CN109692150A - Mesoporous-micropore galapectite-montmorillonite Composite aerogel material and preparation method thereof - Google Patents
Mesoporous-micropore galapectite-montmorillonite Composite aerogel material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides mesoporous-micropore galapectite-montmorillonite Composite aerogel material and preparation method thereof, galapectite dispersion liquid is obtained after galapectite dispersion liquid is polymerize with the mixed solution of dexamethasone, montmorillonite dispersions are prepared again, it is added after initiator that the reaction was continued after two kinds of dispersion liquids are mixed with gentamicin thereto, obtains galapectite-montmorillonite Composite aerogel material.With gradually increasing for soaking time, the drug gentamicin 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 mesoporous-micropore galapectite-montmorillonite
Aerogel composite 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, name, structure, pattern and the curling mechanism of Zhuan Quanchao galapectite
[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 mesoporous-micropore galapectite-montmorillonite Composite airsetting
Glue material and preparation method thereof uses the doughnut with microcellular structure for raw material, builds three-dimensional aeroge network, utilizes gas
The meso-hole structure of gel and the microcellular structure of fiber, load different pharmaceutical respectively, realize the ladder-like classification release of drug.
The purpose of the present invention is achieved by following technical proposals.
Mesoporous-micropore galapectite-montmorillonite Composite aerogel material and preparation method thereof carries out as steps described below:
Step 1,0.5-15 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 0.5-15 parts by weight of styrene sodium sulfonate, 0.05-2 weight
The poly- divinylsiloxanes of part, 0.01-0.5 parts by weight initiator are measured, 0.05-10 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, above-mentioned solution is added in galapectite dispersion liquid after mixing evenly, 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
Afterwards, it is scattered in 100 parts by weight water, warming-in-water to initiated polymerization at 70-80 DEG C, polymerization reaction time at least 50h is washed
It washs and is dispersed in 100 parts by weight water, obtain the dispersion liquid of step 1；
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 is purchased from Dow corning company.
Step 2, by after 0.05-15 parts by weight montmorillonite drying, dispersed with the montmorillonite that solvent is configured to 0.05-25wt%
Liquid, montmorillonite dispersions mechanical stirring is uniform, after being then sonicated, obtain the dispersion liquid of step 2；
Step 3, by the dispersion liquid of 0.5-15 parts by weight step 1, the dispersion liquid of 0.5-35 parts by weight step 2,0.1-20 weight
It measures the gentamycin solution that part mass fraction is 0.05-20wt% to mix, is scattered in decentralized medium, 0.01-2 is added thereto
Parts by weight initiator, after mixing evenly, warming-in-water to initiated polymerization at 70-90 DEG C, polymerization reaction time at least 37h
Afterwards, place the product in CO2In supercritical high-pressure extraction device, with CO2It is medium at 10-300 DEG C of temperature and air pressure 1-20MPa
Supercritical drying at least 1h is carried out, mesoporous-micropore galapectite-montmorillonite Composite aerogel material can be obtained.
In step 1,1-10 parts by weight halloysite nanotubes are added to ultrasonic disperse in the mixed solution of water and ethyl alcohol
1h, by 1-10 parts by weight of styrene sodium sulfonate, the poly- divinylsiloxanes of 0.1-1 parts by weight, 0.01-0.1 parts by weight initiator,
0.1-5 parts by weight dexamethasone is added in the mixed solution of water and ethyl alcohol, is added to above-mentioned solution after stirring 10-60min
In galapectite dispersion liquid, ultrasonic disperse 30min keeps vacuum 1h after vacuumizing, when carrying out polymerization reaction, selection is at 70-80 DEG C
Water bath condition under polymerize 12-24h in 40-60 DEG C of water bath with thermostatic control after prepolymerization 30-60min, then by it successively 80
DEG C, 90 DEG C, it polymerize 2-8h respectively in 100 DEG C of water bath with thermostatic control.
In step 2, montmorillonite drying condition: 60-180 DEG C of temperature, time 5-20h, after the drying of 0.1-10 parts by weight
Montmorillonite be configured to the montmorillonite dispersions that mass fraction is 0.1-20wt% with solvent, by montmorillonite dispersions at 5-35 DEG C
Under 4-10h, then the ultrasonic treatment 6-15h with 50-300W power stirred with the speed mechanical of 150-400r/min.
In step 3, by the dispersion liquid of 1-10 parts by weight step 1, the dispersion liquid of 1-30 parts by weight step 2 and 0.5-15 weight
It measures the gentamycin solution that part mass fraction is 0.05-15wt% to mix, is scattered in 10-1000 parts by weight decentralized medium, adds
Enter 0.01-1 parts by weight initiator, stirs 1h, selection prepolymerization under 70-90 DEG C of water bath condition when carrying out polymerization reaction
It polymerize 12-24h after 30-60min in 30-50 DEG C of water bath with thermostatic control, then by it successively at 80 DEG C, 90 DEG C, 100 DEG C of constant temperature
It polymerize 2-8h in water-bath respectively, freeze-drying condition is -5 DEG C of temperature -- 108 DEG C, 0-60 DEG C of humidity, vacuum degree 10-50000pa,
Time 2-48h, supercritical drying time are 2-4h, preferably 3h.
Initiator selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
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 mesoporous-micropore galapectite-montmorillonite Composite aerogel material, true by taking out
After empty, washing, poly- divinylsiloxanes are copolymerized with sodium styrene sulfonate, are formed and are formed crosslinking inside halloysite nanotubes
Dexamethasone is supported in halloysite nanotubes by structure, and step 3 makes be located at outside halloysite nanotubes hollow structure poly- two
It polymerize under the action of initiator between vinyl functional group on vinylsiloxane, so that halloysite nanotubes and poly-
Tridimensional network is collectively formed in divinylsiloxanes, and the montmorillonite being added in step 2 is successfully configured to network pore structure,
Above-mentioned tridimensional network and montmorillonite are successfully configured to network pore structure and together form three-dimensional network pore structure, above-mentioned
Three-dimensional network pore structure provides meso-hole structure for mesoporous-micropore galapectite-montmorillonite Composite aerogel material, while will celebrate big
Mycin is 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=-0.959/ln (p/p0), unit nm, while adding adsorbent layer thickness t=0.361 [- 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
10.45nm, another kind are 20.53 μm, are measured through multiple groups, and nanoscale hole is average up to 10-12nm, and micro-meter scale hole is flat
Up to 20-22 μm.It can be seen that material exists simultaneously nanoscale and micro-meter scale hole.
Using the Nanosem430 field emission scanning electron microscope of Dutch Philips to the method for the invention system of utilization
The microscopic appearance of standby composite material is observed, as shown in Figure 2.It can be seen from the figure that montmorillonite layer is successfully configured to
Network pore structure, aperture size is in mesoporous scale.It is overlapped to form three-dimensional netted halloysite nanotubes and is uniformly dispersed in cover and take off
In native 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 celebrating is big
Mycin, 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 celebrating being carried in mesoporous is big
Mycin 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 mesoporous-micropore galapectite-montmorillonite Composite aerogel material N2Adsorption-desorption curve；
Fig. 2 is mesoporous-micropore galapectite-montmorillonite Composite aerogel material electromicroscopic photograph；
Fig. 3 is mesoporous-micropore galapectite-montmorillonite Composite aerogel material release product test curve；
Fig. 4 is mesoporous-micropore galapectite-montmorillonite 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
6g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
Galapectite dispersion liquid, by 10g sodium styrene sulfonate, 0.5g poly- divinylsiloxanes (number-average molecular weight 1000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 4%), 0.6g azodiisobutyronitrile (ABIN),
0.3g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 13min, is added to galapectite dispersion liquid
In, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three times
Afterwards, it after product being washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 56min in 50 DEG C of constant temperature
It polymerize 15 hours in water-bath, after it is successively then polymerize 5h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, by product
It after washing, is scattered in 100g water, obtains dispersion liquid A；11h is dried into 10g montmorillonite at 180 DEG C, then is configured to solvent
Mass fraction is the montmorillonite dispersions of 20wt%；Montmorillonite dispersions are stirred at 30 DEG C with the speed mechanical of 165r/min
4h, then with the ultrasonic treatment 14h of 226W power, obtain dispersion liquid B；By 2g dispersion liquid A, 22g dispersion liquid B, 5.5g mass fraction
It mixes, is scattered in 1000g decentralized medium for the gentamycin solution of 10wt%, is added 0.01g azodiisobutyronitrile (ABIN),
Stirring 1h is placed on prepolymerization 39min under 88 DEG C of water bath condition, then polymerize 19h in 42 DEG C of water bath with thermostatic control, then will
It successively respectively places obtained solution after 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, and place the product in CO2Supercritical, high pressure
In extraction equipment, with CO2Supercritical drying 3h is carried out at 189 DEG C of temperature and air pressure 1MPa for medium, and galapectite/illiteracy can be obtained
The de- multiple dimensioned load medicine aeroge of soil.
Embodiment 2
4g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
Galapectite dispersion liquid, by 1g sodium styrene sulfonate, 0.3g poly- divinylsiloxanes (number-average molecular weight 2000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 3%), 1g dibenzoyl peroxide (BPO), 0.5g
Dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 24min, is added in galapectite dispersion liquid,
Ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, after repeating vacuum step three times,
It after product is washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 45min in 50 DEG C of water bath with thermostatic control
Middle polymerization 24 hours, after it is successively then polymerize 8h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is washed
Afterwards, it is scattered in 100g water, obtains dispersion liquid A；20h is dried into 3.4g montmorillonite at 60 DEG C, then is configured to quality with solvent
Score is the montmorillonite dispersions of 0.1wt%；Montmorillonite dispersions are stirred into 5h at 19 DEG C with the speed mechanical of 293r/min,
The ultrasonic treatment 9h for using 300W power again, obtains dispersion liquid B；It is by 1g dispersion liquid A, 12g dispersion liquid B, 8.6g mass fraction
The gentamycin solution of 0.65wt% mixes, and is scattered in 10g decentralized medium, is added 0.3g dibenzoyl peroxide (BPO), stirs
It mixes 1h and is placed on prepolymerization 60min under 70 DEG C of water bath condition, 23h is then polymerize in 30 DEG C of water bath with thermostatic control, then by it
Obtained solution after 2h is respectively successively placed in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, place the product in CO2Supercritical, high pressure extraction
It takes in device, with CO2Supercritical drying 3h is carried out at 55 DEG C of temperature and air pressure 3MPa for medium, and it is de- that galapectite/illiteracy can be obtained
The multiple dimensioned load medicine aeroge of soil.
Embodiment 3
8g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
Galapectite dispersion liquid, by 4g sodium styrene sulfonate, 0.4g poly- divinylsiloxanes (number-average molecular weight 3000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of mole percent 2.5%), 0.44g azodiisobutyronitrile (ABIN),
5g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 34min, is added to galapectite dispersion liquid
In, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three times
Afterwards, it after product being washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 60min in 50 DEG C of constant temperature
It polymerize 20 hours in water-bath, after it is successively then polymerize 6h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, by product
It after washing, is scattered in 100g water, obtains dispersion liquid A；5h is dried into 2.6g montmorillonite at 95 DEG C, then is configured to matter with solvent
Measure the montmorillonite dispersions that score is 8wt%；Montmorillonite dispersions are stirred into 8h at 25 DEG C with the speed mechanical of 400r/min,
The ultrasonic treatment 6h for using 120W power again, obtains dispersion liquid B；It is by 6g dispersion liquid A, 3g dispersion liquid B, 0.5g mass fraction
The gentamycin solution of 0.05wt% mixes, and is scattered in 562g decentralized medium, is added 0.9g azodiisobutyronitrile (ABIN), stirs
It mixes 1h and is placed on prepolymerization 55min under 71 DEG C of water bath condition, 90h is then polymerize in 32 DEG C of water bath with thermostatic control, then by it
Obtained solution after 2h is respectively successively placed in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, place the product in CO2Supercritical, high pressure extraction
It takes in device, with CO2Supercritical drying 3h is carried out at 16 DEG C of temperature and air pressure 15MPa for medium, and it is de- that galapectite/illiteracy can be obtained
The multiple dimensioned load medicine aeroge of soil.
Embodiment 4
9g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
Galapectite dispersion liquid, by 6g sodium styrene sulfonate, 0.1g poly- divinylsiloxanes (number-average molecular weight 3500, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 1.5%), 0.01g dibenzoyl peroxide
(BPO), 0.22g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 60min, is added to Ai Luo
In stone dispersion liquid, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, is then restored to normal pressure, and repetition vacuumizes
Step three times after, after product is washed, be scattered in 100g water, be placed under 75 DEG C of water bath condition after prepolymerization 55min 50
DEG C water bath with thermostatic control in polymerize 12 hours, it is successively then polymerize 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control respectively
Afterwards, it after product being washed, is scattered in 100g water, obtains dispersion liquid A；By 0.1g montmorillonite at 144 DEG C dry 6h, then with molten
Agent is configured to the montmorillonite dispersions that mass fraction is 4.6wt%；By montmorillonite dispersions at 5 DEG C with the speed of 256r/min
Mechanical stirring 10h, then with the ultrasonic treatment 15h of 260W power, obtain dispersion liquid B；By 5.3g dispersion liquid A, 1g dispersion liquid B,
The gentamycin solution that 0.89g mass fraction is 15wt% mixes, and is scattered in 352g decentralized medium, and 0.06g peroxidating is added
Dibenzoyl (BPO), stirring 1h is placed on prepolymerization 53min under 90 DEG C of water bath condition, then in 50 DEG C of water bath with thermostatic control
It polymerize 16h, it is successively respectively then placed into obtained solution after 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is set
In CO2In supercritical high-pressure extraction device, with CO2Supercritical drying 3h is carried out at 300 DEG C of temperature and air pressure 20MPa for medium,
The multiple dimensioned load medicine aeroge of galapectite/montmorillonite can be obtained.
Embodiment 5
1g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
Galapectite dispersion liquid, by 5g sodium styrene sulfonate, (number-average molecular weight 500, contents of ethylene rubs the poly- divinylsiloxanes of 0.7g
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of your percentage 5%), 0.7g azodiisobutyronitrile (ABIN), 0.1g
Dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 29min, is added in galapectite dispersion liquid,
Ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, after repeating vacuum step three times,
It after product is washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 31min in 50 DEG C of water bath with thermostatic control
Middle polymerization 13 hours, after it is successively then polymerize 4h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is washed
Afterwards, it is scattered in 100g water, obtains dispersion liquid A；18h is dried into 6.5g montmorillonite at 120 DEG C, then is configured to quality with solvent
Score is the montmorillonite dispersions of 18wt%；Montmorillonite dispersions are stirred into 3h at 35 DEG C with the speed mechanical of 332r/min,
The ultrasonic treatment 8h for using 250W power again, obtains dispersion liquid B；It is by 10g dispersion liquid A, 9g dispersion liquid B, 15g mass fraction
The gentamycin solution of 5.2wt% mixes, and is scattered in 152g decentralized medium, is added 1g azodiisobutyronitrile (ABIN), stirring
1h is placed on prepolymerization 30min under 76 DEG C of water bath condition, and 15h is then polymerize in 48 DEG C of water bath with thermostatic control, then by its according to
Secondary respectively to place obtained solution after 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, place the product in CO2Supercritical, high pressure extraction
In device, with CO2Supercritical drying 3h is carried out at 225 DEG C of temperature and air pressure 4MPa for medium, and galapectite/montmorillonite can be obtained
Multiple dimensioned load medicine aeroge.
Embodiment 6
10g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
Galapectite dispersion liquid, by 8g sodium styrene sulfonate, (number-average molecular weight 5000, contents of ethylene rubs the poly- divinylsiloxanes of 1g
The poly dimethyl divinylsiloxanes of the amino list sealing end of your percentage 0.1%), 0.5g dibenzoyl peroxide (BPO),
3.5g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 10min, is added to galapectite dispersion liquid
In, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three times
Afterwards, it after product being washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 30min in 50 DEG C of constant temperature
It polymerize in water-bath 21 hours, after it is successively then distinguished polyase 13 h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, by product
It after washing, is scattered in 100g water, obtains dispersion liquid A；15h is dried into 3g montmorillonite at 66 DEG C, then is configured to matter with solvent
Measure the montmorillonite dispersions that score is 0.5wt%；Montmorillonite dispersions are stirred at 6 DEG C with the speed mechanical of 150r/min
9h, then with the ultrasonic treatment 12h of 50W power, obtain dispersion liquid B；It is by 9g dispersion liquid A, 30g dispersion liquid B, 2.6g mass fraction
The gentamycin solution of 13wt% mixes, and is scattered in 998g decentralized medium, is added 0.65g dibenzoyl peroxide (BPO), stirs
It mixes 1h and is placed on prepolymerization 44min under 85 DEG C of water bath condition, 28h is then polymerize in 35 DEG C of water bath with thermostatic control, then by it
Obtained solution after 2h is respectively successively placed in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, place the product in CO2Supercritical, high pressure extraction
It takes in device, with CO2Supercritical drying 3h is carried out at 10 DEG C of temperature and air pressure 10MPa for medium, and it is de- that galapectite/illiteracy can be obtained
The multiple dimensioned load medicine aeroge of soil.
Embodiment 7
0.5g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
To galapectite dispersion liquid, by 0.5g sodium styrene sulfonate, 0.05g poly- divinylsiloxanes (number-average molecular weight 4000, vinyl
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of content mole percent 1.5%), 0.01g azodiisobutyronitrile
(ABIN), 0.05g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 34min, is added to Ai Luo
In stone dispersion liquid, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, is then restored to normal pressure, and repetition vacuumizes
Step three times after, after product is washed, be scattered in 100g water, be placed under 70 DEG C of water bath condition after prepolymerization 60min 40
DEG C water bath with thermostatic control in polymerize 20 hours, it is successively then polymerize 6h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control respectively
Afterwards, it after product being washed, is scattered in 100g water, obtains dispersion liquid A；By 0.05g montmorillonite at 95 DEG C dry 5h, then with molten
Agent is configured to the montmorillonite dispersions that mass fraction is 0.05wt%；By montmorillonite dispersions with the speed of 400r/min at 25 DEG C
Mechanical stirring 8h is spent, then with the ultrasonic treatment 6h of 120W power, obtains dispersion liquid B；By 0.5g dispersion liquid A, 0.5g dispersion liquid B,
The gentamycin solution that 0.1g mass fraction is 0.05wt% mixes, and is scattered in 562g decentralized medium, and 0.01g azo two is added
Isobutyronitrile (ABIN), stirring 1h are placed on prepolymerization 55min under 71 DEG C of water bath condition, then gather in 32 DEG C of water bath with thermostatic control
90h is closed, it is successively respectively then placed into obtained solution after 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, place the product in
CO2In supercritical high-pressure extraction device, with CO2Supercritical drying 4h is carried out at 10 DEG C of temperature and air pressure 1MPa for medium, can be obtained
To the multiple dimensioned load medicine aeroge of galapectite/montmorillonite.
Embodiment 8
15g halloysite nanotubes are added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, ultrasonic disperse 1h is obtained
Galapectite dispersion liquid, by 15g sodium styrene sulfonate, (number-average molecular weight 3200, contents of ethylene rubs the poly- divinylsiloxanes of 2g
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of your percentage 2.4%), 0.5g dibenzoyl peroxide (BPO),
10g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 29min, is added to galapectite dispersion liquid
In, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three times
Afterwards, it after product being washed, is scattered in 100g water, is placed under 80 DEG C of water bath condition after prepolymerization 31min in 60 DEG C of constant temperature
It polymerize 13 hours in water-bath, after it is successively then polymerize 4h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, by product
It after washing, is scattered in 100g water, obtains dispersion liquid A；18h is dried into 15g montmorillonite at 120 DEG C, then is configured to solvent
Mass fraction is the montmorillonite dispersions of 25wt%；Montmorillonite dispersions are stirred at 35 DEG C with the speed mechanical of 332r/min
3h, then with the ultrasonic treatment 8h of 250W power, obtain dispersion liquid B；It is by 15g dispersion liquid A, 35g dispersion liquid B, 20g mass fraction
The gentamycin solution of 20wt% mixes, and is scattered in 152g decentralized medium, is added 2g dibenzoyl peroxide (BPO), stirring
1h is placed on prepolymerization 30min under 76 DEG C of water bath condition, and 15h is then polymerize in 48 DEG C of water bath with thermostatic control, then by its according to
Secondary respectively to place obtained solution after 2h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, place the product in CO2Supercritical, high pressure extraction
In device, with CO2Supercritical drying 2h is carried out at 285 DEG C of temperature and air pressure 12MPa for medium, and it is de- that galapectite/illiteracy can be obtained
The multiple dimensioned load medicine aeroge of soil.
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. mesoporous-micropore galapectite-montmorillonite Composite aerogel material, it is characterised in that: galapectite-montmorillonite Composite aeroge
Material average specific surface area is 600-608m2g-1, exist simultaneously in galapectite-montmorillonite Composite aerogel material nanoscale and
Micro-meter scale hole, nanoscale hole average out to 10-12nm, 20-22 μm of average out to of micro-meter scale hole, as steps described below
It carries out:
Step 1,0.5-15 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 0.5-15 parts by weight of styrene sodium sulfonate, 0.05-2 parts by weight
Poly- divinylsiloxanes, 0.01-0.5 parts by weight initiator, 0.05-10 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, above-mentioned solution is added in galapectite dispersion liquid after mixing evenly, ultrasound point
After dissipating uniformly, vacuum is kept after vacuumizing, and is then restored to normal pressure, after repeating vacuum step three times, after product is washed, point
It dissipates in 100 parts by weight water, warming-in-water to initiated polymerization at 70-80 DEG C, polymerization reaction time at least 50h, washing point
It is dissipated in 100 parts by weight water, obtains the dispersion liquid 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, by after 0.05-15 parts by weight montmorillonite drying, the montmorillonite dispersions of 0.05-25wt% are configured to solvent,
Montmorillonite dispersions mechanical stirring is uniform, after being then sonicated, obtain the dispersion liquid of step 2；
Step 3, by the dispersion liquid of 0.5-15 parts by weight step 1, the dispersion liquid of 0.5-35 parts by weight step 2,0.1-20 parts by weight
The gentamycin solution that mass fraction is 0.05-20wt% mixes, and is scattered in decentralized medium, and 0.01-2 weight is added thereto
Part initiator, after mixing evenly, warming-in-water to initiated polymerization at 70-90 DEG C will after polymerization reaction time at least 37h
Product is placed in CO2In supercritical high-pressure extraction device, with CO2Surpassed at 10-300 DEG C of temperature and air pressure 1-20MPa for medium
Mesoporous-micropore galapectite-montmorillonite Composite aerogel material can be obtained in critical drying at least 1h；
Positive charge is had on the inside of halloysite nanotubes tube wall, and negative electrical charge, the styrene sulfonic acid being added in step 1 are had on the outside of tube wall
Sodium has negative electrical charge, and sodium styrene sulfonate is adsorbed on halloysite nanotubes inner wall by electrostatic interaction, while adding in step 1
Poly- divinylsiloxanes, initiator and the dexamethasone entered is also dispersed in halloysite nanotubes hollow structure, and galapectite is received
Mitron hollow structure provides microcellular structure for mesoporous-micropore galapectite-montmorillonite Composite aerogel material, through vacuumizing,
After washing, poly- divinylsiloxanes are copolymerized with sodium styrene sulfonate, are formed inside halloysite nanotubes and are formed crosslinking knot
Dexamethasone is supported in halloysite nanotubes by structure, and step 3 makes the poly- diethyl being located at outside halloysite nanotubes hollow structure
It polymerize under the action of initiator between vinyl functional group in alkenyl siloxane, so that halloysite nanotubes and poly- two
Tridimensional network is collectively formed in vinylsiloxane, and the montmorillonite being added in step 2 is successfully configured to network pore structure, on
It states tridimensional network and montmorillonite is successfully configured to network pore structure and together forms three-dimensional network pore structure, above-mentioned three
Dimension network pore structure provides meso-hole structure for mesoporous-micropore galapectite-montmorillonite Composite aerogel material, while will celebrate big mould
Element is supported in meso-hole structure.
2. mesoporous-micropore galapectite-montmorillonite Composite aerogel material according to claim 1, it is characterised in that: in step
In rapid 1,1-10 parts by weight halloysite nanotubes are added to ultrasonic disperse 1h in the mixed solution of water and ethyl alcohol, by 1-10 weight
Part sodium styrene sulfonate, the poly- divinylsiloxanes of 0.1-1 parts by weight, 0.01-0.1 parts by weight initiator, 0.1-5 parts by weight
Sai meter Song is added in the mixed solution of water and ethyl alcohol, and above-mentioned solution is added to galapectite dispersion liquid after stirring 10-60min
In, ultrasonic disperse 30min keeps vacuum 1h after vacuumizing, when carrying out polymerization reaction, selection is under 70-80 DEG C of water bath condition
It polymerize 12-24h after prepolymerization 30-60min in 40-60 DEG C of water bath with thermostatic control, then by it successively at 80 DEG C, 90 DEG C, 100 DEG C
Water bath with thermostatic control in polymerize 2-8h respectively.
3. mesoporous-micropore galapectite-montmorillonite Composite aerogel material according to claim 1, it is characterised in that: in step
In rapid 2, montmorillonite drying condition: 60-180 DEG C of temperature, time 5-20h, by montmorillonite of the 0.1-10 parts by weight after dry with molten
Agent is configured to the montmorillonite dispersions that mass fraction is 0.1-20wt%, by montmorillonite dispersions with 150- at 5-35 DEG C
The speed mechanical of 400r/min stirs 4-10h, then the ultrasonic treatment 6-15h with 50-300W power.
4. mesoporous-micropore galapectite-montmorillonite Composite aerogel material according to claim 1, it is characterised in that: in step
In rapid 3, by the dispersion liquid of 1-10 parts by weight step 1, the dispersion liquid of 1-30 parts by weight step 2 and 0.5-15 parts by weight mass fraction
It mixes, is scattered in 10-1000 parts by weight decentralized medium for the gentamycin solution of 0.05-15wt%, 0.01-1 weight is added
Part initiator stirs 1h, when carrying out polymerization reaction selection under 70-90 DEG C of water bath condition after prepolymerization 30-60min
It polymerize 12-24h in 30-50 DEG C of water bath with thermostatic control, then successively gathers it respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control
2-8h is closed, freeze-drying condition is -5 DEG C of temperature -- 108 DEG C, 0-60 DEG C of humidity, vacuum degree 10-50000pa, time 2-48h, surpass
Critical drying time is 2-4h, preferably 3h.
5. mesoporous-micropore galapectite-montmorillonite Composite aerogel material according to claim 1, it is characterised in that: cause
Agent selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
6. mesoporous-micropore galapectite-montmorillonite Composite aerogel material preparation method, it is characterised in that: as steps described below
It carries out:
Step 1,0.5-15 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 0.5-15 parts by weight of styrene sodium sulfonate, 0.05-2 parts by weight
Poly- divinylsiloxanes, 0.01-0.5 parts by weight initiator, 0.05-10 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, above-mentioned solution is added in galapectite dispersion liquid after mixing evenly, ultrasound point
After dissipating uniformly, vacuum is kept after vacuumizing, and is then restored to normal pressure, after repeating vacuum step three times, after product is washed, point
It dissipates in 100 parts by weight water, warming-in-water to initiated polymerization at 70-80 DEG C, polymerization reaction time at least 50h, washing point
It is dissipated in 100 parts by weight water, obtains the dispersion liquid 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, by after 0.05-15 parts by weight montmorillonite drying, the montmorillonite dispersions of 0.05-25wt% are configured to solvent,
Montmorillonite dispersions mechanical stirring is uniform, after being then sonicated, obtain the dispersion liquid of step 2；
Step 3, by the dispersion liquid of 0.5-15 parts by weight step 1, the dispersion liquid of 0.5-35 parts by weight step 2,0.1-20 parts by weight
The gentamycin solution that mass fraction is 0.05-20wt% mixes, and is scattered in decentralized medium, and 0.01-2 weight is added thereto
Part initiator, after mixing evenly, warming-in-water to initiated polymerization at 70-90 DEG C will after polymerization reaction time at least 37h
Product is placed in CO2In supercritical high-pressure extraction device, with CO2Surpassed at 10-300 DEG C of temperature and air pressure 1-20MPa for medium
Mesoporous-micropore galapectite-montmorillonite Composite aerogel material can be obtained in critical drying at least 1h；
Positive charge is had on the inside of halloysite nanotubes tube wall, and negative electrical charge, the styrene sulfonic acid being added in step 1 are had on the outside of tube wall
Sodium has negative electrical charge, and sodium styrene sulfonate is adsorbed on halloysite nanotubes inner wall by electrostatic interaction, while adding in step 1
Poly- divinylsiloxanes, initiator and the dexamethasone entered is also dispersed in halloysite nanotubes hollow structure, and galapectite is received
Mitron hollow structure provides microcellular structure for mesoporous-micropore galapectite-montmorillonite Composite aerogel material, through vacuumizing,
After washing, poly- divinylsiloxanes are copolymerized with sodium styrene sulfonate, are formed inside halloysite nanotubes and are formed crosslinking knot
Dexamethasone is supported in halloysite nanotubes by structure, and step 3 makes the poly- diethyl being located at outside halloysite nanotubes hollow structure
It polymerize under the action of initiator between vinyl functional group in alkenyl siloxane, so that halloysite nanotubes and poly- two
Tridimensional network is collectively formed in vinylsiloxane, and the montmorillonite being added in step 2 is successfully configured to network pore structure, on
It states tridimensional network and montmorillonite is successfully configured to network pore structure and together forms three-dimensional network pore structure, above-mentioned three
Dimension network pore structure provides meso-hole structure for mesoporous-micropore galapectite-montmorillonite Composite aerogel material, while will celebrate big mould
Element is supported in meso-hole structure.
7. mesoporous-micropore galapectite-montmorillonite Composite aerogel material preparation method according to claim 6, special
Sign is: in step 1,1-10 parts by weight halloysite nanotubes being added to ultrasonic disperse in the mixed solution of water and ethyl alcohol
1h, by 1-10 parts by weight of styrene sodium sulfonate, the poly- divinylsiloxanes of 0.1-1 parts by weight, 0.01-0.1 parts by weight initiator,
0.1-5 parts by weight dexamethasone is added in the mixed solution of water and ethyl alcohol, is added to above-mentioned solution after stirring 10-60min
In galapectite dispersion liquid, ultrasonic disperse 30min keeps vacuum 1h after vacuumizing, when carrying out polymerization reaction, selection is at 70-80 DEG C
Water bath condition under polymerize 12-24h in 40-60 DEG C of water bath with thermostatic control after prepolymerization 30-60min, then by it successively 80
DEG C, 90 DEG C, it polymerize 2-8h respectively in 100 DEG C of water bath with thermostatic control.
8. mesoporous-micropore galapectite-montmorillonite Composite aerogel material preparation method according to claim 6, special
Sign is: in step 2, montmorillonite drying condition: 60-180 DEG C of temperature, time 5-20h, after the drying of 0.1-10 parts by weight
Montmorillonite is configured to the montmorillonite dispersions that mass fraction is 0.1-20wt% with solvent, by montmorillonite dispersions at 5-35 DEG C
4-10h, then the ultrasonic treatment 6-15h with 50-300W power are stirred with the speed mechanical of 150-400r/min.
9. mesoporous-micropore galapectite-montmorillonite Composite aerogel material preparation method according to claim 6, special
Sign is: in step 3, by the dispersion liquid of 1-10 parts by weight step 1, the dispersion liquid of 1-30 parts by weight step 2 and 0.5-15 weight
It measures the gentamycin solution that part mass fraction is 0.05-15wt% to mix, is scattered in 10-1000 parts by weight decentralized medium, adds
Enter 0.01-1 parts by weight initiator, stirs 1h, selection prepolymerization under 70-90 DEG C of water bath condition when carrying out polymerization reaction
It polymerize 12-24h after 30-60min in 30-50 DEG C of water bath with thermostatic control, then by it successively at 80 DEG C, 90 DEG C, 100 DEG C of constant temperature
It polymerize 2-8h in water-bath respectively, freeze-drying condition is -5 DEG C of temperature -- 108 DEG C, 0-60 DEG C of humidity, vacuum degree 10-50000pa,
Time 2-48h, supercritical drying time are 2-4h, preferably 3h.
10. mesoporous-micropore galapectite-montmorillonite Composite aerogel material preparation method according to claim 6, special
Sign is: initiator selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520113A (en) * | 2012-07-03 | 2014-01-22 | 中国科学院兰州化学物理研究所 | Halloysite nano composite gel microspheres and preparation method thereof |
| CN105565774A (en) * | 2015-05-11 | 2016-05-11 | 天津城建大学 | High-strength high-thermal-insulation silica aerogel and preparation method thereof |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520113A (en) * | 2012-07-03 | 2014-01-22 | 中国科学院兰州化学物理研究所 | Halloysite nano composite gel microspheres and preparation method thereof |
| CN105565774A (en) * | 2015-05-11 | 2016-05-11 | 天津城建大学 | High-strength high-thermal-insulation silica aerogel and preparation method thereof |
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