel | |
CN106280551A (en) | The preparation method of a kind of compound coated red pigment cerium sulphide and prepared product thereof | |
KR20100120036A (en) | Porous ceramic prepared from sodium silicate and aerogel and a method for preparing thereof | |
CN106145999B (en) | Cubic La2O3-Al2O3Preparation method of composite aerogel | |
CN111072037B (en) | Preparation method of silica aerogel | |
CN114195543A (en) | Mullite whisker/anorthite/SiO2Aerogel porous ceramic, preparation method thereof and heat insulation tile | |
CN110981409A (en) | Low-heat-radiation silicon dioxide aerogel and preparation method thereof | |
CN103509462A (en) | Heat insulation coating, preparation method and application thereof | |
CN101249978A (en) | Method for preparing YAG nano powder | |
CN111099596A (en) | Simple method for coating high-hydrophobicity boron nitride nanosheet thin layer on surface of silicon dioxide aerogel particle |
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 | ||
WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200410 |
|
WW01 | Invention patent application withdrawn after publication |