CN1317233C - Silica aerogel powder moulding method adopting gel injection molding method - Google Patents
Silica aerogel powder moulding method adopting gel injection molding method Download PDFInfo
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- CN1317233C CN1317233C CNB2005100120979A CN200510012097A CN1317233C CN 1317233 C CN1317233 C CN 1317233C CN B2005100120979 A CNB2005100120979 A CN B2005100120979A CN 200510012097 A CN200510012097 A CN 200510012097A CN 1317233 C CN1317233 C CN 1317233C
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Abstract
The present invention provides a method of silica aerogel powder formed by a gel injection molding method. The present invention belongs to the technical field of heat insulating material preparation, and has the technology that a stable suspension liquid is prepared with an organic monomer, crosslinking agents, dispersing agents and silica aerogel powder; 0.1 to 0.8 % of initiating agents by volume and 0.1 to 0.35 % of catalysts by volume are added to the suspension liquid; the suspension liquid which is mixed evenly is injected in a mould and removes bubble within 1 to 5 minutes in vacuum, then the mould which is filled with the suspension liquid is put in water bath at the temperature of 50 to 80 DEG C and keeps constant temperature for 15 min to 3 hours, and a solidified base substrate is obtained. The base substrate is demoulded and dried, and the base substrate carries out heat treatment to obtain a silica aerogel forming body with a certain shape and intensity. The present invention has the advantages that compared with dry pressing forming, hot pressure forming and supercritical dryness primary forming, the method has simple technology, low cost, low bulk density of the obtained silica aerogel forming, high intensity and good heat-insulating property.
Description
Technical field
The invention belongs to the lagging material preparing technical field.A kind of method that adopts gel casting process to come the moulding silica aerogel powder particularly is provided.
Technical background
Along with various countries' rapid development of national economy, mechanize, automatization, electrified degree are more and more higher, and the demand pressure of the energy is huge, energy-conservationly are imminent.Lagging material is cutting down the consumption of energy like this, and the meaning that improves the energy utilization rate aspect is also just more outstanding.
Traditional lagging material adopts asbestos, polyurethane foamed material, pearlstone etc. more.They exist respectively that heat resisting temperature is low, the shortcoming of contaminate environment or heat-proof quality difference.Along with the development of modern science and technology, particularly the development of hard-core technologies such as some military projects, aerospace has proposed more and more higher requirement to lagging material.Traditional lagging material has been difficult to adapt to this demand.Therefore, research and develop the focus that the lagging material with low thermal conductivity becomes present material worker research.
Silica aerogel is a kind of novel nanometer, porous, low density, amorphous material, has the continuous three-dimensional network structure, thereby the heat-proof quality (M.Schmidt that shows abnormality superior, F.Schwertfeger, Journal ofNon-crystalline Solids, 1998,225,364-368).Yet,, all require material not only to have low thermal conductivity and also will have certain shape and higher physical strength for the mostly application aspect heat insulation.
The silica aerogel formed body of being reported mainly is to be prepared by the supercritical drying drying method, as patent EP-A-O 396076 is that colloidal sol or gel are placed autoclave, add certain amount of solvent and with the air in nitrogen or other inert gas replacement still, with certain temperature rise rate heating, when the temperature and pressure in the still reaches supercritical state, after keeping for some time, release also is cooled to room temperature and promptly obtains the aerogel product.The silica aerogel formed body that this method is prepared has kept the original structure of wet gel, porous nickel, and thermal conductivity is little.Yet the pressure technique that relates in the supercritical drying is absolutely unsafe, and apparatus expensive, complex process, and is in addition, very big with the fragility of the silica aerogel of supercritical process preparation.Subcritical drying means prepares aerogel, as patent WO9606051 is to adopt the solvent with volume effect to make drying medium, the aerogel of this method preparation is basic identical with supercritical drying on microtexture, owing to reduced drying pressure, thereby reduced the preparation risk, but the production cost of this method is still very high, and complex process.The method of compacting aerogels is to add in the compression moulding device aerogel particle and compression molding as patent CN 1258231A.This method prepares the aerogel formed body, and technology is fairly simple, but too high pressure can destroy the original pore space structure of aerogel, thereby influences its heat-proof quality.Therefore, research and develop that a kind of cost is low, technology is simple, physical strength is high, be convenient to the preparation method of silica aerogel formed body of mass-producing safety in production for promoting that silica aerogel has crucial meaning in the practical application aspect heat insulation.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts gel casting process to come the moulding silica aerogel powder, reduced cost, simplified technology, improved physical strength, and production security is good.
Concrete technology of the present invention is:
A, preparation contain the more stable suspension of organic monomer, linking agent, dispersion agent, opalizer and silica aerogel powder; The concrete technology of suspension preparation is: monomer, linking agent, water are made into premixed liquid in mixing equipment; Monomer in the premixed liquid: the ratio of linking agent is 24: 1～1.5 (mass ratioes), and the concentration of monomer in the aqueous solution is 5～20 quality %; Silica aerogel powder and opalizer and dispersion agent added carry out mechanical ball milling in the above-mentioned premixed liquid and mix and obtain suspension; The solid contents of suspension is 50～80 volume %, and the add-on of dispersion agent is 0.5～1.5 quality % of silica aerogel powder; The adding of solids is that branch adds for 2～5 times in batches; Opalizer is TiO
2, Fe
3O
4Wherein 1～2 kind.Its total content is 0～30 quality % of silica aerogel powder.
B, in suspension, add initiator and catalyzer; With respect to the volume of suspension, the add-on of initiator is 0.1～0.8 volume %, and the add-on of catalyzer is 0.1～0.35 volume %; The suspension that mixes was injected mould and froth in vacuum 1～5 minute, and it is 50～80 ℃ water-bath constant temperature 15 minutes～3 hours that the mould that suspension will be housed is then put into temperature, makes the solidified base substrate;
C, with the base substrate demoulding, drying and heat-treat the silica aerogel formed body that can obtain to have definite shape and intensity; The drying of base substrate is under the wet condition of control dry 40～60 hours, then 50～70 ℃ of dryings 12～24 hours in baking oven, 105～130 ℃ of dryings 15～30 hours in baking oven again; Thermal treatment temp is 300～600 ℃, and in the heat treatment process, temperature rise rate is 1～2 ℃/min, and soaking time is 1～8 hour, cools to room temperature naturally with the furnace.
Organic monomer of the present invention is acrylamide AM; Described linking agent is methylene-bisacrylamide MBAM; And organic monomer and linking agent are water miscible.Described dispersion agent is a polyacrylamide; Described initiator is an ammonium persulphate; Described catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
The particle diameter of silica aerogel powder of the present invention is 200 μ m～100nm; And the porosity of silica aerogel powder is 60～98%, and density is 0.01～0.5g/cm
3The silica aerogel surface does not have the hydrophobic group.
The material of forming mould of the present invention is tetrafluoroethylene or polystyrene or polypropylene.
The invention has the advantages that: compare with the supercritical methanol technology moulding of generally using, this method cost is low, and technology is simple, production safety, and resulting silica aerogel formed body intensity is big; Compare with dry pressure formed, the porosity height of the silica aerogel formed body that this method is prepared, intensity is big.
Description of drawings
Fig. 1 is the process flow sheet of gel injection method moulding silica aerogel powder
Embodiment
Example 1
Acrylamide AM: methylene-bisacrylamide is made into premixed liquid by weight 24: 1 and water, and wherein the concentration of acrylamide in suspension is 15 quality %.The introducing median size is 50 microns a silica aerogel powder, slip solid load 60 volume %, and the add-on of dispersion agent is 1 quality % of dry powder weight.Wherein, aerogel powder will add in batches, and being respectively for 1/2,1/6,1/6,1/6 each reinforced pitch time is 20 hours.Powder is all added the back and was continued ball milling 24 hours, and mixture is blended into suspension.
In suspension, add the Tetramethyl Ethylene Diamine of 0.15 volume % and the ammonium persulphate of 0.3 volume %, back injection mould stirs, froth in vacuum 4 minutes, put temperature into and be in 60 ℃ the water-bath constant temperature 25 minutes, after the demoulding under the wet condition of control dry 48 hours, put into 55 ℃ in baking oven then dry 12 hours down, then temperature is upgraded to 110 ℃ dry 24 hours again.At last the exsiccant base substrate is placed stove, be raised to 550 ℃, be incubated 2 hours, cool to room temperature then with the furnace with the temperature rise rate of 2 ℃/min.The volume density of the silica aerogel formed body of preparation is 0.451g/cm
3, folding strength is 6MPa, the thermal conductivity under the room temperature is 0.1W/m.K.
Example 2
Acrylamide: methylene-bisacrylamide is made into premixed liquid by weight 24: 1.5 ratios and water, and wherein the concentration of acrylamide in suspension is 12 quality %.The introducing median size is 70 microns a silica aerogel powder, slip solid load 75 volume %, and the add-on of dispersion agent is 0.8 quality % of dry powder weight.Wherein, aerogel powder will add in batches, and being respectively for 1/2,1/4,1/4 each reinforced pitch time is 30 hours, and when adding powder first, adding particle diameter in addition is the TiO of 10 microns 10 quality % (with respect to silica aerogel powder)
2Powder.All add the back and continued ball milling 24 hours, mixture is blended into suspension.
In suspension, add the Tetramethyl Ethylene Diamine of 0.25 volume % and the Ammonium Persulfate 98.5 of 0.7 volume %, back injection mould stirs, froth in vacuum 2 minutes, put temperature into and be in 50 ℃ the water-bath constant temperature 1 hour, after the demoulding under the wet condition of control dry 60 hours, put into 50 ℃ in baking oven then dry 20 hours down, then temperature is upgraded to 130 ℃ dry 15 hours again.At last the exsiccant base substrate is placed stove, be raised to 500 ℃, be incubated 6 hours, cool to room temperature then with the furnace with the temperature rise rate of 1 ℃/min.The volume density of the silica aerogel formed body of preparation is 0.572g/cm
3, folding strength is 7.21MPa, thermal conductivity 0.12W/m.K under the room temperature.
Claims (4)
1, a kind of method that adopts gel casting process to come the moulding silica aerogel powder is characterized in that: concrete technology is:
A, preparation contain the more stable suspension of organic monomer, linking agent, dispersion agent, opalizer and silica aerogel powder; The concrete technology of suspension preparation is: monomer, linking agent, water are made into premixed liquid in mixing equipment; Monomer in the premixed liquid: the ratio of linking agent is 24: 1～1.5 mass ratioes, and the concentration of monomer in premixed liquid is 5～20 quality %; Silica aerogel powder and opalizer and dispersion agent added carry out mechanical ball milling in the above-mentioned premixed liquid and mix and obtain suspension; The solid contents of suspension is 50～80 volume %, and the add-on of dispersion agent is 0.5～1.5 quality % of silica aerogel powder; The adding of solids is that branch adds for 2～5 times in batches; Opalizer is TiO
2, Fe
3O
4Wherein 1～2 kind, its total content is 0～30 quality % of silica aerogel powder;
B, in suspension, add initiator and catalyzer; With respect to the volume of suspension, the add-on of initiator is 0.1～0.8 volume %, and the add-on of catalyzer is 0.1～0.35 volume %; The suspension that mixes was injected mould and froth in vacuum 1～5 minute, and it is 50～80 ℃ water-bath constant temperature 15 minutes～3 hours that the mould that suspension will be housed is then put into temperature, makes the solidified base substrate;
C, with the base substrate demoulding, drying and heat-treat the silica aerogel formed body that can obtain to have definite shape and intensity; The drying of base substrate is under the wet condition of control dry 40～60 hours, then 50～70 ℃ of dryings 12～24 hours in baking oven, 105～130 ℃ of dryings 15～30 hours in baking oven again; Thermal treatment temp is 300～600 ℃, and in the heat treatment process, temperature rise rate is 1～2 ℃/min, and soaking time is 1～8 hour, cools to room temperature naturally with the furnace.
2, in accordance with the method for claim 1, it is characterized in that: described organic monomer is an acrylamide; Described linking agent is a methylene-bisacrylamide; And organic monomer and linking agent are water miscible; Described dispersion agent is a polyacrylamide; Described initiator is an ammonium persulphate; Described catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
3, in accordance with the method for claim 1, it is characterized in that: the particle diameter of described silica aerogel powder is 200 μ m～100nm; And the porosity of silica aerogel powder is 60～98%, and density is 0.01～0.5g/cm
3The silica aerogel surface does not have the hydrophobic group.
4, in accordance with the method for claim 1, it is characterized in that: the material of described forming mould is tetrafluoroethylene or polystyrene or polypropylene.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100120979A CN1317233C (en) | 2005-07-06 | 2005-07-06 | Silica aerogel powder moulding method adopting gel injection molding method |
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| CNB2005100120979A CN1317233C (en) | 2005-07-06 | 2005-07-06 | Silica aerogel powder moulding method adopting gel injection molding method |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525248B (en) * | 2009-04-22 | 2012-07-04 | 哈尔滨工业大学 | Ceramic aerogel and method for preparing the ceramic aerogel by gel injection moulding |
| CN102503508B (en) * | 2011-10-27 | 2013-10-30 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing alumina nanometer porous thermal insulation materials |
| CN102491741A (en) * | 2011-11-15 | 2012-06-13 | 张天舒 | Method for preparing ITO ceramic target |
| CN103272539B (en) * | 2013-05-07 | 2015-08-12 | 李光武 | Drying under reduced pressure prepares the method for aeroge |
| CN104291773B (en) * | 2014-09-29 | 2016-01-27 | 同济大学 | The preparation method of the anti-intense radiation block materials that a kind of low density ultrahigh-temperature is stable |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0396076A1 (en) * | 1989-05-05 | 1990-11-07 | BASF Aktiengesellschaft | Thermal insulating materials based on pigmentic silicia aerogels |
| CN1258231A (en) * | 1997-05-02 | 2000-06-28 | 卡伯特公司 | Method for compacting aerogels |
| CN1456535A (en) * | 2003-05-30 | 2003-11-19 | 武汉理工大学 | Process for preparing porous ceramic by water-based gel injection moulding method |
| CN1559984A (en) * | 2004-03-01 | 2005-01-05 | 清华大学 | Method of gas phase deglue pretreating for gel injucting molding ceranuc blank |
-
2005
- 2005-07-06 CN CNB2005100120979A patent/CN1317233C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0396076A1 (en) * | 1989-05-05 | 1990-11-07 | BASF Aktiengesellschaft | Thermal insulating materials based on pigmentic silicia aerogels |
| CN1258231A (en) * | 1997-05-02 | 2000-06-28 | 卡伯特公司 | Method for compacting aerogels |
| CN1456535A (en) * | 2003-05-30 | 2003-11-19 | 武汉理工大学 | Process for preparing porous ceramic by water-based gel injection moulding method |
| CN1559984A (en) * | 2004-03-01 | 2005-01-05 | 清华大学 | Method of gas phase deglue pretreating for gel injucting molding ceranuc blank |
Non-Patent Citations (4)
| Title |
|---|
| 硅粉凝胶注模成型的研究 谈国强，中国陶瓷工业，第11卷第4期 2004 * |
| 精密陶瓷凝胶注模成型工艺评述 王刚，材料科学与工程学报，第21卷第4期 2003 * |
| 高压陶瓷电容器凝胶注模成型研究 陈寿田，陶瓷学报，第22卷第4期 2001 * |
| 高压陶瓷电容器凝胶注模成型研究 陈寿田，陶瓷学报，第22卷第4期 2001;硅粉凝胶注模成型的研究 谈国强，中国陶瓷工业，第11卷第4期 2004;精密陶瓷凝胶注模成型工艺评述 王刚，材料科学与工程学报，第21卷第4期 2003 * |
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