CN105130365A - Method and apparatus for preparing silicate fiber enhanced silica aerogel under routine conditions - Google Patents
Method and apparatus for preparing silicate fiber enhanced silica aerogel under routine conditions Download PDFInfo
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- CN105130365A CN105130365A CN201510381321.5A CN201510381321A CN105130365A CN 105130365 A CN105130365 A CN 105130365A CN 201510381321 A CN201510381321 A CN 201510381321A CN 105130365 A CN105130365 A CN 105130365A
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- Prior art keywords
- aerogel
- gel
- material preparation
- aerogel material
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 title claims abstract description 19
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title abstract description 10
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title abstract 3
- 239000004964 aerogel Substances 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 150000007524 organic acids Chemical class 0.000 claims abstract description 7
- 230000003068 static effect Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 18
- 238000007791 dehumidification Methods 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 150000004760 silicates Chemical class 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract description 2
- 239000000499 gel Substances 0.000 abstract 3
- 239000005995 Aluminium silicate Substances 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 abstract 1
- 229910000323 aluminium silicate Inorganic materials 0.000 abstract 1
- 235000012211 aluminium silicate Nutrition 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 239000000741 silica gel Substances 0.000 abstract 1
- 229910002027 silica gel Inorganic materials 0.000 abstract 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention relates to a method and an apparatus for preparing a silicate fiber enhanced silica aerogel under routine conditions. The aerogel preparation technology comprises uniformly mixing aluminium silicate fiber, a silicon source, anhydrous ethanol, an organic acid and deionized water in a certain pH value according to definite ratio and sequence so as to form an aerogel precursor solution, after stirring, adding proper amount of ammonia water and performing a sol-gel process, ageing for a certain period, and drying the formed gel under static routine conditions. By employing a vacuum-pumping device, a negative-pressure feeding device, an infrared heating device and other routine equipment, a static negative-pressure low-heat environment is provided for the formed silica gel, and by drying the gel in the environment, the aperture and the skeleton structure of the gel does not easily collapse or rupture, and the prepared silicate fiber enhanced silica aerogel is excellent in performances. The prepared aerogel with stable aperture and skeleton structure has the specific surface area of 450-750 m<2>/g, the pore volume of 1.5-2.5 cm<3>/g and the pore diameter of 1-40 nm.
Description
Technical field
The present invention relates to a kind of method and apparatus preparing aerogel, more specifically, under relating to normal condition, prepare the method and apparatus of ceramic fibre enhancement type aerosil.
Background technology
Aerosil
oneplant the nano-meter porous amorphous state solid material of low density, high porosity, transmittance is higher, also referred to as " blue smoke ", " solid cigarette ", gaseous state dispersion medium is full of in hole, there is continuous print nanoscale three-dimensional network structure and hole, be at present known in the world density minimum and the minimum solid material of thermal conductivity.Its bore hole size and network skeleton are nano level, bore hole size distribution range is 1 ~ 100 nanometer, network skeleton particle size distribution range is 1 ~ 30 nanometer, this special construction makes it have high porosity (80% ~ 99.8%), low density (3 ~ 250kg/m3), high-specific surface area (500 ~ 1000m2/g), low-k (1.1 ~ 2.5), low thermal conductivity (0.013 ~ 0.025w/(mk)) etc. feature, at mechanics, acoustics, calorifics, the many-sides such as optics have peculiar property, in space flight and aviation, military project, petrochemical industry, mineral products, electronics, medical, metallurgy etc. field has broad application prospects.
Prepare the technique of aerosil and device in prior art and usually there is the space of gel and subsiding or breaking easily appears in skeleton, supercritical drying device Keep Clear-High Voltage property is high, power consumption is large, yield poorly, expensive, and general normal pressure prepares aerogel method various problem such as very unstable in system pressure and temperature condition, therefore be badly in need of proposing a kind of novel processing step that can improve prior art and device, for the preparation of aerosil.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, now the present invention is proposed.
According to an aspect of the present invention, provide a kind of preparation method of aerosil, comprising:
According to fixing ratio and order, silicates fiber and silicon source, dehydrated alcohol, organic acid and deionized water are made gel precursor solution specifying to mix under pH, in gel precursor solution, admix proper ammonia gel, aging after, negative pressure pay-off is utilized gel to be sent into the dehumidification system of fixed temperature and pressure, under static normal condition, carry out gel drying, prepare aerogel.
According to the opposing party aspect of the present invention, provide a kind of preparation facilities of aerosil, comprising:
A kind of ceramic fibre enhancement type silica aerogel material preparation facilities, it is characterized in that, whole aerogel production equipment comprises mixing stirring system, plastic ageing system and a few major part of dehumidification system.
Adopt such scheme of the present invention, what can solve in the following problems existed in prior art is one or more: Keep Clear-High Voltage for supercritical drying device, power consumption large, output is few, expensive, general normal pressure prepares aerogel method system pressure, temperature condition is unstable, and gel pore and skeleton structure are very easily broken and subside.
Embodiment
According to one embodiment of present invention, provide a kind of method preparing ceramic fibre enhancement type silica aerogel material, comprise the steps: ceramic fibre such as alumina silica fiber and the silicon source being preferably organosilicon source, dehydrated alcohol, organic acid and deionized water are mixed into gel precursor solution specifying under pH, add appropriate ammoniacal liquor after stirring and carry out sol-gel process, aging again through the set time, under static normal condition, negative pressure pay-off is utilized gel to be sent into the dehumidification system of fixed temperature and pressure, drying is carried out to shaping gel.Wherein, preferably raw material is added according to fixing ratio and order.In the preferred embodiments of the present invention, the conventional equipments such as vacuum extractor, negative pressure pay-off and infrared heating device can be adopted, for shaping silica dioxide gel builds a static negative pressure low thermal environment, gel is dry in so static conventional environment, subsiding or breaking not easily appears in the hole of gel and skeleton structure, prepares the aerosil that the splendid alumina silica fiber of performance strengthens.
Preferably, gel precursor solution is according to mass ratio: ceramic fibre: organosilicon source: dehydrated alcohol: organic acid: the ratio mixing of deionized water=1:15:60:45:20 prepares, addition sequence is preferably ceramic fibre, organosilicon source, dehydrated alcohol, organic acid is finally deionized water.The precursor liquid pH value Absorbable organic halogens of mixing is 2 ~ 3.In drying process, the fixed temperature of dehumidification system can be 180 DEG C ± 5 DEG C, and the fixation pressure of dehumidification system can be 60kPa ± 5kPa.
According to another embodiment of the present invention, provide a kind of device preparing ceramic fibre enhancement type silica aerogel material, this device at least comprises mixing stirring system, plastic ageing system and a few major part of dehumidification system.In a preferred embodiment of the invention, mix stirring system and comprise material allocation device, pay-off, multiple feed inlet stirring and evenly mixing device three part.Wherein material allocation device can comprise work top, allotment bucket; Pay-off distinguishes solid and liquid, all preferably seals feeding; Multiple feed inlet stirring and evenly mixing device can arrange closed opening for feed according to material characteristic.Further, plastic ageing system can comprise into adhesive dispenser and ageing oven two portions.Become adhesive dispenser and ageing oven can be placed in clean confined chamber.Preferably, dehumidification system can comprise dry channel case, vacuum extractor, infrared heating device, negative pressure pay-off four part.Wherein, can transport unit be provided with in dry channel case, channel box both sides and on can arrange and vacuumize hole and Infrared Heating is sunken cord, feeder connection can adopt creeping motion type negative pressure pay-off, and passage two ends can arrange adjustable switch.
Adopt aforesaid method of the present invention and device can prepare hole and the stable aerogel of skeleton structure, aerogel specific surface area reaches 450 ~ 750m2/g, and pore volume is 1.5 ~ 2.5cm3/g, and aperture is 1 ~ 40nm.
It should be noted that above-described embodiment only illustrates inventive concept of the present invention for explaining, but not the restriction to rights protection of the present invention, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should fall into protection scope of the present invention.
Claims (9)
1. a ceramic fibre enhancement type silica aerogel material preparation method, it is characterized in that, silicates fiber and silicon source, dehydrated alcohol, organic acid and deionized water are made gel precursor solution specifying to mix under pH, in gel precursor solution, admix proper ammonia gel, aging after, negative pressure pay-off is utilized gel to be sent into the dehumidification system of fixed temperature and pressure, under static normal condition, carry out gel drying, prepare aerogel.
2. aerogel material preparation method as claimed in claim 1, is characterized in that, according to mass ratio: ceramic fibre: organosilicon source: dehydrated alcohol: organic acid: precursor solution is prepared in the ratio mixing of deionized water=1:15:60:45:20.
3. aerogel material preparation method as claimed in claim 1, it is characterized in that, the pH value of solution after mixing is stabilized in 2 ~ 3.
4. aerogel material preparation method as claimed in claim 1, it is characterized in that, dehumidification system fixed temperature is 180 DEG C ± 5 DEG C.
5. aerogel material preparation method as claimed in claim 1, it is characterized in that, dehumidification system fixation pressure is 60kPa ± 5kPa.
6. a ceramic fibre enhancement type silica aerogel material preparation facilities, is characterized in that, whole aerogel production equipment comprises mixing stirring system, plastic ageing system and a few major part of dehumidification system.
7. aerogel material preparation facilities as claimed in claim 6, is characterized in that, mixing stirring system comprises material allocation device, pay-off, multiple feed inlet stirring and evenly mixing device three part, and wherein material allocation device comprises work top, allotment bucket; Pay-off distinguishes solid and liquid, is sealing feeding; Multiple feed inlet stirring and evenly mixing device arranges closed opening for feed according to material characteristic.
8. aerogel material preparation facilities as claimed in claim 6, it is characterized in that, plastic ageing system comprises into adhesive dispenser and ageing oven two portions, wherein becomes adhesive dispenser and ageing oven to be placed in clean confined chamber.
9. aerogel material preparation facilities as claimed in claim 6, it is characterized in that, dehumidification system comprises dry channel case, vacuum extractor, infrared heating device, negative pressure pay-off four part, wherein, transport unit is provided with in dry channel case, channel box both sides and top arrange and vacuumize hole and Infrared Heating is sunken cord, and feeder connection adopts creeping motion type negative pressure pay-off, and passage two ends arrange adjustable switch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510381321.5A CN105130365A (en) | 2015-07-03 | 2015-07-03 | Method and apparatus for preparing silicate fiber enhanced silica aerogel under routine conditions |
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| CN201510381321.5A CN105130365A (en) | 2015-07-03 | 2015-07-03 | Method and apparatus for preparing silicate fiber enhanced silica aerogel under routine conditions |
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| CN105130365A true CN105130365A (en) | 2015-12-09 |
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| CN201510381321.5A Pending CN105130365A (en) | 2015-07-03 | 2015-07-03 | Method and apparatus for preparing silicate fiber enhanced silica aerogel under routine conditions |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111363416A (en) * | 2020-05-21 | 2020-07-03 | 天津市宏越新材料有限公司 | Intumescent steel structure fireproof coating and preparation method and application thereof |
| CN113071186A (en) * | 2021-03-26 | 2021-07-06 | 深圳市雷军科技有限公司 | Impact-resistant heat-insulating nano material and preparation method thereof |
| CN115010501A (en) * | 2022-06-08 | 2022-09-06 | 佛山市中柔材料科技有限公司 | Elastic ceramic micro-nanofiber aerogel heat insulation material and preparation method and application thereof |
Citations (3)
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| WO2005084650A1 (en) * | 2004-03-03 | 2005-09-15 | Switch Biotech Ag | Pharmaceutical composition for topical use in form of xerogels or films and methods for production |
| CN102115088A (en) * | 2010-01-04 | 2011-07-06 | 新疆大学 | Method for preparing silicon dioxide aerogel by using alcohol amine as alkaline catalyst |
| CN103272539A (en) * | 2013-05-07 | 2013-09-04 | 李光武 | Method and device for preparing aerogel by drying under reduced pressure |
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2015
- 2015-07-03 CN CN201510381321.5A patent/CN105130365A/en active Pending
Patent Citations (3)
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| WO2005084650A1 (en) * | 2004-03-03 | 2005-09-15 | Switch Biotech Ag | Pharmaceutical composition for topical use in form of xerogels or films and methods for production |
| CN102115088A (en) * | 2010-01-04 | 2011-07-06 | 新疆大学 | Method for preparing silicon dioxide aerogel by using alcohol amine as alkaline catalyst |
| CN103272539A (en) * | 2013-05-07 | 2013-09-04 | 李光武 | Method and device for preparing aerogel by drying under reduced pressure |
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| 任海东: "《机电类高职高专规划教材 冷冲压工艺与模具设计》", 30 September 2007, 河南科学技术出版社 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111363416A (en) * | 2020-05-21 | 2020-07-03 | 天津市宏越新材料有限公司 | Intumescent steel structure fireproof coating and preparation method and application thereof |
| CN111363416B (en) * | 2020-05-21 | 2022-04-22 | 天津市宏越新材料有限公司 | Intumescent steel structure fireproof coating and preparation method and application thereof |
| CN113071186A (en) * | 2021-03-26 | 2021-07-06 | 深圳市雷军科技有限公司 | Impact-resistant heat-insulating nano material and preparation method thereof |
| CN115010501A (en) * | 2022-06-08 | 2022-09-06 | 佛山市中柔材料科技有限公司 | Elastic ceramic micro-nanofiber aerogel heat insulation material and preparation method and application thereof |
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Application publication date: 20151209 |
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