CN106430219A - Method for preparing silicon oxide aerogel with low cost - Google Patents
Method for preparing silicon oxide aerogel with low cost Download PDFInfo
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- CN106430219A CN106430219A CN201510343509.0A CN201510343509A CN106430219A CN 106430219 A CN106430219 A CN 106430219A CN 201510343509 A CN201510343509 A CN 201510343509A CN 106430219 A CN106430219 A CN 106430219A
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Abstract
The invention relates to a method for preparing silicon oxide aerogel with low cost. Cheap industrial water glass is adopted as a precursor, water is adopted as a reactive solvent, oxalic acid is adopted as an acid catalyst, and the high-temperature-resistant blocky silicon oxide aerogel with excellent performance is prepared through a normal-pressure drying process. The prepared aerogel sample is low in density, high in specific area and good in temperature resistance, and the hydrophobic temperature resistance in air can reach 400 DEG C. The method has the advantages of being simple in preparation process and low in cost, the application range of the aerogel is widened through excellent high-temperature stability of the prepared aerogel, and the aerogel can be widely applied to the field of heat insulation.
Description
Technical field
The invention belongs to inorganic nano porous material preparing technical field, it is related to a kind of method that low cost prepares silica aerogel.
Background technology
Aeroge is mutually to be coalesced by colloidal particle or high-polymer molecular to constitute nanoporous network structure, and is full of a kind of high dispersive solid-state material of gaseous state disperse medium in hole.This material specific surface area with spongy open-celled structure greatly, and can control the structure of material, thus making it have many unique performances on the micro-scale of nanometer scale.The unique architectural characteristic of aeroge makes aeroge have unusual performance at aspects such as calorifics, electricity, acoustics, optics.
SiO2The preparation of aeroge is usually used supercritical and is dried, and molding effect preferably, can keep nanoporous network structure well.But, the instrument price that supercritical drying needs is expensive, there is High Temperature High Pressure danger higher.Therefore, SiO is prepared using constant pressure and dry2Aeroge is the inevitable requirement accomplished scale production and apply.At present, the silicon source that synthetic silica aeroge is adopted has positive silicate class, multi-polysiloxane, Ludox, waterglass and rice husk or flyash.Expensive, high cost, strong toxicity are haveed such problems as silicon source using positive silicate class, multi-polysiloxane, although rice husk or flyash are cheap, complicated process of preparation, the poor-performing of prepared aeroge.
Patent CN1126591C（ZL97181105.9）The method disclosing organically-modified aeroge, it removes the method for salinity in waterglass is, first in the presence of acid-exchange resin, mineral acid or hydrochloric acid, water glass solution to be adjusted to pH<3, obtain gel by adding base catalyst in silicic acid, be then washed with deionized gel, with the wherein all of electrolyte that dissociates.Chinese patent CN201210121968.0, CN201210114691.9 are with sodium silicate as raw material, using the preparation of collosol and gel two-step method, through ion exchange, ethanol solution with tetraethyl orthosilicate is aging, aeroge is obtained through solvent exchange and modification, constant pressure and dry after, using tetraethyl orthosilicate considerably increase preparation cost, the aeroge density obtaining is also bigger than normal.Ni Xingyuan etc.（Chinese patent, application number 200810042222.4）Disclosing using straw ash is raw material, and by solvent displacement, surface modification, the method preparing hydrophobic type silica aerogel at ambient pressure, but technique is more complicated.Most of technique is all desalination by way of cation exchange at present, but removes the metal ions such as the sodium ion in waterglass using storng-acid cation exchange resin.Due to cation exchange resin finite capacity（Generally 5mmol/g）, still, if industrialized production, the sodium at high concentration ion in waterglass can lead to the rapid saturation of ion exchange resin exchange capacity to this method experiment rank, cannot continuously produce at all.There are many researchs reports preparing silica aerogel with regard to constant pressure and dry at present, but all there is certain defect, such as high cost, complex process, and the aeroge specific surface area of preparation is less than normal, heat resistance is poor, thus constrain the commercial Application of aeroge.Therefore, urgent needss research preparation process is simple, silica aerogel with low cost.
Content of the invention
The present invention is directed to the problems referred to above of prior art, provides a kind of method that low cost prepares silica aerogel.
To achieve the above object of the invention, the technical solution used in the present invention is：A kind of method that low cost prepares silica aerogel, is obtained in the steps below：
Step one：Industrial waterglass is added deionized water dilution to obtain water glass solution, supersound process certain time after filtration；
Step 2：Take the water glass solution of certain volume, be added thereto to a certain amount of dry chemistry controlling agent, after stirring 2 ~ 10min, add finite concentration oxalic acid and treat its gel；
Step 3：Wet gel is placed at a certain temperature in organic reagent aging a period of time；
Step 4：After aging, wet gel is placed in displacement in non-polar solven；
Step 5：Wet gel after displacement is placed in the mixed liquor that siloxane solvent is with non-polar solven and carries out surface modification；
Step 6：By the wet gel after modification in step 5, after non-polar solven washing, constant pressure and dry can get transparent cake silica aerogel.
Silicon source described in step one is preferably 1 with the ratio of the volume of deionized water:2~1:10, the modulus of described silicon source is 3 ~ 3.5 industrial waterglass, and sonication treatment time is 0 ~ 10min.
In step 2, waterglass volume is 10 ~ 50ml, and dry chemistry controlling agent is one of Methanamide, DMF, Polyethylene Glycol, glycerol, oxalic acid, and it is 0 ~ 1 with the mol ratio of Si:1, the concentration of oxalic acid is 0 ~ 2mol/L.
In step 3, organic solvent is one of methanol, ethanol, isopropanol, butanol, and aging temperature is 30 ~ 70 DEG C, and the time is 0 ~ 5d.
Non-polar solven described in step 4 is preferably one of normal hexane, hexamethylene, normal heptane.
Siloxane solvent described in step 5 is preferably one of trim,ethylchlorosilane, hexamethyldisiloxane, hexamethyldisiloxane, APTES, silane coupler is 0.05 ~ 0.5 with the ratio of the volume of wet gel, and described non-polar solven is preferably one of normal hexane, hexamethylene, normal heptane.
Non-polar solven described in step 6 is preferably one of normal hexane, hexamethylene, normal heptane, and constant pressure and dry temperature is 30 ~ 200 DEG C, and drying time is 5 ~ 15h.
The invention discloses a kind of method that low cost prepares silica aerogel, with cheap industrial waterglass as silicon source, add oxalic acid, single step reaction, be prepared for low-density silicon oxide aerogel through constant pressure and dry.In described silica aerogel, prepare silica aerogel using supersound process and interpolation dry chemistry controlling agent through constant pressure and dry, sample has the features such as density is low, pore structure is uniform, and hydrophobic temperature tolerance reaches 400 DEG C.
Brief description：
The photomacrograph of the silica aerogel that accompanying drawing 1 is prepared for the present invention.
Specific embodiment
Embodiment 1
According to industrial waterglass and water by volume 1：4 measure the industrial waterglass that 20ml modulus is 3.2,80ml deionized water mixes in beaker, stirring 10min, it is then passed through supersound process 5min after filter, add 0.47ml glycerol in solution, stirring 3min, add the 1mol/L oxalic acid solution of 8.4ml, stir 1min, treat its complete gel, add deionized water, then it is placed on aging two days in 40 DEG C of water-baths, then through ethanol replacement one day, then wet gel is placed in displacement in normal hexane, wet gel is placed in trim,ethylchlorosilane and the mixed liquor of normal hexane and is modified, under 40 DEG C of water-baths, carry out 10h.Completely gel integrally swims on modified liquid product for modification, then replaces 24h through normal hexane again, after through 40 DEG C, 60 DEG C, 80 DEG C, what 100 DEG C of each two hours were dried obtains aeroge sample.
Obtained aeroge sample rate is 0.068g/cm3, specific surface area is 699.8m2/g.
Embodiment 2
According to industrial waterglass and water by volume 1：4 measure the industrial waterglass that 20ml modulus is 3.2,80ml deionized water mixes in beaker, stirring 10min, it is then passed through supersound process 10min after filter, add 0.47ml glycerol in solution, stirring 3min, add the 1mol/L oxalic acid solution of 8.7ml, stir 1min, treat its complete gel, add deionized water, then it is placed on aging two days in 40 DEG C of water-baths, then through ethanol replacement one day, then wet gel is placed in displacement in normal hexane, wet gel is placed in trim,ethylchlorosilane and the mixed liquor of normal hexane and is modified, under 40 DEG C of water-baths, carry out 10h.Completely gel integrally swims on modified liquid product for modification, then replaces 24h through normal hexane again, after through 40 DEG C, 60 DEG C, 80 DEG C, what 100 DEG C of each two hours were dried obtains aeroge sample.
Obtained aeroge sample rate is 0.070g/cm3, specific surface area is 607.7m2/g.
Below presently preferred embodiments of the present invention is illustrated, but the present invention is not limited to described embodiment, those of ordinary skill in the art also can make a variety of equivalent modifications or replacement without prejudice on the premise of present invention spirit, and these equivalent modifications or replacement are all contained in the application claim limited range.
Claims (7)
1. a kind of low cost prepares the method for silica aerogel it is characterised in that being prepared in the steps below：
Step one：Industrial waterglass is added deionized water dilution to obtain water glass solution, supersound process certain time after filtration；
Step 2：Take above-mentioned water glass solution, be added thereto to a certain amount of dry chemistry controlling agent, after stirring 2 ~ 10min, add finite concentration oxalic acid and treat its gel；
Step 3：Wet gel is placed at a certain temperature in organic reagent aging a period of time；
Step 4：After aging, wet gel is placed in displacement in non-polar solven；
Step 5：Wet gel after displacement is placed in the mixed liquor that siloxane solvent is with non-polar solven and carries out surface modification；
Step 6：By the wet gel after modification in step 5 after non-polar solven washing, constant pressure and dry can get transparent cake silica aerogel.
2. low cost according to claim 1 prepare silica aerogel method it is characterised in that in described step one silicon source and the ratio of the volume of deionized water be preferably 1:2~1:10, the modulus of described silicon source is 3 ~ 3.5 industrial waterglass, and sonication treatment time is 0 ~ 10min.
3. the method that low cost according to claim 1 prepares silica aerogel, it is characterized in that, in described step 2, water glass solution volume is 5 ~ 30ml, dry chemistry controlling agent is Methanamide, N, one of dinethylformamide, Polyethylene Glycol, glycerol, oxalic acid, it is 0 ~ 1 with the mol ratio of Si:1, the concentration of oxalic acid is 0 ~ 2mol/L.
4. low cost according to claim 1 prepare silica aerogel method it is characterised in that in described step 3 organic solvent be one of methanol, ethanol, isopropanol, butanol, aging temperature be 30 ~ 70 DEG C, the time be 0 ~ 5d.
5. low cost according to claim 1 prepares the method for silica aerogel it is characterised in that non-polar solven described in described step 4 is preferably one of normal hexane, hexamethylene, normal heptane.
6. the method that low cost according to claim 1 prepares silica aerogel, it is characterized in that, siloxane solvent described in described step 5 is preferably one of trim,ethylchlorosilane, hexamethyldisiloxane, hexamethyldisiloxane, APTES, silane coupler is 0.05 ~ 0.5 with the ratio of the volume of wet gel, and described non-polar solven is preferably one of normal hexane, hexamethylene, normal heptane.
7. low cost according to claim 1 prepare silica aerogel method it is characterised in that in described step 6 non-polar solven be preferably one of normal hexane, hexamethylene, normal heptane, constant pressure and dry temperature be 30 ~ 200 DEG C, drying time be 5 ~ 15h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188524A (en) * | 2017-06-20 | 2017-09-22 | 中国科学技术大学 | One-step method constant pressure and dry quickly prepares TiO2The method of doping silicon dioxide aerogel powder |
| CN108440016A (en) * | 2018-04-02 | 2018-08-24 | 宿州市鸿宝联节能材料有限公司 | A kind of preparation method of the ultralight high-strength foaming insulation board of cement base |
| CN109762370A (en) * | 2019-03-01 | 2019-05-17 | 确成硅化学股份有限公司 | A kind of preparation method of amino modified silica |
| CN109762414A (en) * | 2018-12-25 | 2019-05-17 | 广东青龙建筑工程有限公司 | Based on the modified heat retaining and insulated waterproof coating and preparation method thereof of aerosil |
| CN109988396A (en) * | 2017-12-31 | 2019-07-09 | 江苏傲伦达科技实业股份有限公司 | A kind of SiO2Aeroge/Bisphenol-s Epoxy Resin heat-insulation composite material preparation method |
| CN113833140A (en) * | 2021-10-20 | 2021-12-24 | 西安工程大学 | Three-phase composite structure heat insulation material and preparation method and application thereof |
| CN114835127A (en) * | 2021-12-08 | 2022-08-02 | 山东工业陶瓷研究设计院有限公司 | Preparation method of hydrophilic aerogel |
| CN115432710A (en) * | 2022-09-16 | 2022-12-06 | 西安科技大学 | Preparation method of ultra-low density silicon dioxide aerogel block |
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| CN102179230A (en) * | 2011-04-01 | 2011-09-14 | 中国科学院生态环境研究中心 | Preparation method of magnetized silicon dioxide aerogel |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188524A (en) * | 2017-06-20 | 2017-09-22 | 中国科学技术大学 | One-step method constant pressure and dry quickly prepares TiO2The method of doping silicon dioxide aerogel powder |
| CN109988396A (en) * | 2017-12-31 | 2019-07-09 | 江苏傲伦达科技实业股份有限公司 | A kind of SiO2Aeroge/Bisphenol-s Epoxy Resin heat-insulation composite material preparation method |
| CN108440016A (en) * | 2018-04-02 | 2018-08-24 | 宿州市鸿宝联节能材料有限公司 | A kind of preparation method of the ultralight high-strength foaming insulation board of cement base |
| CN109762414A (en) * | 2018-12-25 | 2019-05-17 | 广东青龙建筑工程有限公司 | Based on the modified heat retaining and insulated waterproof coating and preparation method thereof of aerosil |
| CN109762370A (en) * | 2019-03-01 | 2019-05-17 | 确成硅化学股份有限公司 | A kind of preparation method of amino modified silica |
| CN113833140A (en) * | 2021-10-20 | 2021-12-24 | 西安工程大学 | Three-phase composite structure heat insulation material and preparation method and application thereof |
| CN113833140B (en) * | 2021-10-20 | 2023-08-25 | 西安工程大学 | Three-phase composite structure heat insulation material and preparation method and application thereof |
| CN114835127A (en) * | 2021-12-08 | 2022-08-02 | 山东工业陶瓷研究设计院有限公司 | Preparation method of hydrophilic aerogel |
| CN115432710A (en) * | 2022-09-16 | 2022-12-06 | 西安科技大学 | Preparation method of ultra-low density silicon dioxide aerogel block |
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Application publication date: 20170222 |