CN108017073B - A method of magnesia aeroge is prepared by raw material of bischofite - Google Patents
A method of magnesia aeroge is prepared by raw material of bischofite Download PDFInfo
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- CN108017073B CN108017073B CN201711448530.2A CN201711448530A CN108017073B CN 108017073 B CN108017073 B CN 108017073B CN 201711448530 A CN201711448530 A CN 201711448530A CN 108017073 B CN108017073 B CN 108017073B
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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
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Abstract
The invention discloses a kind of methods for preparing magnesia aeroge as raw material using bischofite, preparation method includes the following: 1) to mix bischofite, distilled water, alcoholic solvent, water soluble polymer, 5 ~ 120min of stirring obtains clear solution, then epoxide is added to 5 ~ 60min of stirring in solution and obtains colloidal sol;2) colloidal sol obtained 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, no less than three times, distillation water consumption is no less than the volume of wet gel to washing times;4) wet gel after embathing step 3) 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 not easy to control;The problems such as magnesium alkoxide toxicity is big, expensive, and extremely sensitive to the temperature of environment, humidity, is not easily-synthesized, saves.
Description
Technical field
The present invention relates to nano-porous materials preparation technical field, and in particular to a kind of prepared using bischofite as raw material aoxidizes
The method of magnesium aeroge.
Background technique
China salt lake is numerous, and magnesium resource abundant is contained in salt lake bittern.By taking Qinghai Chaerhan salt lakes as an example, wherein chlorine
16.5 hundred million tons of magnesium reserves of change, the 74% of Zhan Quanguo magnesium salts resource, bischofite (magnesium chloride hexahydrate, MgCl2•6H2It O is) in the world
(content up to 96%) best in quality, the maximum magnesium raw material of yield.The development of potash fertilizer industry is that the production of National Agricultural plays promotion
Effect, but since one ton of potassium chloride of every extraction just has 8 ~ 11 tons of magnesium chloride to flow back to salt lake, result in the part of magnesium salts in salt lake
Enrichment becomes " 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
It is broken the structure of salt lake resources, 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, can get magnesium salts primary product bischofite, 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, it is with salt lake magnesium resource
The important channel that raw material directly prepares high-performance, the functional material of high added value is the development and utilization of salt lake magnesium resource.
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 structure 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 (even lower than thermal conductivity (0.024 Wm of air-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, liquefied gas, military affairs, chemical industry, Thermal Power Engineering, Thermal Equipment, communications and transportation, household electrical appliance, naval vessel.Wherein, it gathers around
Having the porous magnesia aerogel material of nanostructure has high-specific surface area, will be the features such as high catalytic activity, lower thermal conductivity
The multiple fields such as catalysis, gas absorption, high efficiency heat insulation material have a wide range of applications.
(S. Utamapanya, K.J. Klabunde, J.R. Schlup, N, the Chemistry of such as Klabunde
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, and specific surface area is up to 1000 m2•g-1.(the J.A. Wang, O. such as Gomez
Novaro, X. Bokhimi, et al., Materials Letters, 1998,35 (5): 317-323.) then with ethyl alcohol
Magnesium is raw material, and second alcohol and water is mixed solvent, and oxalic acid is catalyst, forms gel by hydrolysis-condensation, 70oC is dried to obtain water
Close magnesia aeroge.(W. Dong, S.P. Yen, J.A. Paik, et al., the Journal of the such as Dong
American Ceramic Society, 2009,92 (5): 1011-1016) it reports and is matched using acetic acid and glycerol to be organic
Body prepares wet gel come the hydrolysis for controlling magnesium methoxide and polycondensation speed, 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
Method prepares (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 is that magnesium alkoxide easily hydrolytie polycondensation, process are not easy
Control;Second is that magnesium alkoxide toxicity is big, expensive, and extremely sensitive to the temperature of environment, humidity, it is not easily-synthesized, saves.
Therefore, there is still a need for a kind of simple process, high-efficient production method can utilize cheap Bischofite in Salt lake
The magnesia aerogel material of excellent combination property is prepared as inorganic raw material, pushes the higher value application of salt lake magnesium resource.
Summary of the invention
The present invention provides a kind of method for preparing magnesia aeroge as raw material using bischofite, and the present invention efficiently solves
Existing to prepare magnesia wet gel using magnesium alkoxide, there are magnesium alkoxide easily hydrolytie polycondensation, process is not easy to control;Magnesium alkoxide toxicity
Greatly, expensive and extremely sensitive to the temperature of environment, humidity, the problems such as not being easily-synthesized, save.
The invention is realized by the following technical scheme:
A method of magnesia aeroge is prepared by raw material of bischofite, it is characterised in that: the preparation method packet
Include following steps:
1) bischofite, distilled water, alcoholic solvent, water soluble polymer are mixed, 5 ~ 120min of stirring obtains transparent
Solution, then epoxide is added to 5 ~ 60min of stirring in solution and obtains colloidal sol;Wherein bischofite, distilled water, alcohol are molten
The mass ratio of agent, water soluble polymer and epoxide is 1:1 ~ 50:5 ~ 70:0.01 ~ 1:0.1 ~ 5;
2) by colloidal sol made from step 1) seal carry out gelation, gelling temperature be 20 ~ 95 DEG C, gelation time be 2 ~
20h obtains magnesia wet gel;
3) the magnesia wet gel that step 2 obtains being subjected to washing by soaking with distilled water, washing times are no less than three times,
Each time is no less than 2 hours, and distillation water consumption is no less than the volume of wet gel;
4) wet gel after embathing step 3) is dried, and uses supercritical drying or for vacuum freeze drying or is
Magnesia aeroge is prepared in constant pressure and dry.
The Technological improvement plan that the present invention further solves is:
Alcoholic solvent in the step 1) is one of methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, the tert-butyl alcohol or a variety of
Mixing.
The Technological improvement plan that the present invention further solves is:
Water soluble polymer in the step 1) is polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, polyoxyethylene
Alkene, polyacrylamide, polymethylacrylic acid, polymaleic anhydride, amino resins, phenolic resin, epoxy resin, gathers polyacrylic acid
Urethane resin, alkyd resin, amino resins, starch, chitosan, sodium alginate, gelatin, hydroxypropyl cellulose, carboxymethyl cellulose
One of element or a variety of mixing.
The Technological improvement plan that the present invention further solves is:
Epoxide in the step 1) is that propylene oxide, epoxychloropropane, epoxy bromopropane, 1,2- epoxy are pungent
Alkane, methyloxetane, 1,2- Epoxydodecane, 1,2- cyclopentane epoxide, methyl epichlorohydrin, epihydric acid ethyl ester
One of or a variety of mixing.
The Technological improvement plan that the present invention further solves is:
The mass ratio of distilled water is 10 ~ 30 in the step 1), and the mass ratio of water soluble polymer is 0.05 ~ 0.5, epoxy
The mass ratio of compound is 2 ~ 4.
The Technological improvement plan that the present invention further solves is:
Gelling temperature is 60 ~ 70 DEG C in the step 2.
The Technological improvement plan that the present invention further solves is:
The porosity that magnesia aeroge is made in the step 4) is 71.6 ~ 99.3%, and pore-size distribution is 2 ~ 500nm, BET
Specific surface area is 50 ~ 1000m2·g-1, apparent density is 0.02 ~ 0.85 gcm-3。
The Technological improvement plan that the present invention further solves is:
The compression modulus that magnesia aeroge is made in the step 4) is 0.5 ~ 30 Mpa, and thermal conductivity is 0.01 ~ 0.10
W·m-1·k-1。
The Technological improvement plan that the present invention further solves is:
The apparent density is 0.05 ~ 0.30 g cm-3.
The Technological improvement plan that the present invention further solves is:
The thermal conductivity is 0.01 ~ 0.04Wm-1·k-1。
Compared with prior art, the present invention having following obvious advantage:
One, the present invention using water soluble polymer as network structure guiding agent, can solve divalent state inorganic salts magnesium from
The problem of son occurs precipitating in hydrolysis, polycondensation process and cannot form three-dimensional net structure, the magnesia gel forming of acquisition
Property is good, is easy to get block aeroge.
Two, the present invention uses salt lake bischofite abundant to prepare magnesia aerogel material for raw material, has pushed salt lake
The higher value application of magnesium resource.
Three, the present invention uses Bischofite in Salt lake for inorganic magnesium source, and raw material reserves are big, at low cost, nontoxic.
Detailed description of the invention
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.
Specific embodiment
The technology of the present invention solution is further described below with reference to embodiment:
Embodiment 1
Bischofite, distilled water, ethyl alcohol, polyvinyl alcohol are mixed, stirring 20min obtains clear solution, then by ring
Ethylene Oxide is added to stirring 10min in solution and obtains colloidal sol;Wherein bischofite, distilled water, ethyl alcohol, polyvinyl alcohol and epoxy third
The mass ratio of alkane is 1:10:10:0.05:2.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 30 DEG C, and it is wet to obtain magnesia by gelation time 2h
Then gel is 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, ethyl alcohol, polymaleic anhydride are mixed, stirring 30min obtains clear solution, then will
Propylene oxide is added to stirring 5min in solution and obtains colloidal sol;Wherein bischofite, distilled water, ethyl alcohol, polymaleic anhydride and ring
The mass ratio of Ethylene Oxide 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
Then wet gel is washed four times, each 3h with distilled water immersion, finally dry 24 h under 80 DEG C of atmospheric pressure environment, obtain oxygen
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
Epoxychloropropane is added to stirring 60min in solution and obtains colloidal sol;Wherein bischofite, distilled water, isopropanol, poly
The mass ratio of acid anhydride and 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
Then wet gel is 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 ring
Oxygen chloropropane, which is added in solution, to be stirred 15 min and obtains colloidal sol;Wherein bischofite, distilled water, isopropanol, polyurethane and ring
The mass ratio of oxygen chloropropane is 1:50:70:1:5.
Above-mentioned colloidal sol is sealed and carries out gelation, gelling temperature is 60 DEG C, and it is wet to obtain magnesia by gelation time 6h
Then gel is 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 transparent molten
Liquid, then 1,2- octylene oxide is added in solution and stirs 25 min and obtains colloidal sol;Wherein bischofite, distilled water, isopropyl
The mass ratio of alcohol, polyvinylpyrrolidone and 1,2- octylene oxide 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
Then wet gel is washed four times, each 3h with distilled water immersion, finally dry 48 h under 80 DEG C of atmospheric pressure environment, obtain oxygen
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- octylene oxide, 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,
The mass ratio of 2- octylene oxide 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
Then wet gel is 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, there is no for the purpose of limiting the invention
Protection scope, the equivalent replacement or substitution made based on the above technical solution, all belongs to the scope of protection of the present invention,
Protection scope of the present invention is subject to claims.
Claims (7)
1. a kind of method for preparing magnesia aeroge as raw material using bischofite, it is characterised in that: the preparation method includes
Following steps:
1) bischofite, distilled water, alcoholic solvent, water soluble polymer being 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;Water soluble polymer is polyethylene
Alcohol, polyethylene glycol, polyvinylpyrrolidone, polyethylene glycol oxide, polyacrylic acid, polyacrylamide, polymethylacrylic acid, poly- Malaysia
Acid anhydrides, amino resins, phenolic resin, epoxy resin, polyurethane resin, alkyd resin, amino resins, starch, chitosan, seaweed
One of sour sodium, gelatin, hydroxypropyl cellulose, carboxymethyl cellulose or a variety of mixing;Epoxide is propylene oxide, ring
Oxygen chloropropane, epoxy bromopropane, 1,2- octylene oxide, methyloxetane, 1,2- Epoxydodecane, 1,2- cyclopentane epoxide,
One of methyl epichlorohydrin, epihydric acid ethyl ester or a variety of mixing;
2) colloidal sol made from step 1) being sealed and carries out gelation, gelling temperature is 20 ~ 95 DEG C, and gelation time is 2 ~ 20h,
Obtain magnesia wet gel;
3) the magnesia wet gel that step 2 obtains is subjected to washing by soaking with distilled water, washing times are no less than three times, every time
Time is no less than 2 hours, and distillation water consumption is no less than the volume of wet gel;
4) wet gel after embathing step 3) is dried, and uses supercritical drying or for vacuum freeze drying or be normal pressure
It is dry, magnesia aeroge is prepared;Be made magnesia aeroge porosity be 71.6 ~ 99.3%, pore-size distribution be 2 ~
500nm, BET specific surface area are 50 ~ 1000m2·g-1, apparent density is 0.02 ~ 0.85 gcm-3。
2. a kind of method for preparing magnesia aeroge as raw material using bischofite according to claim 1, feature exist
In: the alcoholic solvent in the step 1) is one of methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, the tert-butyl alcohol or a variety of mixing.
3. a kind of method for preparing magnesia aeroge as raw material using bischofite according to claim 1 or 2, feature
Be: the mass ratio of bischofite and distilled water is 1:10 ~ 30, the matter of bischofite and water soluble polymer in the step 1)
Ratio is measured as 1:0.05 ~ 0.5, the mass ratio of bischofite and epoxide is 1:2 ~ 4.
4. a kind of method for preparing magnesia aeroge as raw material using bischofite according to claim 1 or 2, feature
Be: gelling temperature is 60 ~ 70 DEG C in the step 2.
5. a kind of method for preparing magnesia aeroge as raw material using bischofite according to claim 1 or 2, feature
Be: the compression modulus that magnesia aeroge is made in the step 4) is 0.5 ~ 30 Mpa, and thermal conductivity is 0.01 ~ 0.10 Wm-1·k-1。
6. a kind of method for preparing magnesia aeroge as raw material using bischofite according to claim 1, feature exist
In: the apparent density is 0.05 ~ 0.30 g cm-3。
7. a kind of method for preparing magnesia aeroge as raw material using bischofite according to claim 5, feature exist
In: the thermal conductivity is 0.01 ~ 0.04Wm-1·k-1。
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