CN102167983B - Preparation method of low-density high-temperature-resistant aluminum oxide thermal-insulation material - Google Patents
Preparation method of low-density high-temperature-resistant aluminum oxide thermal-insulation material Download PDFInfo
- Publication number
- CN102167983B CN102167983B CN 201110058828 CN201110058828A CN102167983B CN 102167983 B CN102167983 B CN 102167983B CN 201110058828 CN201110058828 CN 201110058828 CN 201110058828 A CN201110058828 A CN 201110058828A CN 102167983 B CN102167983 B CN 102167983B
- Authority
- CN
- China
- Prior art keywords
- polyoxyethylene
- hours
- temperature
- ethanol
- low
- 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.)
- Expired - Fee Related
Links
Images
Abstract
The invention discloses a preparation method of a low-density high-temperature-resistant aluminum oxide thermal-insulation material, which comprises the following steps: introducing a phase splitting process in a sol-gel method, drying at normal temperature, and carrying out heat treatment at certain temperature to obtain the low-density high-temperature-resistant aluminum oxide thermal-insulation material. The low-density high-temperature-resistant aluminum oxide thermal-insulation material has a hollow microspherical mesoporous-microporous dual structure, and has the advantages of high porosity, low density, low thermal conductivity, favorable high-temperature insulation performance and high strength. The method disclosed by the invention has the advantages of simple technique and low cost, is suitable for industrial production, and has important application prospects in the field of high-temperature insulation.
Description
Technical field
The present invention relates to a kind of preparation method of low density high-temperature resistant aluminium oxide lagging material.
Background technology
The characteristics of porous material are that density is little, and porosity is high, and specific surface area is large, see through effect etc. to gas is selective, be widely used at present various fields, as prevent the loss of heat as lagging material, come one-tenth useful in the Recycling of waste liquid to grade as sorbing material.Under the situation that the energy and environment problem becomes increasingly conspicuous, research preparation high porosity, high-specific surface area, high-intensity porous material has become the emphasis of current scientific research.
Porous material (aerogel) with good thermal and insulating performance uses the sol-gel method preparation usually, normal operation hydrolysis metal alkoxide makes its gelation and cooperates the supercritical drying preparation, but this method has shortcoming clearly: the one, and the metal alkoxide that uses is expensive, the preparation difficulty, hydrolysis rate control difficulty is difficult to industrial applications in the hydrolytic process; The 2nd, the supercritical drying equipment that uses is complicated, and operating process is loaded down with trivial details, and relatively more dangerous, is difficult to obtain large-sized block body stephanoporate material.In addition, adopt the porous material (aerogel) of supercritical drying preparation at high temperature very easily to produce sintering shrinkage, heat insulating in the time of can't being applied to high temperature, therefore, simple, with low cost, the resistant to elevated temperatures novel low density high temperature resistant heat insulation material of development preparation technology tool is of great significance.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, with low cost, be fit to the preparation method of the low density high-temperature resistant aluminium oxide lagging material of suitability for industrialized production.
The preparation method of low density high-temperature resistant aluminium oxide lagging material of the present invention may further comprise the steps
1) gets crystal aluminum chloride, ethanol, deionized water, 1,2-propylene oxide and polyoxyethylene, its mass ratio is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Qu Li Shui ﹕ 1,2-Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕ 0.9-1.1 ﹕ 1.2-1.6 ﹕ 0.014-0.028;
2) under 15 ℃ of-25 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 800 ℃-1200 ℃ thermal treatment 1-5 hour, obtain low density high-temperature resistant aluminium oxide lagging material.
The present invention can change the microscopic appearance of low density high-temperature resistant aluminium oxide lagging material by regulating content and bath temperature and the thermal treatment temp of the polyoxyethylene, 1,2 epoxy prapane and the deionized water that add, realizes that macroscopical density is at 0.1-0.6g/cm
3The Effective Regulation of scope.
The present invention compares with technical background, has following advantage:
The cost of material that the present invention uses is cheap, and the equipment of use is simple, and is easy to operate, and can prepare the high temperature resistant porous alumina lagging material of large-sized low density.The microtexture of the low density high-temperature resistant aluminium oxide lagging material that the inventive method obtains is that hollow ball is piled up, and mesoporous-micropore dual structure that the hollow ball surface exists has high porosity, low density (0.1-0.6g/cm
3), high strength, high temperature resistant (1200
oC), the characteristics such as thermal conductivity is low have important application in the high temperature insulating field.
Description of drawings
Fig. 1 is the low power electron scanning micrograph of the low density high-temperature resistant aluminium oxide lagging material of embodiment 1 preparation.
Fig. 2 is the high power electron scanning micrograph of the low density high-temperature resistant aluminium oxide lagging material of embodiment 1 preparation.
Embodiment:
Embodiment 1
1) the raw materials quality ratio of the present embodiment use is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Qu Li Shui ﹕ 1,2-Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕, 0.9 ﹕, 1.6 ﹕ 0.014;
2) under 15 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 800 ℃ of thermal treatments 5 hours, obtain low density high-temperature resistant aluminium oxide lagging material.
The density of the low density porous aluminum oxide lagging material that this embodiment prepares is as shown in table 1.Its microscopic appearance is seen Fig. 1, Fig. 2.
Embodiment 2
1) the raw materials quality ratio of the present embodiment use is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Shui ﹕ Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕, 0.9 ﹕, 1.6 ﹕ 0.014;
2) under 15 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 800 ℃ of thermal treatments 3 hours, obtain low density high-temperature resistant aluminium oxide lagging material.
The density of the low density porous aluminum oxide lagging material that this embodiment prepares is as shown in table 1.
Embodiment 3
1) the raw materials quality ratio of the present embodiment use is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Shui ﹕ Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕, 0.9 ﹕, 1.6 ﹕ 0.028;
2) under 25 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 800 ℃ of thermal treatments 5 hours, obtain low density high-temperature resistant aluminium oxide lagging material.
The density of the low density porous aluminum oxide lagging material that this embodiment prepares is as shown in table 1.
Embodiment 4
1) the raw materials quality ratio of the present embodiment use is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Shui ﹕ Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕, 1.1 ﹕, 1.6 ﹕ 0.014;
2) under 25 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 800 ℃ of thermal treatments 1 hour, obtain low density high-temperature resistant aluminium oxide lagging material.
The density of the low density porous aluminum oxide lagging material that this embodiment prepares is as shown in table 1.
Embodiment 5
1) the raw materials quality ratio of the present embodiment use is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Shui ﹕ Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕, 0.9 ﹕, 1.6 ﹕ 0.014;
2) under 25 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 1200 ℃ of thermal treatments 1 hour, obtain low density high-temperature resistant aluminium oxide lagging material.
The density of the low density porous aluminum oxide lagging material that this embodiment prepares is as shown in table 1.
Embodiment 6
1) the raw materials quality ratio of the present embodiment use is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Shui ﹕ Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕, 0.9 ﹕, 1.2 ﹕ 0.014;
2) under 25 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 800 ℃ of thermal treatments 5 hours, obtain low density high-temperature resistant aluminium oxide lagging material.
The density of the low density porous aluminum oxide lagging material that this embodiment prepares is as shown in table 1.
Low density porous aluminum oxide lagging material density measurement result after table 1 thermal treatment
| The embodiment numbering | Macroscopic view density (g/cm 3) |
| 1 | 0.1142 |
| 2 | 0.3701 |
| 3 | 0.2907 |
| 4 | 0.4284 |
| 5 | 0.1502 |
| 6 | 0.5963 |
Claims (1)
1. the preparation method of a low density high-temperature resistant aluminium oxide lagging material is characterized in that may further comprise the steps
1) gets crystal aluminum chloride, ethanol, deionized water, 1,2-propylene oxide and polyoxyethylene, its mass ratio is: crystallization Lvization Lv ﹕ Yi Chun ﹕ Qu Li Shui ﹕ 1,2-Huan Yang Bing Wan ﹕ polyoxyethylene=1 ﹕, 1 ﹕ 0.9-1.1 ﹕ 1.2-1.6 ﹕ 0.014-0.028;
2) under 15 ℃ of-25 ℃ of water bath with thermostatic control conditions, polyoxyethylene and ethanol are mixed, polyoxyethylene is well dispersed in the ethanol;
3) keep water bath with thermostatic control, under agitation condition, mixed solution and dripping deionized water at ethanol and polyoxyethylene, make polyoxyethylene be dissolved in the deionized water fully, then add crystal aluminum chloride, crystal aluminum chloride is fully dissolved after, add again 1, the 2-propylene oxide stirs and pours in the mould after 10 seconds;
4) with die sealing, placed 24 hours, form gel;
5) gel is immersed in the aqueous isopropanol wears out, the consumption of Virahol is 3 times of gel volume, changes Virahol one time every 24 hours in originally 72 hours, is immersed in after 72 hours and is aged to 7 days in the aqueous isopropanol;
6) remove aging liquid, dry under the normal temperature, obtain the porous alumina xerogel;
7) with the porous alumina xerogel 800 ℃-1200 ℃ thermal treatment 1-5 hour, obtain low density high-temperature resistant aluminium oxide lagging material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110058828 CN102167983B (en) | 2011-03-11 | 2011-03-11 | Preparation method of low-density high-temperature-resistant aluminum oxide thermal-insulation material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110058828 CN102167983B (en) | 2011-03-11 | 2011-03-11 | Preparation method of low-density high-temperature-resistant aluminum oxide thermal-insulation material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102167983A CN102167983A (en) | 2011-08-31 |
| CN102167983B true CN102167983B (en) | 2013-01-09 |
Family
ID=44489302
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110058828 Expired - Fee Related CN102167983B (en) | 2011-03-11 | 2011-03-11 | Preparation method of low-density high-temperature-resistant aluminum oxide thermal-insulation material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102167983B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688760B (en) * | 2016-01-18 | 2018-01-12 | 浙江大学 | A kind of oxide composite aerogel for the micro-nano porous structure for having um porous/nanoporous concurrently and preparation method thereof |
| CN105670616A (en) * | 2016-03-08 | 2016-06-15 | 浙江大学 | Manganous ion doped spherical aluminum nitride red-light phosphor and preparation method thereof |
| CN109337350B (en) * | 2018-09-11 | 2021-02-12 | 东莞市雄林新材料科技股份有限公司 | Temperature-resistant TPU film for automotive interior and preparation method thereof |
| CN111099909B (en) * | 2019-12-30 | 2020-12-29 | 浙江大学 | High-performance ceramic with surface modified polycrystalline mullite fiber compounded with rare earth lanthanum zirconate and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254449A (en) * | 2008-03-20 | 2008-09-03 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Preparation of oxide nano thread reinforced transparency aerogel block body material |
| CN101456569A (en) * | 2008-07-22 | 2009-06-17 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for quick-speed preparing aerogel by hydro-thermal synthesis at low cost |
-
2011
- 2011-03-11 CN CN 201110058828 patent/CN102167983B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254449A (en) * | 2008-03-20 | 2008-09-03 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Preparation of oxide nano thread reinforced transparency aerogel block body material |
| CN101456569A (en) * | 2008-07-22 | 2009-06-17 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for quick-speed preparing aerogel by hydro-thermal synthesis at low cost |
Non-Patent Citations (6)
| Title |
|---|
| Al2O3气凝胶常压干燥制备方法的研究;黄宝;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20081215;摘要，第15-18页，第22-60页 * |
| Structural characterization of hierachically porous alumina aerogel and xerogel monoliths;Yasuaki Tokudome et.al;《Journal of Colloid and Interface Science》;20091015;第338卷(第2期);第506-513页 * |
| Synthesis of High-Surface-Area Alumina Aerogels without the Use of Alkoxide Precursors;Theodore F. et.al;《Chem.Mater.》;20041224;第17卷(第2期);第395-401页 * |
| Theodore F. et.al.Synthesis of High-Surface-Area Alumina Aerogels without the Use of Alkoxide Precursors.《Chem.Mater.》.2004,第17卷(第2期),第395-401页. |
| Yasuaki Tokudome et.al.Structural characterization of hierachically porous alumina aerogel and xerogel monoliths.《Journal of Colloid and Interface Science》.2009,第338卷(第2期),第506-513页. |
| 黄宝.Al2O3气凝胶常压干燥制备方法的研究.《中国优秀硕士学位论文全文数据库 工程科技I辑》.2008,摘要，第15-18页，第22-60页. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102167983A (en) | 2011-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103086692B (en) | Preparation method of blocky SiO2-Y2O3 compound aerogel | |
| CN102167983B (en) | Preparation method of low-density high-temperature-resistant aluminum oxide thermal-insulation material | |
| CN108689679A (en) | A kind of preparation method of high temperature resistant gradient fiber composite aerogel heat-insulating material | |
| CN104495859A (en) | Preparation method of silicon dioxide aerogel | |
| CN105712400B (en) | Method for preparing zirconia aerogel material | |
| CN103420352A (en) | High-fluoride-content graphite fluoride and preparation method thereof | |
| CN104478475B (en) | A kind of high temperature resistance and high strength SiC carbon coated foam composite heat-insulated material and its preparation method | |
| CN102716700B (en) | Preparation method for high-strength heat-resisting massive C-AlN compound aerogel | |
| CN104761235A (en) | Preparation method of low-temperature-resistant glass-fiber-reinforced SiO2 aerogel composite material | |
| CN105236912A (en) | Composite fiber-reinforced hydrophobic SiO2 aerogel and preparation method thereof | |
| CN106145999B (en) | A kind of bulk La2O3-Al2O3The preparation method of composite aerogel | |
| CN103721645B (en) | A kind of carbon aerogels for electric adsorption electrode and preparation method thereof | |
| CN103408279A (en) | Thermal insulation aerogel material for buildings, and preparation method of aerogel material | |
| CN108358212A (en) | The preparation method and silica aerogel particles of silica aerogel particles | |
| CN107827116A (en) | A kind of preparation method of porous silica silicon bulk aeroge | |
| CN105271403A (en) | Method for preparing zirconium oxide aerogel through combination of secondary gelling method and ambient-pressure drying | |
| CN104556210B (en) | A kind of employing hot two-step method of microwave-assisted solvent prepares Sm2sn2o7/ SnO2the method of nano-complex | |
| CN106186034B (en) | A kind of La2O3The preparation method of aerogel particle | |
| CN102674375A (en) | Method for preparing silica aerogel with low cost in water system | |
| CN102513041B (en) | Method for preparing high-strength and high-temperature-resistance carbon-supported Al2O3-Al4C3 composite blocky aerogel | |
| CN106430265B (en) | Method of the aluminum for alumina aerogels is extracted from bauxite | |
| WO2017211227A1 (en) | High-strength large dimension block-form aerographite, and manufacturing method and application thereof | |
| CN108483452A (en) | A kind of preparation method of the blocky graded composite aeroge of low cost | |
| CN110642257B (en) | Method for preparing silicon dioxide aerogel by using silicon micropowder | |
| CN111215008A (en) | Method for preparing GO-sodium alginate composite microspheres |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130109 Termination date: 20180311 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |