CN108017073A - A kind of method that magnesia aeroge is prepared using bischofite as raw material - Google Patents
A kind of method that magnesia aeroge is prepared using bischofite as raw material Download PDFInfo
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- CN108017073A CN108017073A CN201711448530.2A CN201711448530A CN108017073A CN 108017073 A CN108017073 A CN 108017073A CN 201711448530 A CN201711448530 A CN 201711448530A CN 108017073 A CN108017073 A CN 108017073A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The invention discloses a kind of method that magnesia aeroge is prepared using bischofite as raw material, preparation method includes as follows：1）Bischofite, distilled water, alcoholic solvent, water soluble polymer are mixed, 5 ~ 120min of stirring obtains clear solution, then epoxide is added to 5 ~ 60min of stirring in solution and obtains colloidal sol；2）Obtained colloidal sol is sealed and carries out gelation, gelling temperature is 20 ~ 95 DEG C, and gelation time is 2 ~ 20h, obtains magnesia wet gel；3）Obtained magnesia wet gel is subjected to washing by soaking with distilled water, for washing times no less than three times, distillation water consumption is no less than the volume of wet gel；4）By step 3）Wet gel after embathing is dried, and magnesia aeroge is prepared；The present invention efficiently solves existing utilization magnesium alkoxide and prepares magnesia wet gel, and there are magnesium alkoxide easily hydrolytie polycondensation, process is difficult to control；Magnesium alkoxide toxicity is big, expensive, and temperature, the humidity to environment are extremely sensitive, the problems such as not being easily-synthesized, preserve.
Description
Technical field
The present invention relates to nano-porous materials preparing technical field, and in particular to a kind of prepared using bischofite as raw material aoxidizes
The method of magnesium aeroge.
Background technology
China salt lake is numerous, and abundant magnesium resource is contained in salt lake bittern.By taking Qinghai Chaerhan salt lakes as an example, wherein chlorine
Change 16.5 hundred million tons of magnesium reserves, account for the 74% of national magnesium salts resource, its bischofite（Magnesium chloride hexahydrate, MgCl2•6H2O）It is in the world
It is best in quality（Content is up to 96%）, yield maximum magnesium raw material.The production for developing into National Agricultural of potash fertilizer industry plays promotion
Effect, but since the magnesium chloride that one ton of potassium chloride of every extraction just has 8 ~ 11 tons flows back to salt lake, result in the part of magnesium salts in salt lake
Enrichment, becomes " the magnesium evil " in the development process of salt lake, this not only causes the serious waste of magnesium resource, but also breaks to a certain extent
The structure of salt lake resources is broken, influences the sustainable exploitation utilization of salt lake resources.By means of the superior evaporation conditions in the Caidamu Basin
Make Saturated with Magnesium chloride bittern continue to evaporate, magnesium salts primary product bischofite can be obtained, Cha Er Han Salt Lake can produce tens of every year
Ten thousand tons of bischofites, but price is cheap, and about 200 yuan/ton ~ 300 yuan/ton, added value is very low.Therefore, using salt lake magnesium resource as
The important channel that raw material directly prepares high-performance, the functional material of high added value is salt lake magnesium resource utilization.
Aeroge is a kind of nano material with three-dimensional continuous poriferous network structure, have high porosity, low-density and
The performance characteristics such as the architectural feature and thermal conductivity of high-specific surface area are low, the low harmony propagation rate of refractive index is low.Because its is excellent
Heat-proof quality（The even lower than thermal conductivity of air（0.024 W·m-1·K-1））, aeroge is known as ultra heat insulating material again,
Change the green material in the world.Aeroge can be widely applied to aerospace, building, stone because of its excellent physicochemical properties
The fields such as oil, liquid gas, military affairs, chemical industry, Thermal Power Engineering, Thermal Equipment, communications and transportation, household electrical appliance, naval vessel.Wherein, gather around
The porous magnesia aerogel material for having nanostructured has the features such as high-specific surface area, high catalytic activity, lower thermal conductivity, will be
The multiple fields such as catalysis, gas absorption, high efficiency heat insulation material have a wide range of applications.
Klabunde etc.（S. Utamapanya, K.J. Klabunde, J.R. Schlup, N, Chemistry of
Materials, 1991, 3(1): 175-181.）Earliest using magnesium methoxide as raw material, pass through sol-gel and supercritical drying
Method is prepared for hydrated magnesium aeroge, its specific surface area is up to 1000 m2•g-1.Gomez etc.（J.A. Wang, O.
Novaro, X. Bokhimi, et al., Materials Letters, 1998, 35(5): 317-323.）Then with ethanol
Magnesium is raw material, and second alcohol and water is mixed solvent, and oxalic acid is catalyst, by hydrolysis-condensation formed gel, 70oC is dried to obtain water
Close magnesia aeroge.Dong etc.（W. Dong, S.P. Yen, J.A. Paik, et al., Journal of the
American Ceramic Society, 2009, 92(5): 1011-1016）Report and matched somebody with somebody using acetic acid and glycerine to be organic
Body controls the hydrolysis of magnesium methoxide and polycondensation speed to prepare wet gel, and the magnesia of bulk amorphous is obtained under supercritical drying
Aeroge.In recent years, the magnesia of report and its oxide composite aerogel are still using magnesium alkoxide as raw material and supercritical drying
It is prepared by method（E.V. Ilyina, I.V. Mishakov, A.A Vedyaginet al., Microporous &
Mesoporous Materials, 2012, 160(1): 32-40. A. Feinle, A. Heugenhauser,
N.Hsing, Journal of Supercritical Fluids, 2015, 2(8): 1533-1535.A.T. Vu, S.
Jiang, K. Ho, et al., Chemical Engineering Journal, 2015, 269: 82-93.）.Utilize magnesium
Though alkoxide can quickly prepare magnesia wet gel, there are the following problems：First, magnesium alkoxide easily hydrolytie polycondensation, process are not easy
Control；Second, magnesium alkoxide toxicity is big, expensive, and temperature, the humidity to environment are extremely sensitive, are not easily-synthesized, preserve.
Therefore, there is still a need for a kind of simple, the efficient production method of technique can utilize cheap Bischofite in Salt lake
The magnesia aerogel material of excellent combination property is prepared as inorganic raw material, promotes the higher value application of salt lake magnesium resource.
The content of the invention
The present invention provides a kind of method that magnesia aeroge is prepared using bischofite as raw material, and the present invention efficiently solves
Existing to prepare magnesia wet gel using magnesium alkoxide, there are magnesium alkoxide easily hydrolytie polycondensation, process is difficult to control；Magnesium alkoxide toxicity
Greatly, it is expensive, and temperature, the humidity to environment are extremely sensitive, the problems such as not being easily-synthesized, preserve.
The present invention is achieved through the following technical solutions：
A kind of method that magnesia aeroge is prepared using bischofite as raw material, it is characterised in that：The preparation method is included such as
Lower step：
1）Bischofite, distilled water, alcoholic solvent, water soluble polymer are mixed, 5 ~ 120min of stirring obtains clear solution,
Epoxide is added to 5 ~ 60min of stirring in solution again and obtains colloidal sol；Wherein bischofite, distilled water, alcoholic solvent, water-soluble
Property macromolecule and epoxide mass ratio be 1:1~50:5~70:0.01~1:0.1~5；
2）By step 1）Obtained colloidal sol sealing carries out gelation, and gelling temperature is 20 ~ 95 DEG C, and gelation time is 2 ~ 20h,
Obtain magnesia wet gel；
3）By step 2）Obtained magnesia wet gel carries out washing by soaking with distilled water, and washing times are no less than three times, every time
When time is small no less than 2, distillation water consumption is no less than the volume of wet gel；
4）By step 3）Wet gel after embathing is dried, and uses supercritical drying or for vacuum freeze drying or be normal pressure
It is dry, magnesia aeroge is prepared.
The Technological improvement plan that further solves of the present invention is：
The step 1）In alcoholic solvent be methanol, ethanol, propyl alcohol, isopropanol, butanol, the one or more in the tert-butyl alcohol mix
Close.
The Technological improvement plan that further solves of the present invention is：
The step 1）In water soluble polymer for polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, polyethylene glycol oxide,
Polyacrylic acid, polyacrylamide, polymethylacrylic acid, polymaleic anhydride, amino resins, phenolic resin, epoxy resin, polyurethane
In resin, alkyd resin, amino resins, starch, chitosan, sodium alginate, gelatin, hydroxypropyl cellulose, carboxymethyl cellulose
One or more mixing.
The Technological improvement plan that further solves of the present invention is：
The step 1）In epoxide for propylene oxide, epoxychloropropane, epoxy bromopropane, 1,2- octylene oxides, first
In basic ring Ethylene Oxide, 1,2- Epoxydodecanes, 1,2- cyclopentane epoxides, methyl epichlorohydrin, epihydric acid ethyl ester
One or more mixing.
The Technological improvement plan that further solves of the present invention is：
The step 1）The mass ratio of middle distilled water is 10 ~ 30, and the mass ratio of water soluble polymer is 0.05 ~ 0.5, epoxy compound
The mass ratio of thing is 2 ~ 4.
The Technological improvement plan that further solves of the present invention is：
The step 2）Middle gelling temperature is 60 ~ 70 DEG C.
The Technological improvement plan that further solves of the present invention is：
The step 4）The porosity that magnesia aeroge is made is 71.6 ~ 99.3%, and pore-size distribution is 2 ~ 500nm, and BET compares table
Area is 50 ~ 1000m2·g-1, apparent density is 0.02 ~ 0.85 gcm-3。
The Technological improvement plan that further solves of the present invention is：
The step 4）The compression modulus that magnesia aeroge is made is 0.5 ~ 30 Mpa, and thermal conductivity is 0.01 ~ 0.10 Wm-1·k-1。
The Technological improvement plan that further solves of the present invention is：
The apparent density is 0.05 ~ 0.30 g cm-3.
The Technological improvement plan that further solves of the present invention is：
The thermal conductivity is 0.01 ~ 0.04Wm-1·k-1。
Compared with prior art, the present invention there is following obvious advantage：
First, the present invention can solve divalent state inorganic salts magnesium ion and exist using water soluble polymer as network structure guiding agent
The problem of precipitation occurs in hydrolysis, polycondensation process and cannot form three-dimensional net structure, the magnesia gel forming of acquisition is good,
It is readily available block aeroge.
2nd, the present invention uses the bischofite that salt lake is enriched to prepare magnesia aerogel material for raw material, has promoted salt lake
The higher value application of magnesium resource.
3rd, the present invention uses Bischofite in Salt lake raw material large storage capacity, cost is low, nontoxic for inorganic magnesium source.
Brief description of the drawings
The outside drawing of magnesia aeroge prepared by Fig. 1 embodiment of the present invention 1；
Fig. 2 is the stereoscan photograph of magnesia aeroge prepared by the embodiment of the present invention 3.
Embodiment
The technology of the present invention solution is further described with reference to embodiment：
Embodiment 1
Bischofite, distilled water, ethanol, polyvinyl alcohol are mixed, stirring 20min obtains clear solution, then by epoxy third
Alkane is added to stirring 10min in solution and obtains colloidal sol；Wherein bischofite, distilled water, ethanol, polyvinyl alcohol and propylene oxide
Mass ratio is 1:10:10:0.05:2.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 30 DEG C, and gelation time 2h, it is wet to obtain magnesia
Gel, is then washed three times with distilled water immersion, each 2h, and finally dry 24 h under 80 DEG C of atmospheric pressure environment, are aoxidized
Magnesium aeroge.The density of above-mentioned magnesia aeroge is 0.15 gcm-3, porosity 95.0%, BET specific surface area 200m2·
g-1, pore-size distribution is 5 ~ 250nm, 1.7 MPa of compression modulus, 0.03 Wm of thermal conductivity-1·k-1。
Embodiment 2
Bischofite, distilled water, ethanol, polymaleic anhydride are mixed, stirring 30min obtains clear solution, then by epoxy
Propane is added to stirring 5min in solution and obtains colloidal sol；Wherein bischofite, distilled water, ethanol, polymaleic anhydride and epoxy third
The mass ratio of alkane is 1:1:5:0.05:4.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 70 DEG C, and gelation time 20h, obtains magnesia
Wet gel, is then washed four times, each 3h, finally dry 24 h under 80 DEG C of atmospheric pressure environment, obtain oxygen with distilled water immersion
Change magnesium aeroge.The density of above-mentioned magnesia aeroge is 0.85 gcm-3, porosity 71.6%, BET specific surface area is
50m2·g-1, pore-size distribution is 10 ~ 200nm, compression modulus 30 MPa, thermal conductivity 0.10Wm-1·k-1。
Embodiment 3
Bischofite, distilled water, isopropanol, polymaleic anhydride are mixed, stirring 120min obtains clear solution, then by ring
Oxygen chloropropane is added to stirring 60min in solution and obtains colloidal sol；Wherein bischofite, distilled water, isopropanol, polymaleic anhydride and
The mass ratio of epoxychloropropane is 1:10:20:0.05:5.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 60 DEG C, and gelation time 10h, obtains magnesia
Wet gel, is then washed four times, each 3h with distilled water immersion, finally in -80 DEG C of 24 h of vacuum freeze drying, is aoxidized
Magnesium aeroge.The density of above-mentioned magnesia aeroge is 0.11 gcm-3, porosity 96.3%, BET specific surface area 520m2·
g-1, pore-size distribution is 5 ~ 210nm, compression modulus 1.2 MPa, thermal conductivity 0.027Wm-1·k-1。
Embodiment 4
Bischofite, distilled water, isopropanol, polyurethane are mixed, 60 min of stirring obtain clear solution, then by epoxy chlorine
Propane, which is added in solution, to be stirred 15 min and obtains colloidal sol；Wherein bischofite, distilled water, isopropanol, polyurethane and epoxy chlorine
The mass ratio of propane is 1:50:70:1:5.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 60 DEG C, and gelation time 6h, it is wet to obtain magnesia
Gel, is then washed four times, each 3h with distilled water immersion, finally in 24 h of supercritical drying, obtains magnesia aeroge.On
The density for stating magnesia aeroge is 0.02 gcm-3, porosity 99.3%, BET specific surface area is 1000 m2·g-1, aperture point
Cloth is 2 ~ 500 nm, compression modulus 0.5 MPa, thermal conductivity 0.01Wm-1·k-1。
Embodiment 5
Bischofite, distilled water, isopropanol, polyvinylpyrrolidone are mixed, 40 min of stirring obtain clear solution, then
1,2- octylene oxides are added in solution and stirs 25 min and obtains colloidal sol；Wherein bischofite, distilled water, isopropanol, poly- second
The mass ratio of alkene pyrrolidone and 1,2- octylene oxides is 1:20:30:0.06:4.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 40 DEG C, and gelation time is 8 h, obtains magnesia
Wet gel, is then washed four times, each 3h, finally dry 48 h under 80 DEG C of atmospheric pressure environment, obtain oxygen with distilled water immersion
Change magnesium aeroge.The density of above-mentioned magnesia aeroge is 0.08gcm-3, porosity 97.3%, BET specific surface area 670
m2·g-1, pore-size distribution is 2 ~ 300 nm, compression modulus 0.9 MPa, thermal conductivity 0.02Wm-1·k-1。
Embodiment 6
Bischofite, distilled water, the tert-butyl alcohol, starch are mixed, 40 min of stirring obtain clear solution, then by 1,2- rings
Oxygen octane, which is added in solution, to be stirred 25 min and obtains colloidal sol；Wherein bischofite, distilled water, the tert-butyl alcohol, starch and 1,2- rings
The mass ratio of oxygen octane is 1:20:30:0.06:4.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 40 DEG C, and gelation time is 8 h, obtains magnesia
Wet gel, is then washed four times, each 3h with distilled water immersion, finally in -80 DEG C of 48 h of vacuum freeze drying, is aoxidized
Magnesium aeroge.The density of above-mentioned magnesia aeroge is 0.06 gcm-3, porosity 98%, BET specific surface area is 710 m2·
g-1, pore-size distribution is 5 ~ 260 nm, compression modulus 0.7 MPa, thermal conductivity 0.017Wm-1·k-1。
It should be noted that above-described embodiment is only presently preferred embodiments of the present invention, it is not used for limiting the present invention's
Protection domain, the equivalent substitution or replacement made based on the above technical solutions, belongs to protection scope of the present invention,
Protection scope of the present invention is subject to claims.
Claims (10)
- A kind of 1. method that magnesia aeroge is prepared using bischofite as raw material, it is characterised in that：The preparation method includes Following steps：1）Bischofite, distilled water, alcoholic solvent, water soluble polymer are mixed, 5 ~ 120min of stirring obtains clear solution, Epoxide is added to 5 ~ 60min of stirring in solution again and obtains colloidal sol；Wherein bischofite, distilled water, alcoholic solvent, water-soluble Property macromolecule and epoxide mass ratio be 1:1~50:5~70:0.01~1:0.1~5；2）By step 1）Obtained colloidal sol sealing carries out gelation, and gelling temperature is 20 ~ 95 DEG C, and gelation time is 2 ~ 20h, Obtain magnesia wet gel；3）By step 2）Obtained magnesia wet gel carries out washing by soaking with distilled water, and washing times are no less than three times, every time When time is small no less than 2, distillation water consumption is no less than the volume of wet gel；4）By step 3）Wet gel after embathing is dried, and uses supercritical drying or for vacuum freeze drying or be normal pressure It is dry, magnesia aeroge is prepared.
- 2. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 1, its feature exist In：The step 1）In alcoholic solvent be methanol, ethanol, propyl alcohol, isopropanol, butanol, one or more mixing in the tert-butyl alcohol.
- 3. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 1 or 2, its feature It is：The step 1）In water soluble polymer for polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, polyethylene glycol oxide, Polyacrylic acid, polyacrylamide, polymethylacrylic acid, polymaleic anhydride, amino resins, phenolic resin, epoxy resin, polyurethane In resin, alkyd resin, amino resins, starch, chitosan, sodium alginate, gelatin, hydroxypropyl cellulose, carboxymethyl cellulose One or more mixing.
- 4. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 1 or 2, its feature It is：The step 1）In epoxide for propylene oxide, epoxychloropropane, epoxy bromopropane, 1,2- octylene oxides, In methyloxetane, 1,2- Epoxydodecanes, 1,2- cyclopentane epoxides, methyl epichlorohydrin, epihydric acid ethyl ester One or more mixing.
- 5. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 1 or 2, its feature It is：The step 1）The mass ratio of middle distilled water is 10 ~ 30, and the mass ratio of water soluble polymer is 0.05 ~ 0.5, epoxidation The mass ratio of compound is 2 ~ 4.
- 6. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 1 or 2, its feature It is：The step 2）Middle gelling temperature is 60 ~ 70 DEG C.
- 7. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 1 or 2, its feature It is：The step 4）The porosity that magnesia aeroge is made is 71.6 ~ 99.3%, and pore-size distribution is 2 ~ 500nm, and BET compares table Area is 50 ~ 1000m2·g-1, apparent density is 0.02 ~ 0.85 gcm-3。
- 8. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 1 or 2, its feature It is：The step 4）The compression modulus that magnesia aeroge is made is 0.5 ~ 30 Mpa, and thermal conductivity is 0.01 ~ 0.10 Wm-1·k-1。
- 9. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 7, its feature exist In：The apparent density is 0.05 ~ 0.30 g cm-3.
- 10. a kind of method that magnesia aeroge is prepared using bischofite as raw material according to claim 8, its feature exist In：The thermal conductivity is 0.01 ~ 0.04Wm-1·k-1。
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|---|---|---|---|---|
| WO2005033216A1 (en) * | 2003-10-03 | 2005-04-14 | Tateho Chemical Industries Co., Ltd. | Coated magnesium oxide powder capable of being highly filled and method for production thereof, and resin composition comprising the powder |
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| CN106832388A (en) * | 2017-03-10 | 2017-06-13 | 天津科技大学 | A kind of preparation method of aeroge |
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2017
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| WO2005033216A1 (en) * | 2003-10-03 | 2005-04-14 | Tateho Chemical Industries Co., Ltd. | Coated magnesium oxide powder capable of being highly filled and method for production thereof, and resin composition comprising the powder |
| CN1718281A (en) * | 2004-07-08 | 2006-01-11 | 武汉科技大学 | Cobalt/magnesium oxide aerogel catalyst, and method for producing nano-carbon tube therewith |
| CN103936037A (en) * | 2014-05-14 | 2014-07-23 | 徐子航 | Preparation method of magnesia aerogel material |
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