CN105036143A - Preparation method for nanosilicon dioxide aerogel - Google Patents
Preparation method for nanosilicon dioxide aerogel Download PDFInfo
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- CN105036143A CN105036143A CN201510475623.9A CN201510475623A CN105036143A CN 105036143 A CN105036143 A CN 105036143A CN 201510475623 A CN201510475623 A CN 201510475623A CN 105036143 A CN105036143 A CN 105036143A
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- titanium dioxide
- silica aerogel
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
A preparation method for nanosilicon dioxide aerogel is characterized by including the following steps that a, organosilicone precursor, H2O, low-carbon alcohol and a catalyst are mixed according to the mole ratio of 1 to 1-10 to 10-100 to (0.1-100)*10<-3> (mol), the mixture is placed for 0.1-4 days for ageing, and silicon dioxide acid soil is prepared; b, nanopowder with infrared reflection capacity is dispersed in solvent, and a nanometer solution with the infrared reflection capacity is prepared for standby application after the mixture is stirred and/or ultrasonically dispersed to be uniform, wherein the content of the nanopowder is controlled between 0.1% and 10%; c, the pH value of the silicon dioxide acid sol is regulated, wherein the silicon dioxide sol is mixed with the nanometer solution with the infrared reflection capacity after the pH value is regulated or the pH value is regulated after the silicon dioxide sol is mixed with the nanometer solution with the infrared reflection capacity, the pH value is controlled between 8 and 12, and SiO2 with the weight ratio of 0.1-10 to 100 (wt) is generated through the nanopowder with the infrared reflection capacity; d, the mixture is saturated and submerged on a carrier, and a finished product is obtained by conducting supercritical extraction after the mixture is placed for 0-48 h after isogel.
Description
Technical field
The invention belongs to ceramic and make field, particularly relate to silica dioxide heat-insulating material field.
Background technology
Along with becoming increasingly conspicuous of current energy source problem, energy-saving and emission-reduction have become the focus of current research.Silica aerogel material is due to the heat-insulating capability of its excellence, about come about extensive in the use of field of thermal insulation, use nanometer titanium dioxide Silica Aerogels, not only greatly can reduce insulation layer thickness, and be substantially all made up of, for environment without any harmful pollution silicon-dioxide and glass fibre due to silica aerogel material.It is desirable lagging material substitute.
But, the silica aerogel material of present use is more weak for the obstructing capacity of ir radiation, after use temperature raises, due to the increase of ir radiation heat radiation proportion, its heat conductivility has obvious raising, after use temperature reaches 300 degree, its heat conductivility has the lifting more than more than 50% compared with normal temperature, limits the expansion of nanometer titanium dioxide silica aerogel use range.In existing document and report, yet there are no the related data for this problem
Summary of the invention:
The present invention is the deficiency for existing invention, provides a kind of nanometer titanium dioxide silica aerogel preparation method at high temperature still with higher effect of heat insulation.
For realizing the object of the invention, provide following technical scheme: a kind of nanometer titanium dioxide silica aerogel preparation method, comprises the following steps: a. is by organosilane precursor: H
2* 10 O: low-carbon alcohol solvent: catalyzer=1:1-10:10-100:(0.1-100)
-3(mol) mix, place and carry out ageing in 0.1-4 days, obtained silicon-dioxide acid-sol;
B. be scattered in solvent by the nanometer powder with infrared external reflection ability, it is for subsequent use that stirring and/or ultrasonic disperse evenly obtain the nano-solution with infrared external reflection ability afterwards, and nanometer powder content controls at 0.1%-10%;
C. by silicon-dioxide acid-sol adjust ph, adjust ph after mixing with the nano-solution with infrared external reflection ability or silicon-dioxide acid-sol being mixed with the nano-solution with infrared external reflection ability, pH value controls as 8-12, the nanometer powder of described infrared external reflection ability: generate SiO
2=0.1-10:100(wt);
D. be saturatedly dipped on carrier, after isogel, carry out supercritical extraction after placing 0-48h, obtain finished product.
As preferably, organosilane precursor is tetraethyl orthosilicate, tetrachloro silicane, the one of positive quanmethyl silicate or combination.
As preferably, low-carbon alcohol solvent is ethanol, the one of propyl alcohol or combination.
As preferably, catalyzer is organic or inorganic acid.
As preferably, organic or inorganic acid is a kind of or combination of nitric acid, sulfuric acid, acetic acid.
As preferably, the nanometer powder with infrared external reflection ability is nano indium tin oxide (ITO), Ti
5si
3, TiO
2one or combination.
As preferably, add properties-correcting agent in the time after isogel before supercritical extraction and carry out hydrophobically modified.
As preferably, properties-correcting agent is trimethyl silanol, hexamethyldisilazane or trimethylchlorosilane.
Beneficial effect of the present invention: by SiO
2nano-ITO, Ti is added in aerogel
5si
3, TiO
2etc. the nanometer powder with infrared external reflection ability, while maintaining the good normal temperature heat-proof quality of silica aerogel powder, due to nano-ITO, Ti
5si
3in powder for ultrared reflection, aerosil heat-proof quality at relatively high temperatures can be significantly improved.
Embodiment
Embodiment 1:
Adopt tetraethyl orthosilicate (TEOS), water, dehydrated alcohol, sulfuric acid as raw material, according to TEOS:H
2configure acid-sol, placement 12h after for subsequent use (system A) O: ethanol: sulfuric acid=1:1.5:15:0.01(mol).
By nano-ITO powder ultrasonic disperse in dehydrated alcohol, concentration controls 1%, (system B) for subsequent use.
It is 9 that system A ammonia soln is adjusted to pH value, then mixes with system B, nano-ITO: SiO
2control at 1:100(wt).Place after gel and carry out supercritical drying in 1 day.
Test thermal conductivity after completing, 300 degree are arrived hot coefficient at 0.029W/m/K
Embodiment 2:
Adopt tetraethyl orthosilicate (TEOS), water, dehydrated alcohol, sulfuric acid as raw material, according to TEOS:H
2configure acid-sol, placement 12h after for subsequent use (system A) O: ethanol: sulfuric acid=1:1.5:15:0.01(mol).
By nanometer Ti
5si
3powder ultrasonic is scattered in dehydrated alcohol, and concentration controls 1%, (system B) for subsequent use.
It is 9 that system A ammonia soln is adjusted to pH value, then mixes with system B, nanometer Ti
5si
3: SiO
2control at 1:100(wt).Place after gel and carry out supercritical drying in 1 day.
Test thermal conductivity after completing, 300 degree are arrived hot coefficient at 0.030W/m/K
Comparative example:
Adopt tetraethyl orthosilicate (TEOS), water, dehydrated alcohol, sulfuric acid as raw material, according to TEOS:H
2configure acid-sol, placement 12h after for subsequent use (system A) O: ethanol: sulfuric acid=1:1.5:15:0.01(mol).
It is 9 that system A ammonia soln is adjusted to pH value, places and carry out supercritical drying in 1 day after gel.
Test thermal conductivity after completing, 300 degree are arrived hot coefficient at 0.035W/m/K
Embodiment 3 ~ 8, with reference to embodiment 1, changes optimum configurations into, as shown in the table:
Claims (8)
1. a nanometer titanium dioxide silica aerogel preparation method, is characterized in that comprising the following steps: a. is by organosilane precursor: H
2* 10 O: low-carbon alcohol solvent: catalyzer=1:1-10:10-100:(0.1-100)
-3(mol) mix, place and carry out ageing in 0.1-4 days, obtained silicon-dioxide acid-sol;
B. be scattered in solvent by the nanometer powder with infrared external reflection ability, it is for subsequent use that stirring and/or ultrasonic disperse evenly obtain the nano-solution with infrared external reflection ability afterwards, and nanometer powder content controls at 0.1%-10%;
C. by silicon-dioxide acid-sol adjust ph, adjust ph after mixing with the nano-solution with infrared external reflection ability or silicon-dioxide acid-sol being mixed with the nano-solution with infrared external reflection ability, pH value controls as 8-12, the nanometer powder of described infrared external reflection ability: generate SiO
2=0.1-10:100(wt);
D. be saturatedly dipped on carrier, after isogel, carry out supercritical extraction after placing 0-48h, obtain finished product.
2. a kind of nanometer titanium dioxide silica aerogel preparation method according to claim 1, is characterized in that organosilane precursor is tetraethyl orthosilicate, the one of tetrachloro silicane or combination.
3. a kind of nanometer titanium dioxide silica aerogel preparation method according to claim 1, is characterized in that low-carbon alcohol solvent is ethanol, the one of propyl alcohol or combination.
4. a kind of nanometer titanium dioxide silica aerogel preparation method according to claim 1, is characterized in that catalyzer is organic or inorganic acid.
5. a kind of nanometer titanium dioxide silica aerogel preparation method according to claim 4, is characterized in that organic or inorganic acid is nitric acid, sulfuric acid, acetic acid are a kind of or combination.
6. a kind of nanometer titanium dioxide silica aerogel preparation method according to claim 1, the nanometer powder that it is characterized in that having infrared external reflection ability is nano indium tin oxide (ITO), Ti
5si
3one or combination.
7. a kind of nanometer titanium dioxide silica aerogel preparation method according to claim 1, adds properties-correcting agent and carries out hydrophobically modified in the time after it is characterized in that isogel before supercritical extraction.
8. a kind of nanometer titanium dioxide silica aerogel preparation method according to claim 7, is characterized in that properties-correcting agent is trimethyl silanol, hexamethyldisilazane or trimethylchlorosilane.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478055A (en) * | 2016-11-07 | 2017-03-08 | 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 |
| CN110436470A (en) * | 2019-09-06 | 2019-11-12 | 均一佳(武汉)科技有限公司 | A kind of Gel Treatment agent and its preparation method and application |
| 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 |
| CN115849862A (en) * | 2022-08-19 | 2023-03-28 | 希纳高科(江苏)有限公司 | Preparation method of nanowire fiber reinforced silica aerogel composite material |
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| JPH02304299A (en) * | 1989-05-05 | 1990-12-18 | Basf Ag | Heat insulating material mainly consisting of silica aerogel containing pigment |
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| CN101948296A (en) * | 2010-09-28 | 2011-01-19 | 航天特种材料及工艺技术研究所 | High-performance thermal insulation material and preparation method thereof |
| CN102557577A (en) * | 2011-11-01 | 2012-07-11 | 厦门纳美特新材料科技有限公司 | Preparation and method of silicon dioxide aerogel composite material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478055A (en) * | 2016-11-07 | 2017-03-08 | 江苏德威节能有限公司 | A kind of preparation method of the aerosil felt of hot pressing setting |
| 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 |
| CN110436470A (en) * | 2019-09-06 | 2019-11-12 | 均一佳(武汉)科技有限公司 | A kind of Gel Treatment agent and its preparation method and application |
| 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 |
| CN115849862A (en) * | 2022-08-19 | 2023-03-28 | 希纳高科(江苏)有限公司 | Preparation method of nanowire fiber reinforced silica aerogel composite material |
| 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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Address after: 214225 Nanyuan village, Yicheng street, Yixing City, Wuxi City, Jiangsu Province Patentee after: Jiangsu Dewei Energy Saving Group Co.,Ltd. Address before: 214553 Nanyuan village, Yicheng street, Yixing City, Wuxi City, Jiangsu Province Patentee before: JIANGSU DEWEI ENERGY-SAVING CO.,LTD. |