CN109010250A - Galapectite-silicon dioxide composite aerogel material and preparation method thereof - Google Patents
Galapectite-silicon dioxide composite aerogel material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides galapectite-silicon dioxide composite aerogel material and preparation method thereof, after galapectite dispersion liquid is polymerize with the mixed solution of dexamethasone, after ethyl orthosilicate, hydrochloric acid, Lovastatin and initiator are added into polymerizate again, polymerization reaction is carried out again, sodium hydroxide is added in reaction process, and the reaction was continued, obtains galapectite-silicon dioxide composite aerogel material.With gradually increasing for soaking time, the drug Lovastatin being carried in mesoporous takes the lead in discharging, and with further increasing for soaking time, the subsequent release of dexamethasone drug being carried in micropore realizes primary medication, the effect of multiple dosing.
Description
Technical field
The present invention relates to technical field of nano material, more specifically to a kind of compound airsetting of galapectite-silica
Glue material and preparation method thereof.
Background technique
Galapectite is natural one of clay mineral, belongs to kaolinic mutation, therefore also referred to as metakaolin.It is
It is crimped under field conditions (factors) by kaolinic lamella, main existence form is nanotube-shaped (Ma Zhi, king in nature
Gold leaf, Gao Xiang, Ding Tong, application study status [J] chemical progress of Qin Yongning halloysite nanotubes, 2012, (Z1): 275-
283.).Galapectite mine is distributed in each continent in the whole world, the countries such as China, France, Belgium, New Zealand, the U.S., Turkey
There are reserves abundant.Galapectite mine is mainly distributed on Guangdong, Hubei, Hunan, Sichuan, Guizhou, Yunnan, Shanxi etc. in China and saves
Part.
Galapectite is the double-deck 1:1 type aluminosilicate material, has typical crystalline texture.Galapectite is different from kaolinic
Substantive characteristics is that galapectite interlayer exists or once there is the crystallization water, and the lamella of galapectite is the oxygen-octahedron by outer layer
It is formed with the alumina octahedral regular array of internal layer, is free hydrone among lamella.These hydrones are easy to slough, this
Dehydration is irreversible.The outer surface of galapectite is mainly Si-O-Si key composition, and inner wall is then mainly aluminium hydroxyl (Niu Ji
South, Qiang Yinghuai, Wang Chunyang, Li Xiang, Monday is great, Shang Xiangyu, the village full the name of super galapectite, structure, pattern and curling mechanism
[J] mineral journal, 2014, (01): 13-22.).Silicon/aluminium hydroxyl is present on the crystallization edge of galapectite or the end face of pipe,
There is a small amount of embedding hydroxyl to be present in the inside of crystalline texture.Galapectite contains the water there are three types of state, mainly absorption water, crystallization
Water and chemical water.
Halloysite nanotubes have unique nanostructure, are a kind of natural nano-materials having a extensive future.And galapectite
Nanotube is widely distributed, cheap, nontoxic.Galapectite has following because of its unique nanostructure and tubular character
Advantage: firstly, it is from a wealth of sources, it is cheap；Galapectite is a kind of natural clay mineral, contains abundant, widely distributed and exploitation
It is easier to.Secondly, having good biocompatibility；Halloysite nanotubes self-assembling formation, nontoxic, biocompatibility is preferable.
In addition, active hydroxyl groups are contained in galapectite surface and interlayer, conducive to galapectite modification and further apply.Along with itself
Have the characteristics that biggish draw ratio and specific surface area, nanoscale, galapectite has obtained extensive concern and research in recent years.
The application field of halloysite nanotubes is extensive.In ceramic material, composite material, slow-release material, catalyst carrier, mould
Plate, adsorption applications etc. have a large amount of application.Because halloysite nanotubes are a kind of clay mines, it can be used for ceramic system
Make, this belongs to traditional application field of galapectite.Galapectite has the function of fiber reinforcement, is the ideal for preparing ultra-thin fine ceramics
Raw material.In recent years, the research of galapectite/polymer composites and its performance was becoming increasingly popular.Galapectite can be
Preferably disperse in most polymer composite material, mechanical property, thermal stability, anti-flammability and the knot of polymer can be effectively improved
Brilliant performance, having biggish advantage compared with other conventional fillers, (Wu Wei, Wu Pengjun, He Ding, Cao Xianwu, Zhou Nanqiao galapectite are received
Application progress [J] chemical industry progress of the mitron in high molecule nano composite material, 2011, (12): 2647-2651+2657.).
Galapectite has the characteristics that unique texture, environmental-friendly, cheap and easy to get, can prepare tool using its design feature and characterization of adsorption
There is the material of new structure and performance, is widely used in field of nanocomposite materials.
Summary of the invention
The present invention overcomes deficiencies in the prior art, provide a kind of galapectite-silicon dioxide composite aerogel material
And preparation method thereof, it uses the doughnut with microcellular structure for raw material, builds three-dimensional aeroge network, utilize aeroge
The microcellular structure of meso-hole structure and fiber, loads different pharmaceutical respectively, realizes the ladder-like classification release of drug.
The purpose of the present invention is achieved by following technical proposals.
Galapectite-silicon dioxide composite aerogel material and preparation method thereof carries out as steps described below:
Step 1,0.5-20 parts by weight halloysite nanotubes are added to 50 parts by weight of deionized water and 50 parts by weight of ethanol
Mixed liquor in, ultrasonic disperse is uniform, obtain galapectite dispersion liquid, by 0.5-20 parts by weight of styrene sodium sulfonate, 0.05-5 weight
The poly- divinylsiloxanes of part, 0.01-0.5 parts by weight initiator are measured, 0.05-15 parts by weight dexamethasone is added to 50 parts by weight
In the mixed liquor of deionized water and 50 parts by weight of ethanol, after mixing evenly, above-mentioned solution is added in galapectite dispersion liquid, is surpassed
After sound is uniformly dispersed, vacuum is kept after vacuumizing, is then restored to normal pressure, and after repeating vacuum step three times, product is washed
After be scattered in 100 parts by weight water, warming-in-water to initiated polymerization at 60-120 DEG C, polymerization reaction time is at least 48h,
Obtain the product of step 1；
Step 2, it is scattered in 100 parts by weight water after the product of step 1 being washed, the positive silicic acid second of 70-160 parts by weight is added
Ester, 0.05-2 parts by weight 12mol/L hydrochloric acid, the Lovastatin of 0.01-2 parts by weight initiator and 0.05-20 parts by weight, stirring are equal
After even, 0.01-0.5 parts by weight of sodium hydroxide is then added in warming-in-water to initiated polymerization at 30-75 DEG C, is stirred to it
After being completely dissolved, polymerization reaction time is at least 48h, and the compound wet gel of galapectite-silica is made；
Step 3,0.05-2 parts by weight methacryloxy is added in the above-mentioned compound wet gel of galapectite-silica
Dodecyl trimethyl ammonium chloride, after standing, place the product in CO2In supercritical high-pressure extraction device, with CO2It is medium in temperature
Supercritical drying at least 1h is carried out under 30-60 DEG C of degree and air pressure 5-15MPa, the compound airsetting of galapectite-silica can be obtained
Glue material.
Poly- divinylsiloxanes be number-average molecular weight 500-5000, preferably 1000-3000, contents of ethylene mole hundred
Score (i.e. the ratio of the poly dimethyl divinylsiloxanes molal quantity of vinyl molal quantity and entire amino list sealing end) 0.1-
The poly dimethyl divinylsiloxanes of 5% amino list sealing end or the poly dimethyl divinyl silicon oxygen of amino bi-end-blocking
Alkane, poly- divinylsiloxanes are purchased from Dow corning company.
In step 1, halloysite nanotubes are 1-15 parts by weight, are added in the mixed liquor of deionized water and ethyl alcohol ultrasonic
Disperse 1h, sodium styrene sulfonate is 1-15 parts by weight, and poly- divinylsiloxanes are 0.1-2 parts by weight, initiator 0.01-
0.1 parts by weight, dexamethasone are 0.1-10 parts by weight, are added in the mixed liquor of deionized water and ethyl alcohol and stir 20-60min
Afterwards, it is added in galapectite dispersion liquid, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor.
In step 1, selection polyase 13 0-60min at 60-120 DEG C when carrying out polymerization reaction, is then cooled to 15-
It polymerize 12-24h at 50 DEG C, then successively polymerize 2-8h respectively at 80 DEG C, 90 DEG C and 100 DEG C.
In step 2,80-150 parts by weight ethyl orthosilicate, 0.1-1 parts by weight 12mol/L are added into above-mentioned dispersion liquid
Hydrochloric acid, 0.01-1 parts by weight initiator and 0.1-15 parts by weight Lovastatin stir 15-60min.
In step 2, when carrying out polymerization reaction, selection polymerize 15-40min at 30-75 DEG C, and 0.01-0.2 weight is added
Part sodium hydroxide is measured, stirring is completely dissolved to it, is then cooled in 20-50 DEG C of water bath with thermostatic control and polymerize 20-35h, then successively
It polymerize 2h respectively at 80 DEG C, 90 DEG C and 100 DEG C.
Initiator selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
In step 3, methacryloxy dodecyl trimethyl ammonium chloride is 0.1-1 parts by weight, and time of repose is
2-6h, the condition of supercritical drying are that supercritical drying 2-4h, preferably 3h are carried out at 33-50 DEG C of temperature and air pressure 7-10MPa.
Positive charge is had on the inside of halloysite nanotubes tube wall, and negative electrical charge, the styrene being added in step 1 are had on the outside of tube wall
Sodium sulfonate has negative electrical charge, and sodium styrene sulfonate is adsorbed on halloysite nanotubes inner wall by electrostatic interaction, while in step 1
Poly- divinylsiloxanes, initiator and the dexamethasone of middle addition are also dispersed in halloysite nanotubes hollow structure, Ai Luo
Stone nanotube hollow structure provides microcellular structure for galapectite-silicon dioxide composite aerogel material, by vacuumizing, washing
Afterwards, poly- divinylsiloxanes are copolymerized with sodium styrene sulfonate, are formed and are formed cross-linked structure inside halloysite nanotubes, will
Dexamethasone is supported in halloysite nanotubes, and step 2 makes the poly- divinyl being located at outside halloysite nanotubes hollow structure
It polymerize under the action of initiator between vinyl functional group on siloxanes, so that halloysite nanotubes and poly- divinyl
Radical siloxane is collectively formed tridimensional network, and the ethyl orthosilicate being added in step 2, hydrochloric acid and sodium hydroxide react shape
At SiO2Particle, SiO2Particle is configured to network pore structure, above-mentioned tridimensional network and SiO2The built-up network of particle
Pore structure together forms three-dimensional network pore structure, and above-mentioned three-dimensional network pore structure is that galapectite-silica is compound
Aerogel material provides meso-hole structure, while Lovastatin being supported in meso-hole structure.
Using scientific and technological (Beijing) the Co., Ltd 3H-2000PS1 type static volumetric method specific surface area of Bei Shide instrument and aperture
The N of the tester analysis composite material that according to the present invention prepared by the method2Adsorption-desorption curve, such as Fig. 1.It can be with from figure
Find out, the N of the material2Adsorption-desorption curve is the IV class isothermal curve of H1 type hysteresis loop in IUPAC classification, i.e., by mesoporous knot
Structure generates.Illustrate that material itself has the pore structure of meso-scale.There is vertical ascent trend from the distribution of low pressure endpoint, can see
Sample interior is as caused by absorption potential strong inside micropore there are more micropore out.By nitrogen adsorption desorption isotherm data,
The sample specific surface area can reach 602.14m2g-1, which exists simultaneously mesoporous-micropore second level pore structure, surveys through multiple groups
The average specific surface area for measuring material is 600-608m2g-1。
By N2Data in adsorption-desorption curve are substituted into correlation values, can be arranged by BJH formula and Kelvin equation
Obtain the accounting equation r in aperturek=-0.954/ln (p/p0), unit nm, while adding adsorbent layer thickness t=0.356 [- 5/
ln(p/p0)] ^ (1/3), can obtain effective aperture is r=rk+ t, therefore aperture is the function influenced by relative pressure, so may be used
In the hope of the aperture under different relative pressures, it can calculate and acquire in material that there are two aperture points to be distributed, Yi Zhongwei
10.37nm, another kind are 2.056 μm, are measured through multiple groups, and nanoscale hole is average up to 10-12nm, and micro-meter scale hole is flat
Up to 2-4 μm.It can be seen that material exists simultaneously nanoscale and micro-meter scale hole.
It is saturating using the Nanosem430 field emission scanning electron microscope and TecnaiG2F20 Flied emission of Dutch Philips
It penetrates electron microscope to observe the microscopic appearance of the composite material prepared using the method for the invention, as shown in Figure 2.From
As can be seen that SiO in figure2Particle is successfully configured to network pore structure, and aperture size is in mesoporous scale.It is overlapped to form three-dimensional netted
Halloysite nanotubes be uniformly dispersed in SiO2In three-dimensional network hole, the building of dual load system is realized.
Reference literature (Li Degui, the preparation and characterization of nano-cellulose base Thermosensitive Material Used for Controlled Releasing of Medicine, South China Science & Engineering University,
2016) method described in carries out sustained release performance test characterization to material prepared by the present invention.Two sustained release steps are delayed respectively
It releases product and carries out infrared spectroscopy detection, as a result as shown in figure 3, by being compareed with standard diagram, it was demonstrated that take the lead in release is that Lip river is cut down
Statin, what is then discharged is dexamethasone, realizes the multiple dimensioned load and repeatedly release of different pharmaceutical.
The composite material carrying medicament prepared using the method for the invention is placed in simulation human consumption's liquid, measurement
Its drug release effect, figure 4, it is seen that gradually increasing with soaking time, the drug Lip river being carried in mesoporous is cut down
Statin takes the lead in discharging, and with further increasing for soaking time, the subsequent release of dexamethasone drug being carried in micropore is realized
Primary medication, the effect of multiple dosing.
Detailed description of the invention
Fig. 1 is galapectite-silicon dioxide composite aerogel material N2Adsorption-desorption curve；
Fig. 2 is galapectite-silicon dioxide composite aerogel material electromicroscopic photograph；
Fig. 3 is galapectite-silicon dioxide composite aerogel material release product test curve；
Fig. 4 is galapectite-silicon dioxide composite aerogel material carrying medicament release profiles.
Specific embodiment
Below by specific embodiment, further description of the technical solution of the present invention.
Embodiment 1.
1 parts by weight halloysite nanotubes are added in the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol,
Ultrasonic disperse 1h obtains galapectite dispersion liquid, by 6 parts by weight of styrene sodium sulfonates, the poly- divinylsiloxanes of 0.4 parts by weight
(number-average molecular weight 5000, the poly dimethyl divinyl silicon oxygen of the amino bi-end-blocking of contents of ethylene mole percent 0.1%
Alkane), 0.01 parts by weight azodiisobutyronitrile (ABIN), 10 parts by weight dexamethasone are added to 50 parts by weight of deionized water and 50 weights
In the mixed liquor for measuring part ethyl alcohol, 55min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min, by above-mentioned mixed liquor
1h is kept after vacuumizing, is then restored to normal pressure, after repeating vacuum step three times, product is washed, 100 weights are then dispersed in
It measures in part water, is placed under 120 DEG C of water bath condition after prepolymerization 25min in 50 DEG C of water bath with thermostatic control and polymerize 12 hours, then
After it is successively polymerize 4h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, 100 parts by weight are scattered in after product is washed
In water, 88 parts by weight ethyl orthosilicates, 0.9 parts by weight 12mol/L hydrochloric acid, 1 parts by weight azodiisobutyronitrile (ABIN) and 6 is added
The Lovastatin of parts by weight, at room temperature stir 45min after under 65 DEG C of water bath condition prepolymerization 40min, be then added 0.01
Parts by weight of sodium hydroxide, stirring are completely dissolved to it, then polymerize 25 hours in 40 DEG C of water bath with thermostatic control, then successively by it
The compound wet gel of galapectite-silica is obtained after respectively placing 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, in an angstrom Lip river
0.4 parts by weight methacryloxy dodecyl trimethyl ammonium chloride is added in the compound wet gel of stone-silica, stands 4h
Afterwards, place the product in CO2In supercritical high-pressure extraction device, with CO2Super face is carried out under temperature 50 C and air pressure 7MPa for medium
3h is dried on boundary, and galapectite-silicon dioxide composite aerogel material can be obtained.
Embodiment 2.
15 parts by weight halloysite nanotubes are added in the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol,
Ultrasonic disperse 1h obtains galapectite dispersion liquid, by 10 parts by weight of styrene sodium sulfonates, the poly- divinylsiloxanes of 0.1 parts by weight
(number-average molecular weight 500, the poly dimethyl divinylsiloxanes of the amino list sealing end of contents of ethylene mole percent 5%),
0.1 parts by weight dibenzoyl peroxide (BPO), 5 parts by weight dexamethasone are added to 50 parts by weight of deionized water and 50 parts by weight
In the mixed liquor of ethyl alcohol, 20min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min, above-mentioned mixed liquor taken out true
1h is kept after sky, is then restored to normal pressure, after repeating vacuum step three times, product is washed, 100 parts by weight are then dispersed in
In water, be placed under 98 DEG C of water bath condition after prepolymerization 43min in 40 DEG C of water bath with thermostatic control and polymerize 19 hours, then by its according to
It is secondary polymerize 8h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control after, be scattered in after product is washed in 100 parts by weight water,
80 parts by weight ethyl orthosilicates, 0.5 parts by weight 12mol/L hydrochloric acid, 0.5 parts by weight dibenzoyl peroxide (BPO) and 15 is added
The Lovastatin of parts by weight, at room temperature stir 15min after under 55 DEG C of water bath condition prepolymerization 28min, be then added 0.13
Parts by weight of sodium hydroxide, stirring are completely dissolved to it, then polymerize 20 hours in 50 DEG C of water bath with thermostatic control, then successively by it
The compound wet gel of galapectite-silica is obtained after respectively placing 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, in an angstrom Lip river
0.2 parts by weight methacryloxy dodecyl trimethyl ammonium chloride is added in the compound wet gel of stone-silica, stands 5h
Afterwards, place the product in CO2In supercritical high-pressure extraction device, with CO2Super face is carried out under temperature 45 C and air pressure 8MPa for medium
3h is dried on boundary, and galapectite-silicon dioxide composite aerogel material can be obtained.
Embodiment 3.
8 parts by weight halloysite nanotubes are added in the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol,
Ultrasonic disperse 1h obtains galapectite dispersion liquid, by 15 parts by weight of styrene sodium sulfonates, the poly- divinylsiloxanes of 0.8 parts by weight
(number-average molecular weight 3000, the poly dimethyl divinylsiloxanes of the amino list sealing end of contents of ethylene mole percent 1%),
0.08 parts by weight azodiisobutyronitrile (ABIN), 3 parts by weight dexamethasone are added to 50 parts by weight of deionized water and 50 parts by weight
In the mixed liquor of ethyl alcohol, 52min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min, above-mentioned mixed liquor taken out true
1h is kept after sky, is then restored to normal pressure, after repeating vacuum step three times, product is washed, 100 parts by weight are then dispersed in
In water, be placed under 60 DEG C of water bath condition after prepolymerization 10min in 30 DEG C of water bath with thermostatic control and polymerize 18 hours, then by its according to
It is secondary polymerize 5h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control after, be scattered in after product is washed in 100 parts by weight water,
150 parts by weight ethyl orthosilicates, 0.1 parts by weight 12mol/L hydrochloric acid, 0.9 parts by weight azodiisobutyronitrile (ABIN) and 4 weights are added
Measure part Lovastatin, at room temperature stir 30min after under 66 DEG C of water bath condition prepolymerization 20min, then be added 0.19 weight
Part sodium hydroxide is measured, stirring is completely dissolved to it, and then polyase 13 0 hour in 30 DEG C of water bath with thermostatic control, then successively exists it
80 DEG C, 90 DEG C, the compound wet gel of galapectite-silica is obtained after respectively placing 2h in 100 DEG C of water bath with thermostatic control, in galapectite-
1 parts by weight methacryloxy dodecyl trimethyl ammonium chloride is added in the compound wet gel of silica, it, will after standing 2h
Product is placed in CO2In supercritical high-pressure extraction device, with CO2It is carried out at 38 DEG C of temperature and air pressure 8.5MPa for medium overcritical
Dry 3h, can be obtained galapectite-silicon dioxide composite aerogel material.
Embodiment 4.
3 parts by weight halloysite nanotubes are added in the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol,
Ultrasonic disperse 1h obtains galapectite dispersion liquid, by 5 parts by weight of styrene sodium sulfonates, the poly- divinylsiloxanes of 0.9 parts by weight
(number-average molecular weight 1000, the poly dimethyl divinylsiloxanes of the amino list sealing end of contents of ethylene mole percent 4%),
0.04 parts by weight dibenzoyl peroxide (BPO), 8 parts by weight dexamethasone are added to 50 parts by weight of deionized water and 50 parts by weight
In the mixed liquor of ethyl alcohol, 60min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min, above-mentioned mixed liquor taken out true
1h is kept after sky, is then restored to normal pressure, after repeating vacuum step three times, product is washed, 100 parts by weight are then dispersed in
In water, be placed under 85 DEG C of water bath condition after prepolymerization 19min in 25 DEG C of water bath with thermostatic control and polymerize 15 hours, then by its according to
It is secondary in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control distinguish polyase 13 h after, be scattered in after product is washed in 100 parts by weight water,
90 parts by weight ethyl orthosilicates, 1 parts by weight 12mol/L hydrochloric acid, 0.3 parts by weight dibenzoyl peroxide (BPO) and 7 weight are added
Part Lovastatin, at room temperature stir 55min after under 75 DEG C of water bath condition prepolymerization 15min, then be added 0.02 weight
Part sodium hydroxide, stirring are completely dissolved to it, then polymerize 28 hours in 45 DEG C of water bath with thermostatic control, then by it successively 80
DEG C, 90 DEG C, the compound wet gel of galapectite-silica is obtained after respectively placing 2h in 100 DEG C of water bath with thermostatic control, in galapectite-two
0.7 parts by weight methacryloxy dodecyl trimethyl ammonium chloride is added in the compound wet gel of silica, it, will after standing 3h
Product is placed in CO2In supercritical high-pressure extraction device, with CO2It is carried out at 43 DEG C of temperature and air pressure 7.5MPa for medium overcritical
Dry 3h, can be obtained galapectite-silicon dioxide composite aerogel material.
Embodiment 5.
4 parts by weight halloysite nanotubes are added in the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol,
Ultrasonic disperse 1h obtains galapectite dispersion liquid, by 3 parts by weight of styrene sodium sulfonates, the poly- divinylsiloxanes of 1.4 parts by weight
(number-average molecular weight 2500, the poly dimethyl divinylsiloxanes of the amino bi-end-blocking of contents of ethylene mole percent 3%),
0.05 parts by weight dibenzoyl peroxide (BPO), 0.1 parts by weight dexamethasone are added to 50 parts by weight of deionized water and 50 weight
In the mixed liquor of part ethyl alcohol, 35min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min takes out above-mentioned mixed liquor
1h is kept after vacuum, is then restored to normal pressure, after repeating vacuum step three times, product is washed, 100 weight are then dispersed in
It in part water, is placed under 110 DEG C of water bath condition after prepolymerization 31min and polymerize 24 hours in 35 DEG C of water bath with thermostatic control, then will
After it successively polymerize 2h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, 100 parts by weight water are scattered in after product is washed
In, be added 89 parts by weight ethyl orthosilicates, 0.7 parts by weight 12mol/L hydrochloric acid, 0.1 parts by weight dibenzoyl peroxide (BPO) and
The Lovastatin of 0.1 parts by weight stirs prepolymerization 33min, then addition under 44 DEG C of water bath condition after 41min at room temperature
0.2 parts by weight of sodium hydroxide, stirring are completely dissolved to it, then polymerize 26 hours in 20 DEG C of water bath with thermostatic control, then by it
Obtain the compound wet gel of galapectite-silica after successively respectively placing 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, angstrom
0.8 parts by weight methacryloxy dodecyl trimethyl ammonium chloride is added in Lip river stone-compound wet gel of silica, stands
After 6h, place the product in CO2In supercritical high-pressure extraction device, with CO2It is carried out at 33 DEG C of temperature and air pressure 10MPa for medium
Galapectite-silicon dioxide composite aerogel material can be obtained in supercritical drying 3h.
Embodiment 6.
9 parts by weight halloysite nanotubes are added in the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol,
Ultrasonic disperse 1h obtains galapectite dispersion liquid, by 1 parts by weight of styrene sodium sulfonate, the poly- divinylsiloxanes of 1.8 parts by weight
(number-average molecular weight 4000, the poly dimethyl divinylsiloxanes of the amino list sealing end of contents of ethylene mole percent 1%),
0.07 parts by weight azodiisobutyronitrile (ABIN), 4 parts by weight dexamethasone are added to 50 parts by weight of deionized water and 50 parts by weight
In the mixed liquor of ethyl alcohol, 44min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min, above-mentioned mixed liquor taken out true
1h is kept after sky, is then restored to normal pressure, after repeating vacuum step three times, product is washed, 100 parts by weight are then dispersed in
In water, be placed under 80 DEG C of water bath condition after prepolymerization 60min in 15 DEG C of water bath with thermostatic control and polymerize 20 hours, then by its according to
It is secondary polymerize 6h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control after, be scattered in after product is washed in 100 parts by weight water,
87 parts by weight ethyl orthosilicates, 0.8 parts by weight 12mol/L hydrochloric acid, 0.8 parts by weight azodiisobutyronitrile (ABIN) and 5 weights are added
Measure part Lovastatin, at room temperature stir 60min after under 30 DEG C of water bath condition prepolymerization 25min, then be added 0.18 weight
Part sodium hydroxide is measured, stirring is completely dissolved to it, and then polyase 13 5 hours in 35 DEG C of water bath with thermostatic control, then successively exist it
80 DEG C, 90 DEG C, the compound wet gel of galapectite-silica is obtained after respectively placing 2h in 100 DEG C of water bath with thermostatic control, in galapectite-
0.1 parts by weight methacryloxy dodecyl trimethyl ammonium chloride is added in the compound wet gel of silica, stands 3.5h
Afterwards, place the product in CO2In supercritical high-pressure extraction device, with CO2Super face is carried out at 39 DEG C of temperature and air pressure 9MPa for medium
3h is dried on boundary, and galapectite-silicon dioxide composite aerogel material can be obtained.
Embodiment 7
0.5 parts by weight halloysite nanotubes are added to the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol
In, ultrasonic disperse 1h obtains galapectite dispersion liquid, by 0.5 parts by weight of styrene sodium sulfonate, the poly- divinyl silicon of 0.05 parts by weight
Oxygen alkane (number-average molecular weight 1500, the poly dimethyl divinyl silicon oxygen of the amino list sealing end of contents of ethylene mole percent 2%
Alkane), 0.01 parts by weight dibenzoyl peroxide (BPO), 0.05 parts by weight dexamethasone be added to 50 parts by weight of deionized water and
In the mixed liquor of 50 parts by weight of ethanol, 20min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min, it will be above-mentioned mixed
It closes after liquid vacuumizes and keeps 1h, be then restored to normal pressure, after repeating vacuum step three times, product is washed, is then dispersed in
In 100 parts by weight water, it is placed under 98 DEG C of water bath condition after prepolymerization 43min and polymerize 19 hours in 40 DEG C of water bath with thermostatic control,
After it is successively then polymerize 8h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, 100 weights are scattered in after product is washed
It measures in part water, 70 parts by weight ethyl orthosilicates, 0.05 parts by weight 12mol/L hydrochloric acid, 0.01 parts by weight diphenyl peroxide first is added
The Lovastatin of acyl (BPO) and 0.05 parts by weight, at room temperature stir 15min after under 55 DEG C of water bath condition prepolymerization 28min,
0.01 parts by weight of sodium hydroxide is then added, stirring is completely dissolved to it, then polymerize 20 hours in 50 DEG C of water bath with thermostatic control,
It is then successively respectively placed in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control to obtain galapectite-silica after 2h compound wet
0.05 parts by weight methacryloxy trimethyl is added in gel in the compound wet gel of galapectite-silica
Ammonium chloride, after standing 5h, place the product in CO2In supercritical high-pressure extraction device, with CO2It is medium in 30 DEG C of temperature and air pressure
Supercritical drying 4h is carried out under 15MPa, and galapectite-silicon dioxide composite aerogel material can be obtained.
Embodiment 8
20 parts by weight halloysite nanotubes are added in the mixed liquor of 50 parts by weight of deionized water and 50 parts by weight of ethanol,
Ultrasonic disperse 1h obtains galapectite dispersion liquid, by 20 parts by weight of styrene sodium sulfonates, the poly- divinylsiloxanes of 5 parts by weight (number
Average molecular weight 900, the poly dimethyl divinylsiloxanes of the amino list sealing end of contents of ethylene mole percent 3.5%),
0.5 parts by weight azodiisobutyronitrile (ABIN), 15 parts by weight dexamethasone are added to 50 parts by weight of deionized water and 50 parts by weight
In the mixed liquor of ethyl alcohol, 44min is stirred, is added in galapectite dispersion liquid, ultrasonic disperse 30min, above-mentioned mixed liquor taken out true
1h is kept after sky, is then restored to normal pressure, after repeating vacuum step three times, product is washed, 100 parts by weight are then dispersed in
In water, be placed under 80 DEG C of water bath condition after prepolymerization 60min in 15 DEG C of water bath with thermostatic control and polymerize 20 hours, then by its according to
It is secondary polymerize 6h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control after, be scattered in after product is washed in 100 parts by weight water,
160 parts by weight ethyl orthosilicates, 2 parts by weight 12mol/L hydrochloric acid, 2 parts by weight azodiisobutyronitriles (ABIN) and 20 weight are added
Part Lovastatin, at room temperature stir 60min after under 30 DEG C of water bath condition prepolymerization 25min, then be added 0.5 parts by weight
Sodium hydroxide is stirred to it and is completely dissolved, then polyase 13 5 hours in 35 DEG C of water bath with thermostatic control, then by it successively 80
DEG C, 90 DEG C, the compound wet gel of galapectite-silica is obtained after respectively placing 2h in 100 DEG C of water bath with thermostatic control, in galapectite-two
2 parts by weight methacryloxy dodecyl trimethyl ammonium chloride are added in the compound wet gel of silica, it, will after standing 3.5h
Product is placed in CO2In supercritical high-pressure extraction device, with CO2Supercritical drying is carried out under temperature 60 C and air pressure 5MPa for medium
Galapectite-silicon dioxide composite aerogel material can be obtained in dry 2h.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (10)
1. galapectite-silicon dioxide composite aerogel material, it is characterised in that: galapectite-silicon dioxide composite aerogel material
Average specific surface area is 600-608m2g-1, nanoscale and micro- is existed simultaneously in galapectite-silicon dioxide composite aerogel material
Metrical scale hole, nanoscale hole average out to 10-12nm, 2-4 μm of average out to of micro-meter scale hole, as steps described below into
Row:
Step 1,0.5-20 parts by weight halloysite nanotubes are added to the mixed of 50 parts by weight of deionized water and 50 parts by weight of ethanol
It closes in liquid, ultrasonic disperse is uniform, galapectite dispersion liquid is obtained, by 0.5-20 parts by weight of styrene sodium sulfonate, 0.05-5 parts by weight
Poly- divinylsiloxanes, 0.01-0.5 parts by weight initiator, 0.05-15 parts by weight dexamethasone be added to 50 parts by weight go from
In sub- water and the mixed liquor of 50 parts by weight of ethanol, after mixing evenly, above-mentioned solution is added in galapectite dispersion liquid, ultrasound point
After dissipating uniformly, vacuum is kept after vacuumizing, is then restored to normal pressure, after repeating vacuum step three times, is divided after product is washed
It dissipates in 100 parts by weight water, warming-in-water to initiated polymerization at 60-120 DEG C, polymerization reaction time is at least 48h, obtains
The product of step 1；
Poly- divinylsiloxanes be number-average molecular weight 500-5000, preferably 1000-3000, contents of ethylene mole percent
(i.e. the ratio of the poly dimethyl divinylsiloxanes molal quantity of vinyl molal quantity and entire amino list sealing end) 0.1-5%'s
The poly dimethyl divinylsiloxanes of amino list sealing end or the poly dimethyl divinylsiloxanes of amino bi-end-blocking；
Step 2, it is scattered in 100 parts by weight water after the product of step 1 being washed, 70-160 parts by weight ethyl orthosilicate is added,
0.05-2 parts by weight 12mol/L hydrochloric acid, the Lovastatin of 0.01-2 parts by weight initiator and 0.05-20 parts by weight stir evenly
Afterwards, warming-in-water is then added 0.01-0.5 parts by weight of sodium hydroxide, stirs complete to its to initiated polymerization at 30-75 DEG C
After fully dissolved, polymerization reaction time is at least 48h, and the compound wet gel of galapectite-silica is made；
Step 3,0.05-2 parts by weight methacryloxy 12 is added in the above-mentioned compound wet gel of galapectite-silica
Alkyl trimethyl ammonium chloride, after standing, place the product in CO2In supercritical high-pressure extraction device, with CO2It is medium in temperature 30-
Supercritical drying at least 1h is carried out under 60 DEG C and air pressure 5-15MPa, and galapectite-silicon dioxide composite aerogel material can be obtained
Material.
2. galapectite according to claim 1-silicon dioxide composite aerogel material, it is characterised in that: in step 1,
Halloysite nanotubes are 1-15 parts by weight, are added to ultrasonic disperse 1h, styrene sulfonic acid in the mixed liquor of deionized water and ethyl alcohol
Sodium is 1-15 parts by weight, and poly- divinylsiloxanes are 0.1-2 parts by weight, and initiator is 0.01-0.1 parts by weight, dexamethasone
It for 0.1-10 parts by weight, is added to after stirring 20-60min in the mixed liquor of deionized water and ethyl alcohol, is added to galapectite dispersion
In liquid, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, and when carrying out polymerization reaction, selection is at 60-120 DEG C
Lower polyase 13 0-60min, is then cooled at 15-50 DEG C and polymerize 12-24h, then successively gathers respectively at 80 DEG C, 90 DEG C and 100 DEG C
Close 2-8h.
3. galapectite according to claim 1-silicon dioxide composite aerogel material, it is characterised in that: in step 2,
80-150 parts by weight ethyl orthosilicate, 0.1-1 parts by weight 12mol/L hydrochloric acid, 0.01-1 parts by weight are added into above-mentioned dispersion liquid
Initiator and 0.1-15 parts by weight Lovastatin stir 15-60min, and when carrying out polymerization reaction, selection polymerize at 30-75 DEG C
0.01-0.2 parts by weight of sodium hydroxide is added in 15-40min, and stirring is completely dissolved to it, is then cooled to 20-50 DEG C of constant temperature
It polymerize 20-35h in water-bath, then successively polymerize 2h respectively at 80 DEG C, 90 DEG C and 100 DEG C.
4. galapectite according to claim 1-silicon dioxide composite aerogel material, it is characterised in that: initiator selection
Dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
5. galapectite according to claim 1-silicon dioxide composite aerogel material, it is characterised in that: in step 3,
Methacryloxy dodecyl trimethyl ammonium chloride is 0.1-1 parts by weight, time of repose 2-6h, the item of supercritical drying
Part is that supercritical drying 2-4h, preferably 3h are carried out at 33-50 DEG C of temperature and air pressure 7-10MPa.
6. preparing galapectite as claimed in claim 1 to 5-silicon dioxide composite aerogel material method, feature
It is: carries out as steps described below:
Step 1,0.5-20 parts by weight halloysite nanotubes are added to the mixed of 50 parts by weight of deionized water and 50 parts by weight of ethanol
It closes in liquid, ultrasonic disperse is uniform, galapectite dispersion liquid is obtained, by 0.5-20 parts by weight of styrene sodium sulfonate, 0.05-5 parts by weight
Poly- divinylsiloxanes, 0.01-0.5 parts by weight initiator, 0.05-15 parts by weight dexamethasone be added to 50 parts by weight go from
In sub- water and the mixed liquor of 50 parts by weight of ethanol, after mixing evenly, above-mentioned solution is added in galapectite dispersion liquid, ultrasound point
After dissipating uniformly, vacuum is kept after vacuumizing, is then restored to normal pressure, after repeating vacuum step three times, is divided after product is washed
It dissipates in 100 parts by weight water, warming-in-water to initiated polymerization at 60-120 DEG C, polymerization reaction time is at least 48h, obtains
The product of step 1；
Poly- divinylsiloxanes be number-average molecular weight 500-5000, preferably 1000-3000, contents of ethylene mole percent
(i.e. the ratio of the poly dimethyl divinylsiloxanes molal quantity of vinyl molal quantity and entire amino list sealing end) 0.1-5%'s
The poly dimethyl divinylsiloxanes of amino list sealing end or the poly dimethyl divinylsiloxanes of amino bi-end-blocking；
Step 2, it is scattered in 100 parts by weight water after the product of step 1 being washed, 70-160 parts by weight ethyl orthosilicate is added,
0.05-2 parts by weight 12mol/L hydrochloric acid, the Lovastatin of 0.01-2 parts by weight initiator and 0.05-20 parts by weight stir evenly
Afterwards, warming-in-water is then added 0.01-0.5 parts by weight of sodium hydroxide, stirs complete to its to initiated polymerization at 30-75 DEG C
After fully dissolved, polymerization reaction time is at least 48h, and the compound wet gel of galapectite-silica is made；
Step 3,0.05-2 parts by weight methacryloxy 12 is added in the above-mentioned compound wet gel of galapectite-silica
Alkyl trimethyl ammonium chloride, after standing, place the product in CO2In supercritical high-pressure extraction device, with CO2It is medium in temperature 30-
Supercritical drying at least 1h is carried out under 60 DEG C and air pressure 5-15MPa, and galapectite-silicon dioxide composite aerogel material can be obtained
Material.
7. galapectite according to claim 6-silicon dioxide composite aerogel material preparation method, it is characterised in that:
In step 1, halloysite nanotubes are 1-15 parts by weight, are added to ultrasonic disperse 1h in the mixed liquor of deionized water and ethyl alcohol,
Sodium styrene sulfonate is 1-15 parts by weight, and poly- divinylsiloxanes are 0.1-2 parts by weight, and initiator is 0.01-0.1 weight
Part, dexamethasone is 0.1-10 parts by weight, is added to after stirring 20-60min in the mixed liquor of deionized water and ethyl alcohol, is added to
In galapectite dispersion liquid, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, the selection when carrying out polymerization reaction
The polyase 13 0-60min at 60-120 DEG C, is then cooled at 15-50 DEG C and polymerize 12-24h, then successively at 80 DEG C, 90 DEG C and 100
It polymerize 2-8h at DEG C respectively.
8. galapectite according to claim 6-silicon dioxide composite aerogel material preparation method, it is characterised in that:
In step 2, into above-mentioned dispersion liquid be added 80-150 parts by weight ethyl orthosilicate, 0.1-1 parts by weight 12mol/L hydrochloric acid,
0.01-1 parts by weight initiator and 0.1-15 parts by weight Lovastatin stir 15-60min, and when carrying out polymerization reaction, selection exists
It polymerize 15-40min at 30-75 DEG C, 0.01-0.2 parts by weight of sodium hydroxide is added, stirring is completely dissolved to it, is then cooled to
It polymerize 20-35h in 20-50 DEG C of water bath with thermostatic control, then successively polymerize 2h respectively at 80 DEG C, 90 DEG C and 100 DEG C.
9. galapectite according to claim 6-silicon dioxide composite aerogel material preparation method, it is characterised in that:
Initiator selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
10. galapectite according to claim 6-silicon dioxide composite aerogel material preparation method, it is characterised in that:
In step 3, methacryloxy dodecyl trimethyl ammonium chloride is 0.1-1 parts by weight, and time of repose 2-6h is super to face
The dry condition in boundary is that supercritical drying 2-4h, preferably 3h are carried out at 33-50 DEG C of temperature and air pressure 7-10MPa.
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