CN102515182A - Method for preparing SiO2 aerogel by compounding flyash and kieselguhr - Google Patents
Method for preparing SiO2 aerogel by compounding flyash and kieselguhr Download PDFInfo
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- CN102515182A CN102515182A CN2011104457845A CN201110445784A CN102515182A CN 102515182 A CN102515182 A CN 102515182A CN 2011104457845 A CN2011104457845 A CN 2011104457845A CN 201110445784 A CN201110445784 A CN 201110445784A CN 102515182 A CN102515182 A CN 102515182A
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- flyash
- zeyssatite
- kieselguhr
- sio2
- aerogel
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Abstract
The invention provides a method for preparing a SiO2 aerogel by compounding flyash and kieselguhr. The method comprises six steps of mechanically activating the flyash and the kieselguhr at intermediate temperature, preparing a SiO2 sol, preparing a wet gel, ageing a mother solution, performing one-step solvent exchange for surface modification, and drying under normal pressure. The obtained SiO2 aerogel has properties similar to an aerogel material taking water glass as a silicon source; and the flyash and the kieselguhr are compounded to serve as a cheap silicon source and a normal pressure drying process is adopted, so that the production cost is greatly reduced, and the SiO2 aerogel has a wider application prospect in the fields such as building materials, thermal insulation, environment-friendly absorption and the like.
Description
Technical field
The present invention relates to a kind of by flyash and the compound preparation SiO of zeyssatite
2The method of aerogel material belongs to the functional materials preparation field.
Background technology
SiO
2Gas gel be a kind of be the novel amorphous solid-state material of dispersion medium by the nanometer scale particle accumulation and with the air, it has nanostructure, and (hole is 1～100nm, and skeleton particle is 1～20nm), low volume density (0.01～0.2g/cm
3), bigger serface (reaches as high as 800～1000m
2/ g), high porosity (can up to 80%～99.8%), lower thermal conductivity (single particle gas gel: 0.013～0.02W/mK under the normal temperature, pile up: 0.4W/m by aerogel particle
2K) etc. characteristics all have wide practical use in fields such as heat-insulation material, optics, acoustics, electricity, catalysis, pharmaceutical carrier, sorbing materials.Yet, because silica aerogel material thermal conductivity at high temperature sharply increases, largely limit its application at heat-insulation material, in addition because gas gel is the SiO by the nanometer scale size
2Particle packing forms, and porosity is big, so its intensity is very low, and fragility is bigger, has greatly limited its application in each field.The silicon source of existing preparation gas gel mainly contains: silicoorganic compound such as tetraethoxy, polyethoxye sily oxide, methyltrimethoxy silane, silicon tetrachloride; It is the silicon source that the present invention adopts cheap flyash and tripolite compound cooperation, greatly reduces the production cost of gas gel.
Summary of the invention
In order to overcome the shortcoming that existing aerogel material preparation cost is high, the production cycle is long, the present invention provides a kind of low cost to prepare the method for silica aerogel material.This preparing method's core content is being the silicon source with high-quality fly ash and tripolite compound cooperation, prepares SiO through series of process
2Aerogel material, this preparation technology's reaction conditions realize easily, and with short production cycle, cost is low, the SiO of gained
2Reaching existing on the gas gel fundamental property index is the prepared SiO in silicon source with service water glass
2The technical performance index of gas gel.
The compound SiO that makes of the present invention's flyash and zeyssatite
2The preparation technology of aerogel material has comprised that flyash and diatomite material mechanical activation are handled, SiO
2Colloidal sol preparation, wet gel preparation, aging, a step solvent exchange/surface-treated, six steps of constant pressure and dry.Said SiO
2Following technology has been adopted in the colloidal sol preparation:
A. be raw material with flyash and zeyssatite, mix according to the certain mass ratio after the for some time of activation at a certain temperature; Said temperature is 300～800 ℃, and the time is 10min～90min, and said specified proportion is meant mass ratio, flyash and zeyssatite quality than optimum value between 1: 2～3: 1.
B. press specified proportion at a certain temperature with certain density solution alkali hybrid reaction for some time, to react the back mixture carry out suction filtration, filtrating is diluted with certain proportion with zero(ppm) water, the mistake strongly acidic cation-exchange; Said temperature of reaction optimum value is 70～120 ℃, and alkali concn is between 5%～20%, and the reaction times, optimum value was between 0.5h～6h; Said filtrating and distilled water diluting ratio optimum value are between 1: 0.5～1: 5;
C. it is aging to treat that it immerses behind gel in the organic solvent solution under field conditions (factors); Gel after aging is immersed in a certain proportion of ethanol/trimethylchlorosilane/normal hexane mixing solutions; Make the solvent exchange surface-treated in a step, accomplish; At last the organogel after the modification is carried out drying for some time at normal temperatures and pressures, promptly get SiO
2Aerogel material.Ethanol and trimethylchlorosilane mol ratio ratio are between 1: 0.5～1: 3 in the said mixing solutions, and be 40 ℃～60 ℃ down dry 2～6h said time of drying, 80 ℃～150 ℃ down dry 1～3h.
Said alkali can be selected from: sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, sodium hydrogencarbonate, saleratus, ammoniacal liquor etc.
Said organic solvent can be selected from: methyl alcohol, ethanol, propyl alcohol, the trimethyl carbinol etc.
The compound aerogel material that makes of the present invention's flyash and zeyssatite is close for the gas gel performance of silicon source preparation with employing water glass; And production technique is simple, reduced production cost; Can be widely used in heat-insulation material, environmental protection sorbing material etc., all have been widely used in fields such as material of construction, aerospace, environment environmental protection.
Description of drawings
Fig. 1 is the SiO that the present invention's low-cost constant pressure and dry makes
2The photo of gas gel.
Fig. 2 is the SiO that the present invention's low-cost constant pressure and dry makes
2The process flow sheet of gas gel.
Embodiment
Be described in detail embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
Flyash 50g, activation 60min in 800 ℃ of retort furnaces; Zeyssatite 50g, roasting 3h in 600 ℃ of retort furnaces is in the NaOH solution of 10% concentration that joins 500mL after flyash mixes; 80 ℃ of following reaction 150min cross leaching filtrating, with zero(ppm) water with 1: 1 dilution proportion; Cross resin cation(R.C.), control pH is 2-3; To pH=5.5, the gained hydrogel wears out down at 30 ℃, carries out solvent exchange/surface-treated with ethanol, normal hexane, trimethylchlorosilane then with ammonia water titration; Ethanol and trimethylchlorosilane mol ratio are 2: 3, and trimethylchlorosilane and wet gel volume ratio are 1: 1, and the time is 24h.Be placed on dry 2h in 80 ℃ the baking oven again, 150 times dry 1h promptly make SiO
2Gas gel, its specific surface area are 531.7m
2/ g, density is 0.129g/cm
3, the internal capillary mean pore size is 25nm.
Embodiment 2
Flyash 70g, zeyssatite 50g, activation 70min in 700 ℃ of retort furnaces; Zeyssatite 50g, roasting 4h in 500 ℃ of retort furnaces crosses 200 mesh sieves, in the NaOH solution of 15% concentration that joins 500mL after flyash mixes; 90 ℃ of following reaction 120min cross leaching filtrating, with zero(ppm) water with 1: 2 dilution proportion; Cross resin cation(R.C.), control pH is 2-3; To pH=6.0, the gained hydrogel wears out down at 30 ℃, carries out solvent exchange/surface-treated with ethanol, normal hexane, trimethylchlorosilane then with ammonia water titration; Ethanol and trimethylchlorosilane mol ratio are 1: 1, and trimethylchlorosilane and wet gel volume ratio are 1: 1.5, and the time is 48h.Be placed on dry 4h in 80 ℃ the baking oven again, 150 times dry 1h promptly make SiO
2Gas gel, its specific surface area are 548.4m
2/ g, density is 0.105g/cm
3, the internal capillary mean pore size is 18nm.
Claims (3)
1. flyash and the compound preparation SiO of zeyssatite
2The gas gel method is characterized in that,
A. be raw material with flyash and zeyssatite, after 300～800 ℃ of following activation, mix that the time is 10min～90min; Flyash and zeyssatite blended mass ratio are between 1: 2～3: 1;
B. in proportion 70～120 ℃ of following and alkaline solution hybrid reactions, carry out suction filtration, filtrating is diluted, cross strongly acidic cation-exchange with zero(ppm) water to reacting the back mixture; The concentration of alkaline solution is that the reaction times is between 0.5h～6h between 5%～20%; Said filtrating and distilled water diluting ratio are between 1: 0.5～1: 5;
C. it is aging to treat that it immerses behind gel in the organic solvent solution under field conditions (factors); Gel after aging is immersed in ethanol/trimethylchlorosilane/normal hexane mixing solutions; Make the solvent exchange surface-treated in a step, accomplish; At last the organogel after the modification is carried out drying for some time at normal temperatures and pressures, promptly get SiO
2Aerogel material; Ethanol and trimethylchlorosilane mol ratio are between 1: 0.5～1: 3 in the mixing solutions; Be 40 ℃～60 ℃ down dry 2～6h time of drying, 80 ℃～150 ℃ down dry 1～3h.
2. a kind of flyash according to claim 1 and the compound preparation SiO2 of zeyssatite gas gel method is characterized in that said alkali is selected from sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, sodium hydrogencarbonate, saleratus, ammoniacal liquor.
3. a kind of flyash according to claim 1 and the compound preparation SiO2 of zeyssatite gas gel method is characterized in that said organic solvent is selected from methyl alcohol, ethanol, propyl alcohol, the trimethyl carbinol.
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| CN2011104457845A CN102515182A (en) | 2011-12-28 | 2011-12-28 | Method for preparing SiO2 aerogel by compounding flyash and kieselguhr |
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| CN2011104457845A CN102515182A (en) | 2011-12-28 | 2011-12-28 | Method for preparing SiO2 aerogel by compounding flyash and kieselguhr |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818912A (en) * | 2014-01-21 | 2014-05-28 | 合肥科斯孚安全科技有限公司 | Method for preparing silicon dioxide aerogel with low density and large specific surface area at ordinary pressure |
| CN103977749A (en) * | 2014-06-05 | 2014-08-13 | 武汉理工大学 | Method for preparing amorphous SiO2-Al2O3 aerogel by taking metakaolin as raw material |
| CN104961135A (en) * | 2015-07-01 | 2015-10-07 | 卓达新材料科技集团有限公司 | Preparation method of silicon dioxide aerogel |
| CN105418052A (en) * | 2015-11-09 | 2016-03-23 | 大连理工大学 | Preparation technology of carbon nanofiber composite silicon dioxide aerogel |
| CN107057406A (en) * | 2017-05-17 | 2017-08-18 | 锦洋高新材料股份有限公司 | A kind of functional modification white carbon and preparation method thereof |
| CN109078588A (en) * | 2018-09-11 | 2018-12-25 | 淮阴工学院 | Recessed native composite aerogel of extremely-low density sodium alginate-and preparation method thereof |
| CN109265131A (en) * | 2018-11-12 | 2019-01-25 | 中研信源（北京）节能科技有限公司 | A kind of preparation method of aerogel vacuum thermal insulation plate and its core material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244825A (en) * | 2008-03-20 | 2008-08-20 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for producing silicon dioxide silica aerogel with tripolite as raw material |
| CN101538046A (en) * | 2009-03-10 | 2009-09-23 | 大连工业大学 | Method for simultaneously preparing SiO2 aerogel and zeolite by utilizing fly ash |
-
2011
- 2011-12-28 CN CN2011104457845A patent/CN102515182A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244825A (en) * | 2008-03-20 | 2008-08-20 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for producing silicon dioxide silica aerogel with tripolite as raw material |
| CN101538046A (en) * | 2009-03-10 | 2009-09-23 | 大连工业大学 | Method for simultaneously preparing SiO2 aerogel and zeolite by utilizing fly ash |
Non-Patent Citations (1)
| Title |
|---|
| 王宝民等: "硅藻土资源的综合利用研究", 《材料导报》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818912A (en) * | 2014-01-21 | 2014-05-28 | 合肥科斯孚安全科技有限公司 | Method for preparing silicon dioxide aerogel with low density and large specific surface area at ordinary pressure |
| CN103818912B (en) * | 2014-01-21 | 2015-10-21 | 合肥科斯孚安全科技有限公司 | A kind of normal pressure prepares the method for low density bigger serface aerosil |
| CN103977749A (en) * | 2014-06-05 | 2014-08-13 | 武汉理工大学 | Method for preparing amorphous SiO2-Al2O3 aerogel by taking metakaolin as raw material |
| CN104961135A (en) * | 2015-07-01 | 2015-10-07 | 卓达新材料科技集团有限公司 | Preparation method of silicon dioxide aerogel |
| CN105418052A (en) * | 2015-11-09 | 2016-03-23 | 大连理工大学 | Preparation technology of carbon nanofiber composite silicon dioxide aerogel |
| CN105418052B (en) * | 2015-11-09 | 2018-08-28 | 大连理工大学 | A kind of preparation process of carbon nano-fiber combined oxidation silica aerogel |
| CN107057406A (en) * | 2017-05-17 | 2017-08-18 | 锦洋高新材料股份有限公司 | A kind of functional modification white carbon and preparation method thereof |
| CN109078588A (en) * | 2018-09-11 | 2018-12-25 | 淮阴工学院 | Recessed native composite aerogel of extremely-low density sodium alginate-and preparation method thereof |
| CN109265131A (en) * | 2018-11-12 | 2019-01-25 | 中研信源（北京）节能科技有限公司 | A kind of preparation method of aerogel vacuum thermal insulation plate and its core material |
| CN109265131B (en) * | 2018-11-12 | 2021-06-15 | 王贵然 | Aerogel vacuum insulation panel and preparation method of core material thereof |
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Application publication date: 20120627 |