CN109985580A - Mesoporous-micropore carbon nanotube-galapectite aerogel composite and preparation method thereof - Google Patents
Mesoporous-micropore carbon nanotube-galapectite aerogel composite and preparation method thereof Download PDFInfo
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Abstract
The present invention provides mesoporous-micropore carbon nanotube-galapectite aerogel composite and preparation method thereof, galapectite dispersion liquid is obtained after galapectite dispersion liquid is polymerize with the mixed solution of dexamethasone, the wet gel of lauryl sodium sulfate and carbon nanotube is prepared again, it is added after initiator and gentamicin that the reaction was continued after dispersion liquid is mixed with wet gel thereto, obtains mesoporous-micropore carbon nanotube-galapectite aerogel composite.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 the mesoporous-micropore carbon nanotube-Ai Luo of one kind
Stone 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 carbon nanotube-compound gas of galapectite
Gel rubber material and preparation method thereof uses the doughnut with microcellular structure for raw material, builds three-dimensional aeroge network, utilizes
The meso-hole structure of aeroge 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 carbon nanotube-galapectite aerogel composite 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
Sound is uniformly dispersed, and vacuum is kept after vacuumizing, and is then restored to normal pressure, after repeating vacuum step three times, after product is washed,
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, washs
It is dispersed 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 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 2,0.5-15 parts by weight lauryl sodium sulfate is taken to be added in 100 parts by weight water, after sonic oscillation, thereto
The carbon nanotube of 0.5-15 parts by weight is added, after ultrasonic disperse is uniform, vacuum is kept after vacuumizing, is then restored to normal pressure, weight
Multiple vacuum step three times, obtains the wet gel of step 2；
Step 3, the dispersion liquid of 0.5-15 parts by weight step 1 is mixed with the wet gel of 0.5-25 parts by weight step 2, Xiang Qi
Middle addition 0.01-2 parts by weight initiator, 0.01-10 parts by weight gentamicin, after ultrasonic disperse is uniform, warming-in-water to 70-80
Initiated polymerization at DEG C after polymerization reaction time at least 50h, product is freeze-dried, drying time at least 2h is situated between
Hole-micropore carbon nanotube-galapectite aerogel composite.
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 2,1-10 parts by weight lauryl sodium sulfate is added to the water, after sonic oscillation 2-48h, thereto plus
Enter the carbon nanotube of 1-10 parts by weight, after the uniform 1-24h of ultrasonic disperse, vacuum 1h is kept after vacuumizing.
In step 3, the dispersion liquid of 1-10 parts by weight step 1 is mixed with the wet gel of 1-20 parts by weight step 2, Xiang Qi
Middle addition 0.01-1 parts by weight initiator, 0.05-5 parts by weight gentamicin, after ultrasonic disperse is uniform, when carrying out polymerization reaction
Selection polymerize 12-24h in 40-60 DEG C of water bath with thermostatic control after prepolymerization 30-60min under 70-80 DEG C of water bath condition, then
It is successively polymerize to 2-8h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, 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.
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 carbon nanotube-galapectite aerogel composite, by taking out
After vacuum, washing, poly- divinylsiloxanes are copolymerized with sodium styrene sulfonate, are formed to be formed inside halloysite nanotubes and be handed over
It is coupled structure, dexamethasone is supported in halloysite nanotubes, step 3 to be located at poly- outside halloysite nanotubes hollow structure
Polymerize under the action of initiator between vinyl functional group in divinylsiloxanes so that halloysite nanotubes and
Tridimensional network is collectively formed in poly- divinylsiloxanes, and the carbon nanotube being added in step 2 is successfully configured to network pore
Structure, above-mentioned tridimensional network and carbon nanotube are successfully configured to network pore structure and together form three-dimensional network hole knot
Structure, above-mentioned three-dimensional network pore structure provide meso-hole structure for mesoporous-micropore carbon nanotube-galapectite aerogel composite,
Gentamicin is supported in meso-hole structure simultaneously.
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=-0.961/ln (p/p0), unit nm, while adding adsorbent layer thickness t=0.364 [- 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
10.43nm, another kind are 20.51 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 carbon nano-tube fibre successfully constructs
For network pore structure, aperture size is in mesoporous scale.It is overlapped to form three-dimensional netted halloysite nanotubes and is uniformly dispersed in carbon
In nanotube 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 carbon nanotube-galapectite aerogel composite N2Adsorption-desorption curve；
Fig. 2 is mesoporous-micropore carbon nanotube-galapectite aerogel composite electromicroscopic photograph；
Fig. 3 is mesoporous-micropore carbon nanotube-galapectite aerogel composite release product test curve；
Fig. 4 is mesoporous-micropore carbon nanotube-galapectite aerogel composite carrying medicament release profiles.
Specific embodiment
Below by specific embodiment, further description of the technical solution of the present invention.
Embodiment 1
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 2g sodium styrene sulfonate, 0.2g poly- divinylsiloxanes (number-average molecular weight 3500, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of mole percent 2.5%), 0.01g azodiisobutyronitrile (ABIN),
3g 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 35min in 50 DEG C of constant temperature
It polymerize 12 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 galapectite and carry medicine dispersion liquid；It takes 1g lauryl sodium sulfate to be added in 100g water, surpasses
After sound oscillation 2h, the carbon nanotube of 4g is added, ultrasonic disperse 1h obtains dispersion liquid；1h is kept after above-mentioned dispersion liquid is vacuumized,
It is then restored to normal pressure, repeats vacuum step three times, carbon nanotube is obtained and carries medicine wet gel；2g galapectite is carried into medicine dispersion liquid
Medicine wet gel is carried with 1g carbon nanotube to mix, is added 0.5g azodiisobutyronitrile (ABIN), 0.05g gentamicin, then ultrasound point
Dissipate 2h, be placed under 75 DEG C of water bath condition after prepolymerization 30min in 50 DEG C of water bath with thermostatic control and polymerize 14 hours, then by its according to
It is secondary polymerize 4h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control after, product is freeze-dried, cryogenic temperature be -5 DEG C, do
Eliminating dampness degree is 0 DEG C, and dry vacuum degree is generally 2000pa, and drying time is generally 2 hours, and it is more to obtain carbon nanotube/galapectite
Scale carries medicine aeroge.
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, 0.5g poly- divinylsiloxanes (number-average molecular weight 4000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 1.5%), 0.04g azodiisobutyronitrile (ABIN),
4g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 30min, 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 14 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 galapectite and carry medicine dispersion liquid；It takes 2g lauryl sodium sulfate to be added in 100g water, surpasses
After sound oscillation 48h, the carbon nanotube of 10g is added, ultrasonic disperse 4h obtains dispersion liquid；It is kept after above-mentioned dispersion liquid is vacuumized
1h is then restored to normal pressure, repeats vacuum step three times, obtains carbon nanotube and carries medicine wet gel；4g galapectite is carried into medicine point
Dispersion liquid carries medicine wet gel with 5g carbon nanotube and mixes, and is added 0.01g azodiisobutyronitrile (ABIN), 1g gentamicin, then ultrasound
Disperse 10h, be placed under 75 DEG C of water bath condition after prepolymerization 40min and polymerize 12 hours in 50 DEG C of water bath with thermostatic control, then will
After it successively polymerize 6h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is freeze-dried, cryogenic temperature is -108
DEG C, dry humidity is 20 DEG C, and dry vacuum degree is generally 10pa, and drying time is generally 48 hours, obtains carbon nanotube/Ai Luo
The multiple dimensioned load medicine aeroge of stone.
Embodiment 3
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 6g sodium styrene sulfonate, 0.1g poly- divinylsiloxanes (number-average molecular weight 2500, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 1.5%), 0.08g azodiisobutyronitrile (ABIN),
5g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 60min, 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 40min in 50 DEG C of constant temperature
It polymerize in water-bath 16 hours, after it is successively then distinguished polymerase 17 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 galapectite and carry medicine dispersion liquid；It takes 10g lauryl sodium sulfate to be added in 100g water, surpasses
After sound oscillation for 24 hours, the carbon nanotube of 1g is added, ultrasonic disperse 10h obtains dispersion liquid；It is kept after above-mentioned dispersion liquid is vacuumized
1h is then restored to normal pressure, repeats vacuum step three times, obtains carbon nanotube and carries medicine wet gel；1g galapectite is carried into medicine point
Dispersion liquid carries medicine wet gel with 8g carbon nanotube and mixes, and is added 0.2g azodiisobutyronitrile (ABIN), 2g gentamicin, then ultrasound point
Dissipate 1h, be placed under 75 DEG C of water bath condition after prepolymerization 45min in 50 DEG C of water bath with thermostatic control and polymerize 18 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, product is freeze-dried, cryogenic temperature be -40 DEG C, do
Eliminating dampness degree is 30 DEG C, and dry vacuum degree is generally 4000pa, and drying time is generally 10 hours, obtains carbon nanotube/galapectite
Multiple dimensioned load medicine aeroge.
Embodiment 4
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 8g sodium styrene sulfonate, (number-average molecular weight 2000, contents of ethylene rubs the poly- divinylsiloxanes of 1g
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of your percentage 3%), 0.1g azodiisobutyronitrile (ABIN), 2g
Sai meter Song is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 40min, is added in galapectite dispersion liquid, is surpassed
Sound disperses 30min, and 1h is kept after above-mentioned mixed liquor is vacuumized, and is then restored to normal pressure, will after repeating vacuum step three times
After product washing, it is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 60min in 50 DEG C of water bath with thermostatic control
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 galapectite and carry medicine dispersion liquid；8g lauryl sodium sulfate is taken to be added in 100g water, ultrasound vibration
After swinging 30h, the carbon nanotube of 6g is added, ultrasonic disperse for 24 hours, obtains dispersion liquid；1h is kept after above-mentioned dispersion liquid is vacuumized, with
After be restored to normal pressure, repeat vacuum step three times, obtain carbon nanotube and carry medicine wet gel；By 6g galapectite carry medicine dispersion liquid with
20g carbon nanotube carries the mixing of medicine wet gel, is added 0.8g azodiisobutyronitrile (ABIN), 3g gentamicin, re-ultrasonic dispersion 4h,
It is placed under 75 DEG C of water bath condition after prepolymerization 60min and polymerize 16 hours in 50 DEG C of water bath with thermostatic control, then it successively exists
80 DEG C, 90 DEG C, after polymerizeing 2h respectively in 100 DEG C of water bath with thermostatic control, product is freeze-dried, cryogenic temperature is -80 DEG C, and drying is wet
Degree is 40 DEG C, and dry vacuum degree is generally 1000pa, and drying time is generally 20 hours, obtains the more rulers of carbon nanotube/galapectite
Degree carries medicine aeroge.
Embodiment 5
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 10g sodium styrene sulfonate, 0.7g poly- divinylsiloxanes (number-average molecular weight 3000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 2%), 0.06g dibenzoyl peroxide (BPO),
1g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 50min, 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 45min in 50 DEG C of constant temperature
It polymerize 18 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 galapectite and carry medicine dispersion liquid；It takes 6g lauryl sodium sulfate to be added in 100g water, surpasses
After sound oscillation 35h, the carbon nanotube of 8g is added, ultrasonic disperse 20h obtains dispersion liquid；It is kept after above-mentioned dispersion liquid is vacuumized
1h is then restored to normal pressure, repeats vacuum step three times, obtains carbon nanotube and carries medicine wet gel；8g galapectite is carried into medicine point
Dispersion liquid carries medicine wet gel with 12g carbon nanotube and mixes, and is added 1g dibenzoyl peroxide (BPO), 4g gentamicin, then ultrasound point
Dissipate 6h, be placed under 75 DEG C of water bath condition after prepolymerization 50min in 50 DEG C of water bath with thermostatic control and polymerize 20 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, product is freeze-dried, cryogenic temperature be -60 DEG C, do
Eliminating dampness degree is 50 DEG C, and dry vacuum degree is generally 50000pa, and drying time is generally 30 hours, obtains carbon nanotube/galapectite
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 7g sodium styrene sulfonate, 0.9g poly- divinylsiloxanes (number-average molecular weight 1000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 4%), 0.07g dibenzoyl peroxide (BPO),
0.1g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 20min, 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 50min in 50 DEG C of constant temperature
It polymerize 20 hours in water-bath, after it is successively then polymerize 2h 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 galapectite and carry medicine dispersion liquid；It takes 5g lauryl sodium sulfate to be added in 100g water, surpasses
After sound oscillation 40h, the carbon nanotube of 5g is added, ultrasonic disperse 15h obtains dispersion liquid；It is kept after above-mentioned dispersion liquid is vacuumized
1h is then restored to normal pressure, repeats vacuum step three times, obtains carbon nanotube and carries medicine wet gel；10g galapectite is carried into medicine point
Dispersion liquid carries medicine wet gel with 16g carbon nanotube and mixes, and is added 0.6g dibenzoyl peroxide (BPO), 5g gentamicin, then ultrasound
Disperse 8h, is placed under 75 DEG C of water bath condition after prepolymerization 55min and polymerize 24 hours in 50 DEG C of water bath with thermostatic control, then by it
After successively distinguishing polymerase 17 h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is freeze-dried, cryogenic temperature is -95 DEG C,
Dry humidity is 60 DEG C, and dry vacuum degree is generally 3000pa, and drying time is generally 40 hours, obtains carbon nanotube/Ai Luo
The multiple dimensioned load medicine aeroge of stone.
Embodiment 7
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 500, contents of ethylene rubs the poly- divinylsiloxanes of 2g
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of your percentage 5%), 0.5g dibenzoyl peroxide (BPO), 10g
Dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 30min, 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 70 DEG C of water bath condition after prepolymerization 30min in 40 DEG C of water bath with thermostatic control
Middle polymerization 14 hours, after it is successively then polymerize 6h 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 galapectite and carry medicine dispersion liquid；15g lauryl sodium sulfate is taken to be added in 100g water, ultrasound vibration
After swinging 48h, the carbon nanotube of 15g is added, ultrasonic disperse 4h obtains dispersion liquid；1h is kept after above-mentioned dispersion liquid is vacuumized, with
After be restored to normal pressure, repeat vacuum step three times, obtain carbon nanotube and carry medicine wet gel；15g galapectite is carried into medicine dispersion liquid
Medicine wet gel is carried with 25g carbon nanotube to mix, and is added 2g dibenzoyl peroxide (BPO), 10g gentamicin, re-ultrasonic dispersion
10h is placed under 70 DEG C of water bath condition after prepolymerization 40min in 40 DEG C of water bath with thermostatic control and polymerize 12 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, product is freeze-dried, cryogenic temperature be -108 DEG C,
Dry humidity is 20 DEG C, and dry vacuum degree is generally 10pa, and drying time is generally 48 hours, obtains carbon nanotube/galapectite
Multiple dimensioned load medicine aeroge.
Embodiment 8
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 5000, vinyl
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of content mole percent 0.1%), 0.01g dibenzoyl peroxide
(BPO), 0.05g dexamethasone is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 50min, 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 80 DEG C of water bath condition after prepolymerization 45min 60
DEG C water bath with thermostatic control in polymerize 18 hours, it is successively then polymerize 5h 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 galapectite and carry medicine dispersion liquid；0.5g lauryl sodium sulfate is taken to be added
In 100g water, after sonic oscillation 35h, the carbon nanotube of 0.5g is added, ultrasonic disperse 20h obtains dispersion liquid；By above-mentioned dispersion liquid
1h is kept after vacuumizing, is then restored to normal pressure, repeats vacuum step three times, is obtained carbon nanotube and is carried medicine wet gel；It will
0.5g galapectite carries medicine dispersion liquid and mixes with 0.5g carbon nanotube load medicine wet gel, and 0.01g dibenzoyl peroxide is added
(BPO), 0.01g gentamicin, re-ultrasonic dispersion 6h are placed under 80 DEG C of water bath condition after prepolymerization 50min in 60 DEG C of perseverance
It polymerize 20 hours in tepidarium, after it is successively then polymerize 5h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, will produces
Object freeze-drying, cryogenic temperature are -60 DEG C, and dry humidity is 50 DEG C, and dry vacuum degree is generally 50000pa, drying time one
As be 30 hours, obtain the multiple dimensioned load medicine aeroge of carbon nanotube/galapectite.
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 carbon nanotube-galapectite aerogel composite, it is characterised in that: the compound gas of carbon nanotube-galapectite
Gel rubber material average specific surface area is 600-608m2g-1, nanometer is existed simultaneously in carbon nanotube-galapectite aerogel composite
Scale and micro-meter scale hole, nanoscale hole average out to 10-12nm, 20-22 μm of average out to of micro-meter scale hole, under
State step progress:
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
It dissipates uniformly, vacuum is kept after vacuumizing, be then restored to normal pressure, after repeating vacuum step three times, after product is washed, dispersion
In 100 parts by weight water, warming-in-water to initiated polymerization at 70-80 DEG C, polymerization reaction time at least 50h, washing dispersion
Into 100 parts by weight water, the dispersion liquid of step 1 is obtained；
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 takes 0.5-15 parts by weight lauryl sodium sulfate to be added in 100 parts by weight water, after sonic oscillation, is added thereto
The carbon nanotube of 0.5-15 parts by weight after ultrasonic disperse is uniform, keeps vacuum after vacuumizing, be then restored to normal pressure, repeats to take out
Vacuum step three times, obtains the wet gel of step 2；
Step 3, the dispersion liquid of 0.5-15 parts by weight step 1 is mixed with the wet gel of 0.5-25 parts by weight step 2, thereto plus
Enter 0.01-2 parts by weight initiator, 0.01-10 parts by weight gentamicin, after ultrasonic disperse is uniform, warming-in-water is at 70-80 DEG C
Initiated polymerization after polymerization reaction time at least 50h, product is freeze-dried, drying time at least 2h is obtained mesoporous-micro-
Hole carbon nanotube-galapectite aerogel composite；
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 carbon nanotube-galapectite aerogel composite, 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 carbon nanotube being added in step 2 is successfully configured to network pore knot
Structure, above-mentioned tridimensional network and carbon nanotube are successfully configured to network pore structure and together form three-dimensional network hole knot
Structure, above-mentioned three-dimensional network pore structure provide meso-hole structure for mesoporous-micropore carbon nanotube-galapectite aerogel composite,
Gentamicin is supported in meso-hole structure simultaneously.
2. mesoporous-micropore carbon nanotube-galapectite aerogel composite according to claim 1, it is characterised in that:
In step 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
Measure 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
Dexamethasone 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 carbon nanotube-galapectite aerogel composite according to claim 1, it is characterised in that:
In step 2,1-10 parts by weight lauryl sodium sulfate is added to the water, after sonic oscillation 2-48h, 1-10 weight is added thereto
Part carbon nanotube, after the uniform 1-24h of ultrasonic disperse, vacuum 1h is kept after vacuumizing.
4. mesoporous-micropore carbon nanotube-galapectite aerogel composite according to claim 1, it is characterised in that:
In step 3, the dispersion liquid of 1-10 parts by weight step 1 is mixed with the wet gel of 1-20 parts by weight step 2, is added thereto
0.01-1 parts by weight initiator, 0.05-5 parts by weight gentamicin, after ultrasonic disperse is uniform, when carrying out polymerization reaction, selection exists
Polymerize 12-24h under 70-80 DEG C of water bath condition after prepolymerization 30-60min in 40-60 DEG C of water bath with thermostatic control, then by its according to
Secondary to polymerize 2-8h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, freeze-drying condition is -5 DEG C of temperature -- it is 108 DEG C, wet
0-60 DEG C, vacuum degree 10-50000pa, time 2-48h of degree.
5. mesoporous-micropore carbon nanotube-galapectite aerogel composite according to claim 1, it is characterised in that: draw
Send out agent selection dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
6. mesoporous-micropore carbon nanotube-galapectite aerogel composite preparation method, it is characterised in that: according to following steps
It is rapid to carry 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
It dissipates uniformly, vacuum is kept after vacuumizing, be then restored to normal pressure, after repeating vacuum step three times, after product is washed, dispersion
In 100 parts by weight water, warming-in-water to initiated polymerization at 70-80 DEG C, polymerization reaction time at least 50h, washing dispersion
Into 100 parts by weight water, the dispersion liquid of step 1 is obtained；
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 takes 0.5-15 parts by weight lauryl sodium sulfate to be added in 100 parts by weight water, after sonic oscillation, is added thereto
The carbon nanotube of 0.5-15 parts by weight after ultrasonic disperse is uniform, keeps vacuum after vacuumizing, be then restored to normal pressure, repeats to take out
Vacuum step three times, obtains the wet gel of step 2；
Step 3, the dispersion liquid of 0.5-15 parts by weight step 1 is mixed with the wet gel of 0.5-25 parts by weight step 2, thereto plus
Enter 0.01-2 parts by weight initiator, 0.01-10 parts by weight gentamicin, after ultrasonic disperse is uniform, warming-in-water is at 70-80 DEG C
Initiated polymerization after polymerization reaction time at least 50h, product is freeze-dried, drying time at least 2h is obtained mesoporous-micro-
Hole carbon nanotube-galapectite aerogel composite；
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 carbon nanotube-galapectite aerogel composite, 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 carbon nanotube being added in step 2 is successfully configured to network pore knot
Structure, above-mentioned tridimensional network and carbon nanotube are successfully configured to network pore structure and together form three-dimensional network hole knot
Structure, above-mentioned three-dimensional network pore structure provide meso-hole structure for mesoporous-micropore carbon nanotube-galapectite aerogel composite,
Gentamicin is supported in meso-hole structure simultaneously.
7. mesoporous-micropore carbon nanotube-galapectite aerogel composite preparation method according to claim 6,
It is characterized in that: 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 carbon nanotube-galapectite aerogel composite preparation method according to claim 6,
It is characterized in that: in step 2,1-10 parts by weight lauryl sodium sulfate being added to the water, after sonic oscillation 2-48h, thereto
The carbon nanotube of 1-10 parts by weight is added, after the uniform 1-24h of ultrasonic disperse, vacuum 1h is kept after vacuumizing.
9. mesoporous-micropore carbon nanotube-galapectite aerogel composite preparation method according to claim 6,
It is characterized in that: in step 3, the dispersion liquid of 1-10 parts by weight step 1 being mixed with the wet gel of 1-20 parts by weight step 2, to
0.01-1 parts by weight initiator is wherein added, 0.05-5 parts by weight gentamicin after ultrasonic disperse is uniform, is carrying out polymerization reaction
When selection polymerize 12-24h in 40-60 DEG C of water bath with thermostatic control after prepolymerization 30-60min under 70-80 DEG C of water bath condition, with
It is successively polymerize to 2-8h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control afterwards, 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.
10. mesoporous-micropore carbon nanotube-galapectite aerogel composite preparation method according to claim 6,
Be characterized in that: initiator selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
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| CN101612128A (en) * | 2009-07-23 | 2009-12-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Alginic acid inorganic nanometer composite gel microspheres and preparation method thereof |
| WO2011030170A1 (en) * | 2009-09-14 | 2011-03-17 | The University Of Nottingham | Cellulose nanoparticle aerogels, hydrogels and organogels |
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