CN1724353A - Process for preparing hydrophobic silicon dioxide aerogel using rice husk ash as raw material - Google Patents
Process for preparing hydrophobic silicon dioxide aerogel using rice husk ash as raw material Download PDFInfo
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- CN1724353A CN1724353A CN 200510012186 CN200510012186A CN1724353A CN 1724353 A CN1724353 A CN 1724353A CN 200510012186 CN200510012186 CN 200510012186 CN 200510012186 A CN200510012186 A CN 200510012186A CN 1724353 A CN1724353 A CN 1724353A
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- aerogel
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Abstract
A process for preparing the hydrophobic SiO2 aero-gel from rice husk ash includes such steps as burning rice husk to obtain its ash, extracting its hydro-gel in inorganic strong-alkaline aqueous solution, neutralizing by inorganic strong acid, laying aside to generate SiO2 hydro-gel, filter, acid treating, ageing, water washing, displacing the water from the hydro-gel by organic solvent, supercritical drying and modifying surface. Its advantages are high specific surface area and pore volume, and low apparent density.
Description
Technical field
With the rice hull ash is the method for feedstock production hydrophobic silicon dioxide aerogel, relates to the preparation method of hydrophobic silicon dioxide aerogel, belongs to chemical materials technology of preparing scope.
Background technology
Aerosil is a kind of porous amorphous solid-state material that includes a large amount of air, low density, high porosity, and its porosity rate can reach more than 90%, and typical bore hole size is in 1～100nm scope.Aerosil is at mechanics, acoustics, calorifics, many-sides such as optics all demonstrate unique character, they obviously are different from the porous material of pore space structure in micron and millimeter magnitude, and its very thin nanostructure makes that the thermal conductivity of material is extremely low, has great specific surface area, to light, the scattering of sound is all much smaller than traditional porous material.Therefore silica aerogel has broad application prospects, and can be used as transparent thermal insulation material, the refrigerator thermal insulation material, and the specific acoustic resistance coupling material can also be as the super capacitor material, new gas strainer, aspects such as new catalyst or support of the catalyst.But the wetting ability of aerogel has limited its utilization in some field, meets water or water vapour its structure is changed, and loses its original distinctive character.
The production method of existing hydrophobic silicon dioxide aerogel, in the domestic and international academic paper of publishing, its preparation mostly is to be raw material with four alkoxyl silicones, and the organosilicon of alkyl silicate and so on is done additive, adopts supercritical fluid technology to carry out exsiccant then.Be published in the article on Materials Research Bulletin 37 (2002) 1667-1677, A.Venkateswara Rao and Manish M.Kulkarni etc., do raw material with tetramethoxy-silicane, add trimethylethoxysilane simultaneously and carry out finishing, prepare the hydrophobicity aerogel thereby in supercritical methanol, carry out drying.
Be published in the article on Science and Technology of Advanced Materials 4 (2003) 509-515, A.Venkateswara Rao and Ravindra R.Kalesh etc., adopt tetraethoxysilane as raw material, additive has been selected multiple alkyl silicate such as methyltrimethoxy silane for use, Union carbide A-162, ethyl triethoxysilane etc. and chlorosilane such as dimethylchlorosilane etc., after the aerogel that supercritical drying is prepared all has certain hydrophobicity, wherein be that the sample hydrophobicity that goes out of additive preparation is best with the trimethylethoxysilane.
Be published in the article on Ceramics International 28 (2002) 43-50, P.B.Wagh and S.V.Ingale etc., adopt tetramethoxy-silicane to do raw material, add methyltrimethoxy silane simultaneously, behind supercritical drying, prepare the hydrophobicity aerogel as hydrophobic agents.
Comprehensive existing patented technology and bibliographical information, existing hydrophobic silicon dioxide aerogel production method adopts organosilicon to do raw material more, is aided with alkyl silicon simultaneously and does additive, and supercritical drying is produced product then.But all have the high problem of the expensive cost of raw material, this has directly influenced the large-scale production and the application of aerogel.
Previous Chinese patent (application number 03127920.1 the inventor, publication number CN1449997A) introduced the rice hull ash used after the burning of agricultural wastes rice husk in as the silicon source, method by sol-gel and supercritical drying production silica aerogel, though cost has largely reduced, still there is the wetting ability problem in the product of preparation.
The method that in another Chinese patent (application number 200510011378.2) of the inventor, proposes, also utilize rice hull ash as the silicon source, realized that drying is prepared aerosil under the condition of normal pressure, but still there is the wetting ability problem in the product of preparation, and compare with the product of supercritical drying preparation, exist pore volume little, the big and little problem in aperture of density.
Summary of the invention
The present invention utilizes rice hull ash as the silicon source, through the sol-gel stage, prepares the wetting ability aerosil behind the supercritical drying, and aerogel is carried out finishing, prepares hydrophobic silicon dioxide aerogel.From existing patented technology and bibliographical information, the same or analogous technology of making the feedstock production hydrophobic silicon dioxide aerogel of rice hull ash of Shang Weiyou and the present invention.
The objective of the invention is to propose is being the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, with rice hull ash through in the leaching of inorganic strong alkali solution, the inorganic acid and basic solution generates that silica hydrogel, hydrogel are aging, moisture, supercritical drying in the washing, organic solvent replacing water gel, aerogel is carried out finishing, prepare hydrophobic silicon dioxide aerogel, this method may further comprise the steps:
(1) preparation of the water-sol
Rice hull ash is added in the strong base solution that concentration is 0.1～1.0mol/L, and the volume of its alkaline solution and rice hull ash and mass ratio are 20～50 liters: 1 kilogram, the atmospheric boiling state leached 5～120 minutes down;
(2) filtration and acid treatment process
Is 5～9 with the leaching liquid filtrate filtered with the inorganic acid titration of the 0.1～1.0mol/L pH value that neutralizes, and preferably being titrated to pH value is 6～8, leaves standstill and makes silica hydrogel;
(3) aging
The hydrogel of preparation in above-mentioned (2) is worn out, and temperature is 15～60 ℃, and the time was at 1 minute to 48 hours;
(4) washing
With the hydrogel that obtains in the deionized water wash above-mentioned (3) 1～5 time; The volume ratio of deionized water and hydrogel is 1～5: 1;
(5) organic solvent displacement
With organic solvent the moisture in the hydrogel of above-mentioned (4) preparation is cemented out; Time swap is 1.5～6 hours, and the volume ratio of organic solvent and hydrogel is 1～3: 1;
(6) supercritical drying
The hydrogel that above-mentioned (5) are handled well adopts supercritical carbon dioxide fluid to carry out drying, obtains aerogel;
(7) finishing
The aerogel that above-mentioned (6) are made is put into the steam bath 1 minute to 96 hours of silicoorganic compound, temperature range is at 20 ℃～40 ℃, the quality amount ratio of silicoorganic compound and aerogel is 1: 20～1: 1, is preferably 1: 25～1: 3, just prepares the hydrophobicity aerogel after the taking-up.
Described strong base solution is the inorganic hydrogen aqueous solution of sodium oxide, or potassium hydroxide aqueous solution.
Used inorganic acid is hydrochloric acid or sulfuric acid.
Described organic solvent is the low-carbon (LC) monohydroxy-alcohol, as methyl alcohol, and ethanol; Or ketone, as acetone and butanone.
Described silicoorganic compound comprise: alkyl silicate, chemical molecular formula are R
4-nSi (OR)
n, R can be a methyl, ethyl or many carbon alkyl group, and n gets 1,2 or 3, as Trimethoxy silane, dimethyldimethoxysil,ne, trimethylammonium silicic acid methyl esters; Or nitrogenous silane, chemical molecular formula is (R
3Si)
2NH, R can be methyl, and ethyl or many carbon alkyl group are as hexamethyldisilazane etc.
Beneficial effect of the present invention:
1. replace expensive organosilicon to do raw material production nanostructure solid material aerosil with the waste material rice hull ash after the agriculture waste product rice husk burning, production cost is greatly reduced.
2. after the aerogel behind the supercritical drying carries out finishing, can prepare the hydrophobicity aerogel.Hydrophobicity is detected discovery, and the aerogel of this kind method preparation is planar water not substantially.Adopt the hydrophobic standard of commercial measurement---utilize methanol aqueous solution to measure hydrophobicity, the percentage composition of methyl alcohol shows hydrophobicity in the solution when promptly adopting aerogel to begin to sink, and percentage composition high hydrophobicity more is good more.Measuring result shows that this index of the aerogel that this kind method is prepared is 10%～45%.
3. the aerogel of preparing has high-specific surface area (200～800m through the n2 absorption apparatus measurement
2/ g), high pore volume (1.0 ~ 6.0cm
3/ g), (0.02 ~ 0.40g/cm3), the aperture of contained micropore is nano level (pore size distribution range 1 ~ 80nm, a mean pore size 20～50nm) to low bulk density.
4. technology is simple, easy to operate, is fit to large-scale production and application.
Embodiment
The present invention for a kind of be the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash.With the waste material rice hull ash after the rice husk burning, through in the leaching of the inorganic strong alkali aqueous solution, the inorganic acid and basic solution generates that silica hydrogel, hydrogel are aging, moisture, supercritical drying in the washing, organic solvent replacing water gel, aerogel is carried out finishing, prepare hydrophobic silicon dioxide aerogel; Its technological process is as follows:
(1) preparation of the water-sol: rice hull ash is added in the strong base solution that concentration is 0.1～1.0mol/L, and the ratio of its alkaline solution and rice hull ash is 20～50: 1 (L/kg), and the atmospheric boiling state leached 5～120 minutes down;
(2) filter and the acid treatment process: is 5～9 with the leaching liquid filtrate filtered with the inorganic acid titration of the 0.1～1.0mol/L pH value that neutralizes, and leaves standstill and makes silica hydrogel;
(3) aging, the hydrogel for preparing in above-mentioned (2) is worn out, temperature is between 15～60 ℃, and the time was at 1 minute to 48 hours;
(4) washing, with the gel that obtains in the deionized water wash above-mentioned (3) 1～5 time, the volume ratio of deionized water and gel is 1～5: 1;
(5) organic solvent displacement cements out the moisture in the hydrogel of above-mentioned (4) preparation with organic solvent, and time swap was at 1.5～6 hours, and the volume ratio of organic solvent and gel is 1～3: 1;
(6) supercritical drying, the gel that above-mentioned (5) are handled well adopts supercritical carbon dioxide fluid to carry out drying;
(7) steam bath 1 minute to 96 hours of silicoorganic compound is put in finishing, the aerogel that above-mentioned (6) are made, preferably between 1 hour to 72 hours; Temperature range is preferably 25 ℃～30 ℃ at 20 ℃～40 ℃; The quality amount ratio of silicoorganic compound and aerogel is 1: 20～1: 1, is preferably 1: 25～1: 3; Just prepare the hydrophobicity aerogel after the taking-up.
Described strong base solution is the inorganic hydrogen aqueous solution of sodium oxide, or potassium hydroxide aqueous solution.
Used inorganic acid is hydrochloric acid or sulfuric acid.
Described organic solvent is the low-carbon (LC) monohydroxy-alcohol, as methyl alcohol, and ethanol; Or ketone, as acetone and butanone.
Described silicoorganic compound are: alkyl silicate, chemical molecular formula are R
4-nSi (OR)
n, R can be a methyl, ethyl or many carbon alkyl group, and n gets 1,2 or 3, as Trimethoxy silane, dimethyldimethoxysil,ne, trimethylammonium silicic acid methyl esters; Or nitrogenous silane, chemical molecular formula is (R
3Si)
2NH, R can be methyl, and ethyl or many carbon alkyl group are as hexamethyldisilazane etc.
Lift following specific embodiment again and be used to illustrate the present invention.
Example 1
The NaOH solution of 10 gram rice hull ash and 300 milliliters of 0.9mol/L mix, and boiling is 90 minutes under normal pressure, and the filtrate that obtains after the filtration is 7 with the sulfuric acid of 1mol/L with its pH value that neutralizes; Leave standstill the formation hydrogel; The hydrogel of gained wore out 48 hours at 25 ℃, washed 3 times; Used the alcohol immersion hydrogel then 4 hours, the back adopts the method for supercritical drying to prepare the aerosil of white, puts it in the steam bath of hexamethyldisilazane 1 hour (30 ℃), just obtains hydrophobic aerosil after the taking-up.Hydrophobicity is measured, directly the aerogel for preparing is put into water, weigh after 10 days, find not have fully planar water; Method with methanol aqueous solution is measured hydrophobicity, and index can reach 40%.Its specific surface area is 460.7m
2/ g, pore volume are 3.3cm
3/ g, apparent density is 39.8kg/m
3, inner micropore mean pore size is 33 nanometers.
Example 2
The NaOH solution of 15 gram rice hull ash and 500 milliliters of 0.1mol/L mix, and boiling is 120 minutes under normal pressure, and the filtrate that obtains after the filtration is 8 with the hydrochloric acid of 1mol/L with its pH value that neutralizes; Leave standstill the formation hydrogel; The hydrogel of gained wore out 35 hours at 27 ℃, used deionized water wash afterwards 4 times; Soaked hydrogel 6 hours with methyl alcohol then, the back adopts supercritical carbon dioxide fluid to carry out drying, promptly make the aerosil of white, put it in the steam bath of dimethyldimethoxysil,ne, (26 ℃) just obtained hydrophobic aerosil in 12 hours.Hydrophobicity is measured, directly product is put on the water surface, weigh after 15 days and find not have fully planar water; Method with methanol aqueous solution is measured hydrophobicity, and index can reach 15%.Its specific surface area is 417.7m
2/ g, apparent density is 40.7kg/m
3, pore volume is 2.5cm
3/ g, inner micropore mean pore size is 29 nanometers.
Example 3
The KOH solution of 10g rice hull ash and 200 milliliters of 1mol/L mixes, and boiling is 90 minutes under normal pressure, and the filtrate that obtains after the filtration is 6.5 with the sulfuric acid of 1mol/L with its pH value that neutralizes; Leave standstill the formation hydrogel; The hydrogel of gained wore out 40 hours at 21 ℃, used deionized water wash afterwards 4 times; Use the alcohol immersion hydrogel then 6 hours, and behind supercritical drying, promptly made the aerosil of white, get its part and put into the steam bath of trimethylammonium methoxy silane (28 ℃), just obtain hydrophobic aerosil after 48 hours.Hydrophobicity is measured, directly product is put on the water surface, weigh after 15 days and find that weightening finish is 1%; Method with methanol aqueous solution is measured hydrophobicity, and index can reach 10%.Its specific surface area is 398.5m
2/ g, apparent density is 41.1kg/m
3, pore volume is 1.9cm
3/ g, inner micropore mean pore size is 25.5 nanometers.
Example 4
The NaOH solution of 15 gram rice hull ash and 500 milliliters of 0.1mol/L mix, and boiling is 100 minutes under normal pressure, and the filtrate that obtains after the filtration is 8 with the sulfuric acid of 1mol/L with its pH value that neutralizes; Leave standstill the formation hydrogel; The hydrogel of gained wore out 35 hours at 20 ℃, used deionized water wash afterwards 4 times; Used the alcohol immersion hydrogel then 6 hours, the back adopts supercritical carbon dioxide fluid to carry out drying, promptly make the aerosil of white, put it in the steam bath of methyltrimethoxy silane after 72 hours (25 ℃), just obtain hydrophobic aerosil.Hydrophobicity is measured, directly product is put on the water surface, weigh after 15 days and find that weightening finish is 15%; Method with methanol aqueous solution is measured hydrophobicity, and index can reach 15%.Its specific surface area is 298.1m
2/ g, apparent density is 45.2g/cm
3, pore volume is 1.5cm
3/ g, inner micropore mean pore size is 27.3 nanometers.
Claims (10)
1, be the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that this method may further comprise the steps:
(1) preparation of the water-sol
Rice hull ash is added in the strong base solution that concentration is 0.1～1.0mol/L, and the volume of its alkaline solution and rice hull ash and mass ratio are 20～50 liters: 1 kilogram, the atmospheric boiling state leached 5～120 minutes down;
(2) filtration and acid treatment process
Is 5～9 with the leaching liquid filtrate filtered with the inorganic acid titration of the 0.1～1.0mol/L pH value that neutralizes, and leaves standstill and makes silica hydrogel;
(3) aging
The hydrogel of preparation in above-mentioned (2) is worn out, and temperature is 15～60 ℃, and the time was at 1 minute to 48 hours;
(4) washing
With the hydrogel that obtains in the deionized water wash above-mentioned (3);
(5) organic solvent displacement
With organic solvent the moisture in the hydrogel of above-mentioned (4) preparation is cemented out;
(6) supercritical drying
The hydrogel that above-mentioned (5) are handled well adopts supercritical carbon dioxide fluid to carry out drying, obtains aerogel;
(7) finishing
The aerogel that above-mentioned (6) are made is put into the steam bath 1 minute to 96 hours of silicoorganic compound, and temperature range is at 20 ℃～40 ℃, and the quality amount ratio of silicoorganic compound and aerogel is 1: 20～1: 1, just prepares the hydrophobicity aerogel after the taking-up.
2, according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: during with inorganic acid titration filtrate, titration pH value is preferably 6～8.
3. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, and it is characterized in that: selected silicoorganic compound comprise: alkyl silicate, chemical molecular formula are R
4-nSi (OR)
n, R is a methyl, ethyl or many carbon alkyl group, and n gets 1,2 or 3; Or nitrogenous silane, chemical molecular formula is (R
3Si)
2NH, R can be methyl, ethyl or many carbon alkyl group.
4. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: during with the deionized water wash gel, washing times is 1～5 time.
5. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: during with the deionized water wash gel, the volume ratio of deionized water and gel is 1～5: 1.
6. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: during moisture in the organic solvent replacing water gel, time swap is 1.5～6 hours.
7. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: during moisture in the organic solvent replacing water gel, the volume ratio of organic solvent and gel is 1～3: 1.
8. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: the time priority that finishing is handled is between 1 hour 72 hours.
9. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: the temperature range that finishing is handled is preferentially at 25 ℃～30 ℃.
10. according to claim 1 is the method for feedstock production hydrophobic silicon dioxide aerogel with the rice hull ash, it is characterized in that: when finishing was handled, the quality amount ratio of silicoorganic compound and aerogel was preferably 1: 25～and 1: 3.
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