CN105036143B - Preparation method of nano silicon dioxide aerogel - Google Patents
Preparation method of nano silicon dioxide aerogel Download PDFInfo
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- CN105036143B CN105036143B CN201510475623.9A CN201510475623A CN105036143B CN 105036143 B CN105036143 B CN 105036143B CN 201510475623 A CN201510475623 A CN 201510475623A CN 105036143 B CN105036143 B CN 105036143B
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- infrared reflection
- reflection capability
- silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims description 5
- 239000004964 aerogel Substances 0.000 title abstract description 7
- 239000005543 nano-size silicon particle Substances 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000011858 nanopowder Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 5
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 5
- 239000012467 final product Substances 0.000 claims abstract description 3
- 230000002431 foraging effect Effects 0.000 claims abstract description 3
- 239000012686 silicon precursor Substances 0.000 claims abstract description 3
- 238000002791 soaking Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000004965 Silica aerogel Substances 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- 150000007522 mineralic acids Chemical class 0.000 claims description 4
- 150000007524 organic acids Chemical group 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 claims description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims description 2
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 2
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical group C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 238000001879 gelation Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 229910009871 Ti5Si3 Inorganic materials 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000352 supercritical drying Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Silicon Compounds (AREA)
Abstract
A process for preparing the aerogel of nano silicon dioxideCharacterized by comprising the following steps: a. according to the organic silicon precursor: h2O: low-carbon alcohol solvent: catalyst = 1: 1-10: 10-100: (0.1-100)*10‑3(mol) mixing, standing for 0.1-4 days for aging to prepare silicon dioxide acid sol; b. dispersing the nano powder with infrared reflection capability in a solvent, stirring and/or ultrasonically dispersing uniformly to prepare a nano solution with infrared reflection capability for later use, wherein the content of the nano powder is controlled to be 0.1-10%; c. adjusting the pH value of silica acid sol, mixing the silica acid sol with a nano solution with infrared reflection capability or adjusting the pH value of the silica acid sol after mixing the silica acid sol with the nano solution with infrared reflection capability, wherein the pH value is controlled to be 8-12, and the weight ratio of the nano powder with infrared reflection capability is as follows: formation of SiO2= 0.1-10: 100 (wt); d. soaking in carrier, standing for 0-48 hr after gelling, and performing supercritical extraction to obtain the final product.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic material manufacturing, and particularly relates to the field of silicon dioxide heat-insulating materials.
Background
With the increasing prominence of the current energy problem, energy conservation and emission reduction have become the hot spots of the current research. The silica aerogel material is widely used in the heat insulation field due to the excellent heat insulation capability, the thickness of the heat insulation layer can be greatly reduced by using the nano silica aerogel material, and the silica aerogel material basically and completely consists of silica and glass fiber, so that the silica aerogel material does not have any harmful pollution to the environment. Is an ideal substitute of heat-insulating materials.
However, the existing silica aerogel material has a weak infrared radiation blocking capability, and after the use temperature rises, the thermal conductivity of the silica aerogel material is obviously improved due to the increase of the proportion of infrared radiation heat dissipation, for example, after the use temperature reaches 300 ℃, the thermal conductivity of the silica aerogel material is improved by more than 50% compared with the normal temperature, and the expansion of the use range of the nano silica aerogel is limited. In the existing literature and reports, no relevant data aiming at the problem are found
The invention content is as follows:
aiming at the defects of the prior invention, the invention provides a preparation method of nano silicon dioxide aerogel with higher heat insulation effect at high temperature.
In order to realize the purpose of the invention, the following technical scheme is provided: a preparation method of nano silica aerogel comprises the following steps: a. according to the organic silicon precursor: h2O: low-carbon alcohol solvent: catalyst = 1: 1-10: 10-100: (0.1-100)*10-3(mol) mixing, standing for 0.1-4 days for aging to prepare silicon dioxide acid sol;
b. dispersing the nano powder with infrared reflection capability in a solvent, stirring and/or ultrasonically dispersing uniformly to prepare a nano solution with infrared reflection capability for later use, wherein the content of the nano powder is controlled to be 0.1-10%;
c. adjusting the pH value of silica acid sol, mixing the silica acid sol with a nano solution with infrared reflection capability or adjusting the pH value of the silica acid sol after mixing the silica acid sol with the nano solution with infrared reflection capability, wherein the pH value is controlled to be 8-12, and the weight ratio of the nano powder with infrared reflection capability is as follows: formation of SiO2=0.1-10：100（wt）；
d. Soaking in carrier, standing for 0-48 hr after gelling, and performing supercritical extraction to obtain the final product.
Preferably, the organosilicon precursor is one or a combination of tetraethyl orthosilicate, tetrachlorosilane and tetramethyl orthosilicate.
Preferably, the low-carbon alcohol solvent is one or a combination of ethanol and propanol.
Preferably, the catalyst is an organic or inorganic acid.
Preferably, the organic or inorganic acid is one or a combination of nitric acid, sulfuric acid and acetic acid.
Preferably, the nanopowder with infrared reflection capability is nano Indium Tin Oxide (ITO) or Ti5Si3、TiO2One or a combination thereof.
Preferably, the hydrophobic modification is carried out by adding the modifier after the gelation until the supercritical extraction.
Preferably, the modifier is trimethylsilanol, hexamethyldisilazane or trimethylchlorosilane.
The invention has the beneficial effects that: by reaction on SiO2Adding nanometer ITO and Ti into aerogel5Si3、TiO2The nanometer powder with infrared reflection capability maintains the good normal temperature heat insulation performance of the silicon dioxide aerogel powder, and simultaneously, the nanometer ITO and the Ti are used5Si3The reflection of the powder to infrared rays can obviously improve the heat insulation performance of the silicon dioxide aerogel at higher temperature.
Detailed Description
Example 1:
tetraethyl orthosilicate (TEOS), water, absolute ethyl alcohol and sulfuric acid are used as raw materials, and the weight ratio of TEOS: h2O: ethanol: sulfuric acid = 1: 1.5: 15: 0.01 (mol) of acid sol is prepared and is kept for 12h for later use (system A).
And ultrasonically dispersing the nano ITO powder into absolute ethyl alcohol, and controlling the concentration to be 1% for later use (a system B).
Adjusting the pH value of the system A to 9 by using an ammonia solution, and then mixing the system A with the system B, wherein the ratio of nano ITO: SiO22Controlling the conditions as 1: 100 (wt). Standing for 1 day after gelation for supercritical drying.
After the completion of the test, the thermal conductivity coefficient is measured from 300 ℃ to 0.029W/m/K
Example 2:
tetraethyl orthosilicate (TEOS), water, absolute ethyl alcohol and sulfuric acid are used as raw materials, and the weight ratio of TEOS: h2O: ethanol: sulfuric acid = 1: 1.5: 15: 0.01 (mol) of acid sol is prepared and is kept for 12h for later use (system A).
Mixing nanometer Ti5Si3The powder was ultrasonically dispersed in absolute ethanol with a concentration controlled at 1% for use (system B).
Adjusting the pH value of the system A to 9 by using an ammonia water solution, mixing the system A with the system B, and obtaining nano Ti5Si3：SiO2Controlling the conditions as 1: 100 (wt). Standing for 1 day after gelation for supercritical drying.
After the completion of the test, the thermal conductivity coefficient is measured from 300 ℃ to the thermal coefficient of 0.030W/m/K
Comparative example:
tetraethyl orthosilicate (TEOS), water, absolute ethyl alcohol and sulfuric acid are used as raw materials, and the weight ratio of TEOS: h2O: ethanol: sulfuric acid = 1: 1.5: 15: 0.01 (mol) of acid sol is prepared and is kept for 12h for later use (system A).
Adjusting the pH value of the system A to 9 by using an ammonia water solution, and standing for 1 day for supercritical drying after gelation.
After the completion of the test, the thermal conductivity coefficient is measured from 300 ℃ to 0.035W/m/K
Examples 3 to 8, with reference to example 1, parameters were set as shown in the following table:
Claims (7)
1. a preparation method of nano silica aerogel is characterized by comprising the following steps:
a. according to the organic silicon precursor: H2O: low-carbon alcohol solvent: catalyst = 1: 1-10: 10-100: (0.1-100)*10-3(mol) mixing, standing for 0.1-4 days for aging to prepare silicon dioxide acid sol;
b. dispersing the nano powder with infrared reflection capability in a solvent, stirring and/or ultrasonically dispersing uniformly to prepare a nano solution with infrared reflection capability for later use, wherein the content of the nano powder is controlled to be 0.1-10%;
c. adjusting the pH value of silica acid sol, mixing the silica acid sol with a nano solution with infrared reflection capability or adjusting the pH value of the silica acid sol after mixing the silica acid sol with the nano solution with infrared reflection capability, wherein the pH value is controlled to be 8-12, and the weight ratio of the nano powder with infrared reflection capability is as follows: SiO2= 0.1-10: 100 (wt);
d. soaking in carrier, standing for 0-48 hr after gelling, and performing supercritical extraction to obtain the final product;
the nano powder with infrared reflection capability is one or a combination of nano Indium Tin Oxide (ITO) and Ti5Si 3.
2. The method for preparing nano silica aerogel according to claim 1, wherein the organosilicon precursor is one or a combination of tetraethyl orthosilicate and tetrachlorosilane.
3. The method for preparing nano silica aerogel according to claim 1, wherein the low carbon alcohol solvent is one or a combination of ethanol and propanol.
4. The method for preparing nano silica aerogel according to claim 1, wherein the catalyst is organic or inorganic acid.
5. The method for preparing nano silica aerogel according to claim 4, wherein the organic or inorganic acid is one or a combination of nitric acid, sulfuric acid and acetic acid.
6. The method for preparing nano silica aerogel according to claim 1, wherein the modifying agent is added for hydrophobic modification within the time from the time of gel waiting to the time of supercritical extraction.
7. The method for preparing nano-silica aerogel according to claim 6, wherein the modifier is trimethylsilanol, hexamethyldisilazane or trimethylchlorosilane.
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| CN201510475623.9A CN105036143B (en) | 2015-08-06 | 2015-08-06 | Preparation method of nano silicon dioxide aerogel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106478055B (en) * | 2016-11-07 | 2018-08-31 | 江苏德威节能有限公司 | A kind of preparation method of the aerosil felt of hot pressing setting |
| CN108147415A (en) * | 2018-01-04 | 2018-06-12 | 中国科学技术大学 | A kind of preparation method of silica aerogel material |
| CN110436470B (en) * | 2019-09-06 | 2020-08-28 | 均一佳(武汉)科技有限公司 | Gel treating agent and preparation method and application thereof |
| CN110981409A (en) * | 2020-01-20 | 2020-04-10 | 成都新柯力化工科技有限公司 | Low-heat-radiation silicon dioxide aerogel and preparation method thereof |
| CN115108561A (en) * | 2022-07-25 | 2022-09-27 | 山东大学 | Transparent heat-insulation aerogel structure for concentrating photo-thermal power station and preparation method |
| CN115849862B (en) * | 2022-08-19 | 2024-01-30 | 希纳高科(江苏)有限公司 | Preparation method of nanowire fiber reinforced silicon aerogel composite material |
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| CN104497688A (en) * | 2014-12-05 | 2015-04-08 | 航天特种材料及工艺技术研究所 | Aerogel thermal insulation coating and preparation method thereof |
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2015
- 2015-08-06 CN CN201510475623.9A patent/CN105036143B/en active Active
Patent Citations (8)
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| JPH02304299A (en) * | 1989-05-05 | 1990-12-18 | Basf Ag | Heat insulating material mainly consisting of silica aerogel containing pigment |
| US5122291A (en) * | 1989-05-05 | 1992-06-16 | Basf Aktiengesellschaft | Thermal insulating material based on pigment containing silica aerogels |
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