CN105236419A - Preparation method for corrosion-free SiO2 aerogel - Google Patents
Preparation method for corrosion-free SiO2 aerogel Download PDFInfo
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- CN105236419A CN105236419A CN201510343705.8A CN201510343705A CN105236419A CN 105236419 A CN105236419 A CN 105236419A CN 201510343705 A CN201510343705 A CN 201510343705A CN 105236419 A CN105236419 A CN 105236419A
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Abstract
The invention relates to a preparation method for corrosion-free SiO2 aerogel. The preparation method for the corrosion-free SiO2 aerogel adopts a sol-gel two-step method and comprises the steps of enabling a mixed solution of industrial water glass and deionized water to be subjected to exchange with weakly acidic cation exchange resin so as to remove Na<+> and obtain sol with the pH of 3.0-4.0, standing the sol, then, adjusting the pH value of the sol with ammonia water so as to obtain wet gel, then, aging the wet gel in an aging solution of ethyl orthosilicate and ethanol, putting the aged wet gel in ethanol for solvent replacement, then, putting the wet gel subjected to solvent replacement in a mixed solution of hexamethyldisilazane and ethanol for surface modification, then, putting the modified wet gel in ethanol for second-time solvent replacement, and finally, putting the wet gel in a carbon-dioxide supercritical drying kettle for supercritical drying, thereby preparing the SiO2 aerogel which has the advantages of no corrosion, excellent product performance and low process cost.
Description
Technical field
The present invention relates to SiO
2the preparation field of aerogel, is specifically related to a kind of corrosion-free SiO
2the preparation method of aerogel.
Technical background
Aerogel is current the lightest known solid in the world, and its porosity can up to 99.8%, and bore hole size is at 1 ~ 100nm, and specific surface area can up to 1590m
2/ g, volume density can at 3 ~ 500kg/m
3between change, being a kind of hi-tech, environmental protection, energy-efficient lagging material, minimumly under its thermal conductivity normal temperature and pressure reaching 0.010W/ (mK), is the one that thermal conductivity is minimum in known solid-state material at present.Due to unique texture and the performance of aerogel, this material is expected there is huge application prospect in field widely at Aeronautics and Astronautics, industrial energy saving, building energy conservation and sound insulation, damping, explosion-proof, environmental protection, energy storage etc.
SiO
2aerogel is studied the earliest, is also the aerogel material of current most application prospect.Its preparation is usual is raw material with organosilicon, and through supercritical process, is air by the solvent replacing in gel.Organosilicon source with high costs, therefore at present the general cheap water glass etc. of adopting for preparing aerogel in silicon source.
Shaoxing Nanuo Technology Co., Ltd. patent CN101318659A(2008), be silicon source with water glass, prepare the plural gel of colloidal sol and quartz wool sheet, use the water of 50 times of volumes to clean 120 hours, the Na in removing wet gel
+, adopt hydrochloric acid as acid catalyst, prepare SiO
2aerogel fiberboard.
Tokuyama Corp patent CN103118979A(2011), adopt the Na in highly acid Zeo-karb removal water glass
+, and adopt hydrochloric acid, sulfuric acid to carry out activating and regenerating to Zeo-karb, obtained a kind of SiO
2aerogel particle.
Shaanxi obtains wave material Science and Technology Ltd. patent CN102642841A(2012), water glass diluent is removed Na through storng-acid cation exchange resin
+, the HCl adjust ph re-using 1mol/L, to 1 ~ 2, does not wash with water and directly carries out solvent exchange, and obtained thermal conductivity is the SiO of 0.020 ~ 0.021W/ (mK)
2aerogel.
Zhejiang University patent CN103755152A(2013), water glass solution is filtered through Zeo-karb, is soaked in the mixed solution of hexamethyldisiloxane and hydrochloric acid during hydrophobically modified, add sulfuric acid as catalyzer, obtained SiO
2aerogel.
University Of Tianjin patent CN104478394A(2014), take water glass as silicon source, hydrofluoric acid is the alkylating reagent such as catalyzer, trimethylchlorosilane is hydrophobic modifier, by glass fibre and SiO
2aerogel compound has prepared SiO
2aerogel warming plate.
Nanuo Technology Co., Ltd. patent CN104556063A(2015), after organosilicate, inorganic silicate and water being mixed in proportion, regulate pH to make its gel with hydrochloric acid, sulfuric acid etc.Gel is washed 1 ~ 24h in the tap water of 20 ~ 90 DEG C, then hydrogel is proceeded to immersion 1 ~ 24h in water phase surfactant mixture, drying technique obtains aerogel.
As can be seen from these patent reports, at present in the preparation process of aerogel, have multiple step can introduce corrosive ion in the finished product:
One is the use of catalyzer.In existing technology, usually can add hydrofluoric acid, hydrochloric acid or sulfuric acid etc. as acid catalyst, this can introduce corrosive F wherein
-, Cl
-or SO
4 2-.
Two is the process to silicon source impurity.Treatment process mainly contains washing and resin cation exchange two kinds.In water washing treatment method, need in solution, add acid for adjusting pH value and make its gel, corrosive ion can be introduced from acid catalyst; In Zeo-karb treatment process, what above document all adopted is strong-acid ion exchange resin, and strong-acid ion exchange resin must adopt the strong acid such as hydrochloric acid or sulfuric acid to activate, and just can reuse.At this moment also Cl can be introduced
-or SO
4 2-deng the acid ion of severe corrosive.
Three is the modification stages at wet gel, and conventional art adopts trimethylchlorosilane to carry out hydrophobically modified to it usually, and this also can introduce corrosive Cl wherein
-.
At building field, Cl
-or SO
4 2-concrete can be destroyed Deng severe corrosive acid ion and accelerate steel bar corrosion, China's correlation standard, Cl in cement
-≤ 0.06%, Cl in concrete
-≤ 0.2%; Thermal insulation material field is used, the leachable Cl of standard regulation thermal insulation material at industrial pipeline
-+ F
-≤ 0.001%.Therefore, at SiO
2in aerogel preparation technology, if not to F
-, Cl
-or SO
4 2-controlled Deng severe corrosive acid ion, the application of aerogel in above-mentioned field will be restricted.
Summary of the invention
Contain the technical problem of caustic acid radical ion for aerosil in prior art, the object of this invention is to provide a kind of low cost, corrosion-free to metal, can the preparation method of aerosil of suitability for industrialized production.With cheap water glass for silicon source, mating surface modification, supercritical drying process, the good and non-corrosive aerosil of preparation thermal and insulating performance.
The invention provides a kind of preparation method of corrosion-free aerosil, its technical scheme is as follows:
(1) ion exchange resin activation
Select weakly acidic cation-exchange resin or phosphate Zeo-karb, after resin is soaked 12 ~ 24h with deionized water, wash to resin clarification, then use the phosphoric acid solution of 5% ~ 15% concentration to wash; After deionized water wash to neutrality, wash with the NaOH of 5% ~ 15% concentration, remove organic impurity; After deionized water wash to neutrality, with the phosphoric acid washing of 5% ~ 15% concentration, again stand-by to neutrality with deionized water wash.
(2) two-step approach collosol and gel
Industrial waterglass and deionized water are mixed, the Zeo-karb after activated exchanges removing Na
+, obtain the colloidal sol of pH=3.0 ~ 4.0, leave standstill 5 ~ 15h.Then with ammoniacal liquor, pH value is adjusted to 6.0 ~ 7.0, leaves standstill, obtain wet gel.
(3) aging and solvent exchange
Be aged at room temperature 6 ~ 48h in the tetraethoxy alcoholic solution of 5% ~ 50% by wet gel in equal-volume, concentration after gel, then use isopyknic ethanol to carry out solvent exchange 1 ~ 6 time, each 1 ~ 12h.
(4) surface modification and secondary solvent displacement
Use equal-volume, concentration are that the ethanolic soln of the hexamethyldisilazane of 5% ~ 20% carries out hydrophobically modified 6 ~ 48h, reuse isopyknic ethanol afterwards and carry out solvent exchange 1 ~ 3 time, each 1 ~ 12h.
(5) dry
CO is carried out according to certain condition
2supercritical drying, namely obtains corrosion-free aerosil.
The advantage that the present invention has relative to prior art and beneficial effect:
1, with the industrial-grade sodium silicate of cheapness for silicon source, in conjunction with CO
2supercritical drying prepares aerosil, and product quality is high, preparation technology is simple, is easy to realize industrialization;
2, adopt the sodium ion in weakly acidic cation-exchange resin removal silicon source, both efficiently, turn avoid and use acid catalyst to introduce caustic acid radical ion.Adopt phosphoric acid to activate weakly acidic cation-exchange resin, residual phosphate anion, not only to metal non-corrosiveness, also has etch-proof function simultaneously.
3, the hydrophobic modifier used can not introduce corrosive ion.Therefore, the present invention both ensure that the security of product, expanded again the Application Areas of aerosil.
Embodiment
Embodiment 1
According to the ratio of volume ratio 1:5, industrial waterglass and deionized water are mixed, exchange removing Na through carboxylic acid group's Zeo-karb
+, obtain the colloidal sol of pH=3.0, leave standstill 5h.Then with ammoniacal liquor, pH value is adjusted to 6.0, obtains wet gel.Wet gel is placed in the aging 24h of Ageing solution of tetraethoxy and ethanol mixing, the volume ratio of wet gel and Ageing solution is 1:1, and tetraethoxy and the ethanol mass ratio in mixed solution is 1:4.Wet gel after aging is placed in ethanol solvent exchange 3 times, each 12h, and the volume ratio of wet gel and ethanol is 1:1.Wet gel after solvent exchange is placed in the mixed solution hydrophobically modified 24h of hexamethyldisilazane and ethanol, the volume ratio of wet gel and modification liquid is 1:1, and hexamethyldisilazane and the ethanol mass ratio in mixed solution is 1:9.Wet gel after finishing is placed in CO 2 supercritical drying kettle, supercritical drying 4.5h, obtained corrosion-free aerosil.
Obtained aerosil density is 0.050g/cm
3, thermal conductivity is 0.023W/ (mK), detects according to GB/T17393: leach liquor pH=8.6, ω (F
-)=0.0015%, ω (Cl
-)=0.0040%, ω (Na
+)=0.4%, ω (SiO
3 2-)=1.4%, result of determination is non-corrosiveness.
Embodiment 2
According to the ratio of volume ratio 1:10, industrial waterglass and deionized water are mixed, exchange removing Na through phosphate Zeo-karb
+, obtain the colloidal sol of pH=3.5, leave standstill 10h.Then with ammoniacal liquor, pH value is adjusted to 6.5, obtains wet gel.Wet gel is placed in the aging 24h of Ageing solution of tetraethoxy and ethanol mixing, the volume ratio of wet gel and Ageing solution is 1:1, and tetraethoxy and the ethanol mass ratio in mixed solution is 1:4.Wet gel after aging is placed in ethanol solvent exchange 3 times, each 12h, and the volume ratio of wet gel and ethanol is 1:1.Wet gel after solvent exchange is placed in the mixed solution hydrophobically modified 24h of hexamethyldisilazane and ethanol, the volume ratio of wet gel and modification liquid is 1:1, and hexamethyldisilazane and the ethanol mass ratio in mixed solution is 1:5.Wet gel after finishing is placed in CO 2 supercritical drying kettle, supercritical drying 5h, obtained corrosion-free aerosil.
Obtained aerosil density is 0.045g/cm
3, thermal conductivity is 0.021W/ (mK), detects according to GB/T17393: leach liquor pH=9.0, ω (F
-)=0.0011%, ω (Cl
-)=0.0035%, ω (Na
+)=0.5%, ω (SiO
3 2-)=1.3%, result of determination is non-corrosiveness.
Embodiment 3
According to the ratio of volume ratio 1:20, industrial waterglass and deionized water are mixed, exchange removing Na through carboxylic acid group's Zeo-karb
+, obtain the colloidal sol of pH=4.0, leave standstill 15h.Then with ammoniacal liquor, pH value is adjusted to 7.0, obtains wet gel.Wet gel is placed in the aging 24h of Ageing solution of tetraethoxy and ethanol mixing, the volume ratio of wet gel and Ageing solution is 1:1, and tetraethoxy and the ethanol mass ratio in mixed solution is 1:4.Wet gel after aging is placed in ethanol solvent exchange 3 times, each 12h, and the volume ratio of wet gel and ethanol is 1:1.Wet gel after exchange of solvent is placed in the mixed solution hydrophobically modified 24h of hexamethyldisilazane and ethanol, the volume ratio of wet gel and modification liquid is 1:1, and hexamethyldisilazane and the ethanol mass ratio in mixed solution is 1:4.Wet gel after finishing is placed in CO 2 supercritical drying kettle, supercritical drying 6h, obtained corrosion-free aerosil.
Obtained aerosil density is 0.035g/cm
3, thermal conductivity is 0.020W/ (mK), detects according to GB/T17393: leach liquor pH=9.2, ω (F
-)=0.0012%, ω (Cl
-)=0.0039%, ω (Na
+)=0.2%, ω (SiO
3 2-)=1.2%, result of determination is non-corrosiveness.
Claims (7)
1. a corrosion-free SiO
2the preparation method of aerogel, is characterized in that comprising following step:
(1) adopt phosphoric acid to activate weakly acidic cation-exchange resin: to select weakly acidic cation-exchange resin, after resin is soaked 12 ~ 24h with deionized water, wash to resin clarification, then use the phosphoric acid solution of 5% ~ 15% concentration to wash; After deionized water wash to neutrality, wash with the NaOH of 5% ~ 15% concentration, remove organic impurity; After deionized water wash to neutrality, with the phosphoric acid washing of 5% ~ 15% concentration, again stand-by to neutrality with deionized water wash.
2.(2) sol-gel two-step approach: industrial waterglass and deionized water are mixed, exchanges removing Na through Zeo-karb
+, obtain the colloidal sol of pH=3.0 ~ 4.0, leave standstill 5 ~ 15h.
3. then with ammoniacal liquor, pH value is adjusted to 6.0 ~ 7.0, leaves standstill, obtain wet gel.
4.(3) aging and solvent exchange: be aged at room temperature 6 ~ 48h in the tetraethoxy alcoholic solution of 5% ~ 50% by wet gel in equal-volume, concentration after gel, then use isopyknic ethanol to carry out solvent exchange 1 ~ 6 time, each 1 ~ 12h.
5.(4) surface modification and secondary solvent displacement: use equal-volume, concentration are that the hydrophobic modifier such as the ethanolic soln of the hexamethyldisilazane of 5% ~ 20% carry out surface modification 6 ~ 48h, reuse isopyknic ethanol afterwards and carry out solvent exchange 1 ~ 3 time, each 1 ~ 12h.
6.(5) dry: to carry out CO according to certain condition
2supercritical drying, namely obtains corrosion-free aerosil.
7. according to the corrosion-free SiO of one according to claim 1
2the preparation method of aerogel, is characterized in that Zeo-karb is the weakly acidic cation-exchange resin such as carboxylic acid group's Zeo-karb, phosphate Zeo-karb, and the activated acids of Zeo-karb regeneration is phosphoric acid;
According to the corrosion-free SiO of one according to claim 1
2the preparation method of aerogel, is characterized in that surface-modifying agent is the surface hydrophobicity properties-correcting agent of the not chloride ion-containing such as hexamethyldisilazane, hexamethyldisiloxane;
According to the corrosion-free SiO of one according to claim 1
2the preparation method of aerogel, is characterized in that supercritical co drying process 3 ~ 12h time of drying.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688761A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Ambient pressure drying method for sodium metaaluminate modified resin purified sodium silicate aerogel |
| CN105727851A (en) * | 2016-01-29 | 2016-07-06 | 卓达新材料科技集团有限公司 | Supercritical drying method of silicon-aluminium composite aerogel |
| CN105776967A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Preparation method for fiber needled felt-enhanced sodium metaaluminate-modified aerogel |
| CN105776234A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Supercritical drying method of sodium metaaluminate modified resin purified water-glass aerogel |
| CN108002395A (en) * | 2017-12-07 | 2018-05-08 | 北京工业大学 | It is a kind of to reduce method of the aerosil drying process to equipment corrosion |
| CN108314411A (en) * | 2018-01-03 | 2018-07-24 | 深圳中凝科技有限公司 | The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine |
| CN109179431A (en) * | 2018-09-13 | 2019-01-11 | 安徽山河药用辅料股份有限公司 | A kind of preparation method of high bulk density silica |
| CN109351292A (en) * | 2018-10-22 | 2019-02-19 | 天津摩根坤德高新科技发展有限公司 | The preparation method and aeroge of sodium ion screener modified sodium silicate aeroge |
| CN111170497A (en) * | 2019-11-29 | 2020-05-19 | 南京大学 | Method for promoting Fenton oxidation efficiency by resin regulation and control |
| CN113401910A (en) * | 2021-07-30 | 2021-09-17 | 江苏泛亚微透科技股份有限公司 | Silicon dioxide aerogel and low-corrosion preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688761A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Ambient pressure drying method for sodium metaaluminate modified resin purified sodium silicate aerogel |
| CN105727851A (en) * | 2016-01-29 | 2016-07-06 | 卓达新材料科技集团有限公司 | Supercritical drying method of silicon-aluminium composite aerogel |
| CN105776967A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Preparation method for fiber needled felt-enhanced sodium metaaluminate-modified aerogel |
| CN105776234A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Supercritical drying method of sodium metaaluminate modified resin purified water-glass aerogel |
| CN108002395A (en) * | 2017-12-07 | 2018-05-08 | 北京工业大学 | It is a kind of to reduce method of the aerosil drying process to equipment corrosion |
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| CN108314411A (en) * | 2018-01-03 | 2018-07-24 | 深圳中凝科技有限公司 | The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine |
| CN109179431A (en) * | 2018-09-13 | 2019-01-11 | 安徽山河药用辅料股份有限公司 | A kind of preparation method of high bulk density silica |
| CN109351292A (en) * | 2018-10-22 | 2019-02-19 | 天津摩根坤德高新科技发展有限公司 | The preparation method and aeroge of sodium ion screener modified sodium silicate aeroge |
| CN111170497A (en) * | 2019-11-29 | 2020-05-19 | 南京大学 | Method for promoting Fenton oxidation efficiency by resin regulation and control |
| CN113401910A (en) * | 2021-07-30 | 2021-09-17 | 江苏泛亚微透科技股份有限公司 | Silicon dioxide aerogel and low-corrosion preparation method thereof |
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