CN109988274A - With mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite and preparation method thereof - Google Patents
With mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite and preparation method thereof Download PDFInfo
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Abstract
The present invention provides the mesh carbon nanotube-galapectite aerogel composite and preparation method thereof with mesoporous and micropore, galapectite dispersion liquid is obtained after galapectite dispersion liquid is polymerize with the mixed solution of deca-BDE, the wet gel of lauryl sodium sulfate and carbon nanotube is prepared again, it is added after initiator and ammonium polyphosphate that the reaction was continued after dispersion liquid is mixed with wet gel thereto, obtains that there is mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite.It uses the doughnut with microcellular structure for raw material, builds three-dimensional aeroge network, using the meso-hole structure of aeroge and the microcellular structure of fiber, load deca-BDE and ammonium polyphosphate respectively, different characteristics fire retardant is combined, realize cooperative flame retardant effect.
Description
Technical field
The present invention relates to technical field of nano material, more specifically to a kind of with mesoporous and micropore reticulated carbon
Nanotube-galapectite 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 with mesoporous and micropore mesh carbon nanotube-
Galapectite aerogel composite and preparation method thereof uses the doughnut with microcellular structure for raw material, builds three-dimensional gas
Gel network loads different flame retardant respectively, different characteristics is hindered using the meso-hole structure of aeroge and the microcellular structure of fiber
It fires agent to combine, realizes cooperative flame retardant effect.
The purpose of the present invention is achieved by following technical proposals.
With mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite and preparation method thereof, under
State step progress:
Step 1,0.7-12 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, galapectite dispersion liquid is obtained, by 0.7-12 parts by weight of styrene sodium sulfonate, 0.06-1.6
The poly- divinylsiloxanes of parts by weight, 0.01-0.3 parts by weight initiator, 0.08-8 parts by weight deca-BDE are added to 50 weights
In the mixed liquor for measuring part deionized water and 50 parts by weight of ethanol, above-mentioned solution is added to galapectite dispersion liquid after mixing evenly
In, ultrasonic disperse is uniform, and vacuum is kept after vacuumizing, and is then restored to normal pressure, and after repeating vacuum step three times, product is washed
It after washing, 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,
Washing 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 2,0.6-12 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 0.6-12 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 0.8-12 parts by weight step 1 is mixed with the wet gel of 0.7-22 parts by weight step 2, Xiang Qi
Middle addition 0.01-1.2 parts by weight initiator, 0.03-7 parts by weight ammonium polyphosphate, after ultrasonic disperse is uniform, warming-in-water to 70-
Initiated polymerization at 80 DEG C after polymerization reaction time at least 50h, product is freeze-dried, drying time at least 2h is had
There is mesoporous and micropore mesh 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 deca-BDE is added in the mixed solution of water and ethyl alcohol, and above-mentioned solution is added after stirring 10-60min
Into galapectite dispersion liquid, ultrasonic disperse 25-35min keeps vacuum 0.5-1.5h, the choosing when carrying out polymerization reaction after vacuumizing
It selects and 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 will
It successively polymerize 2-8h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control respectively.
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 ammonium polyphosphate, 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 -6 DEG C of temperature -- 105
DEG C, 2-55 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 deca-BDE of middle addition are also dispersed in halloysite nanotubes hollow structure, angstrom
Lip river stone nanotube hollow structure is provides micropore with mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite
Structure, after vacuumizing, washing, poly- divinylsiloxanes are copolymerized with sodium styrene sulfonate, are formed galapectite and are received
Cross-linked structure is formed inside mitron, deca-BDE is supported in halloysite nanotubes, and step 3 to be located at galapectite nanometer
It polymerize under the action of initiator between the vinyl functional group in poly- divinylsiloxanes outside pipe hollow structure, with
So that halloysite nanotubes and poly- divinylsiloxanes is collectively formed tridimensional network, the carbon nanotube being added in step 2 at
Function is configured to network pore structure, and above-mentioned tridimensional network is successfully configured to network pore structure with carbon nanotube and is collectively formed
Three-dimensional network pore structure, above-mentioned three-dimensional network pore structure are with mesoporous and mesh carbon nanotube-galapectite of micropore
Aerogel composite provides meso-hole structure, while ammonium polyphosphate being supported in meso-hole structure.
Using scientific and technological (Beijing) the Co., Ltd 3H-2000PS1 type static volumetric method specific surface area of Bei Shide instrument and aperture
The N of the tester analysis composite material that according to the present invention prepared by the method2Adsorption-desorption curve, such as Fig. 1.It can be with from figure
Find out, the N of the material2Adsorption-desorption curve is the IV class isothermal curve of H1 type hysteresis loop in IUPAC classification, i.e., by mesoporous knot
Structure generates.Illustrate that material itself has the pore structure of meso-scale.There is vertical ascent trend from the distribution of low pressure endpoint, can see
Sample interior is as caused by absorption potential strong inside micropore there are more micropore out.By nitrogen adsorption desorption isotherm data,
The sample specific surface area can reach 601.94m2g-1, which exists simultaneously mesoporous-micropore second level pore structure, surveys through multiple groups
The average specific surface area for measuring material is 600-603m2g-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=-0.962/ln (p/p0), unit nm, while adding adsorbent layer thickness t=0.359 [- 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
11.3nm, another kind are 5.62 μm, are measured through multiple groups, and nanoscale hole is average up to 9-13nm, and micro-meter scale hole is average
Up to 4-8 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.
Detailed description of the invention
Fig. 1 is that have mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite N2Adsorption-desorption is bent
Line；
Fig. 2 is that have mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite electromicroscopic photograph.
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, (number-average molecular weight 800, contents of ethylene rubs the poly- divinylsiloxanes of 0.2g
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of your percentage 3.5%), 0.01g azodiisobutyronitrile (ABIN), 3g
Deca-BDE 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 25min keeps 1.5h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three
It after secondary, after product is washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 35min in 50 DEG C of perseverance
It polymerize 12 hours in tepidarium, after it is successively then polymerize 4h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, will produces
After object washing, it is scattered in 100g water, obtains galapectite support dispersion；1g lauryl sodium sulfate is taken to be added in 100g water,
After sonic oscillation 2h, the carbon nanotube of 4g is added, ultrasonic disperse 1h 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 carrier wet gel；By 2g galapectite carrier point
Dispersion liquid is mixed with 1g carbon nanotube carrier wet gel, is added 0.5g azodiisobutyronitrile (ABIN), 0.05g ammonium polyphosphate, then surpass
Sound disperses 2h, is placed under 75 DEG C of water bath condition after prepolymerization 30min and polymerize 14 hours in 50 DEG C of water bath with thermostatic control, then will
After it successively polymerize 4h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is freeze-dried, cryogenic temperature is -6
DEG C, dry humidity is 2 DEG C, and dry vacuum degree is generally 2000pa, and drying time is generally 2 hours, obtains carbon nanotube/Ai Luo
The multiple dimensioned carrier aeroge of stone.
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 2500, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of mole percent 2%), 0.04g dibenzoyl peroxide (BPO),
4g deca-BDE 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 35min keeps 0.5h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three
It after secondary, after product is washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 30min in 50 DEG C of perseverance
It polymerize 14 hours in tepidarium, after it is successively then polymerize 6h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, will produces
After object washing, it is scattered in 100g water, obtains galapectite support dispersion；2g lauryl sodium sulfate is taken to be added in 100g water,
After sonic oscillation 48h, the carbon nanotube of 10g is added, ultrasonic disperse 4h obtains dispersion liquid；It is protected after above-mentioned dispersion liquid is vacuumized
1h is held, normal pressure is then restored to, vacuum step is repeated three times, obtains carbon nanotube carrier wet gel；By 4g galapectite carrier
Dispersion liquid is mixed with 5g carbon nanotube carrier wet gel, is added 0.01g dibenzoyl peroxide (BPO), 1g ammonium polyphosphate, then surpass
Sound disperses 10h, is placed under 75 DEG C of water bath condition after prepolymerization 40min in 50 DEG C of water bath with thermostatic control and polymerize 12 hours, then
After it is 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 be-
105 DEG C, dry humidity is 20 DEG C, and dry vacuum degree is generally 10pa, and drying time is generally 48 hours, obtain carbon nanotube/
The multiple dimensioned carrier aeroge of galapectite.
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 2000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 3%), 0.08g azodiisobutyronitrile (ABIN), 5g
Deca-BDE 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 28min 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 support dispersion；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 carrier wet gel；By 1g galapectite carrier point
Dispersion liquid is mixed with 8g carbon nanotube carrier wet gel, is added 0.2g azodiisobutyronitrile (ABIN), 2g ammonium polyphosphate, 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 carrier 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 4000, contents of ethylene rubs the poly- divinylsiloxanes of 1g
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of your percentage 1.5%), 0.1g dibenzoyl peroxide (BPO), 2g
Deca-BDE is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 40min, is added to galapectite dispersion liquid
In, ultrasonic disperse 32min keeps 1.5h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three
It after secondary, after product is washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 60min in 50 DEG C of perseverance
It polymerize 24 hours in tepidarium, after it is successively then polymerize 8h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, will produces
After object washing, it is scattered in 100g water, obtains galapectite support dispersion；8g lauryl sodium sulfate is taken to be added in 100g water,
After sonic oscillation 30h, the carbon nanotube of 6g is added, ultrasonic disperse for 24 hours, obtains dispersion liquid；It is protected after above-mentioned dispersion liquid is vacuumized
1h is held, normal pressure is then restored to, vacuum step is repeated three times, obtains carbon nanotube carrier wet gel；By 6g galapectite carrier
Dispersion liquid is mixed with 20g carbon nanotube carrier wet gel, is added 0.8g dibenzoyl peroxide (BPO), 3g ammonium polyphosphate, then surpass
Sound disperses 4h, 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 will
After it successively polymerize 2h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is freeze-dried, cryogenic temperature is -80
DEG C, dry humidity is 40 DEG C, and dry vacuum degree is generally 1000pa, and drying time is generally 20 hours, obtain carbon nanotube/angstrom
The multiple dimensioned carrier aeroge of Lip river stone.
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 bi-end-blocking of mole percent 1.5%), 0.06g azodiisobutyronitrile (ABIN),
1g deca-BDE 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 33min keeps 0.5h after vacuumizing above-mentioned mixed liquor, be then restored to normal pressure, repeats vacuum step three
It after secondary, 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 perseverance
It polymerize 18 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
After object washing, it is scattered in 100g water, obtains galapectite support dispersion；6g lauryl sodium sulfate is taken to be added in 100g water,
After sonic oscillation 35h, the carbon nanotube of 8g is added, ultrasonic disperse 20h obtains dispersion liquid；It is protected after above-mentioned dispersion liquid is vacuumized
1h is held, normal pressure is then restored to, vacuum step is repeated three times, obtains carbon nanotube carrier wet gel；By 8g galapectite carrier
Dispersion liquid is mixed with 12g carbon nanotube carrier wet gel, is added 1g azodiisobutyronitrile (ABIN), 4g ammonium polyphosphate, then ultrasound
Disperse 6h, is placed under 75 DEG C of water bath condition after prepolymerization 50min and polymerize 20 hours in 50 DEG C of water bath with thermostatic control, then by it
After successively polymerizeing 5h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is freeze-dried, cryogenic temperature is -60 DEG C,
Dry humidity is 50 DEG C, and dry vacuum degree is generally 50000pa, and drying time is generally 30 hours, obtains carbon nanotube/Ai Luo
The multiple dimensioned carrier aeroge of stone.
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 deca-BDE is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, stirs 20min, is added to galapectite dispersion
In liquid, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, is then restored to normal pressure, repeats vacuum step three
It after secondary, after product is washed, is scattered in 100g water, is placed under 75 DEG C of water bath condition after prepolymerization 50min in 50 DEG C of perseverance
It polymerize 20 hours in tepidarium, after it is successively then polymerize 2h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, will produces
After object washing, it is scattered in 100g water, obtains galapectite support dispersion；5g lauryl sodium sulfate is taken to be added in 100g water,
After sonic oscillation 40h, the carbon nanotube of 5g is added, ultrasonic disperse 15h obtains dispersion liquid；It is protected after above-mentioned dispersion liquid is vacuumized
1h is held, normal pressure is then restored to, vacuum step is repeated three times, obtains carbon nanotube carrier wet gel；By 10g galapectite carrier
Dispersion liquid is mixed with 16g carbon nanotube carrier wet gel, is added 0.6g dibenzoyl peroxide (BPO), 5g ammonium polyphosphate, then surpass
Sound disperses 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 will
After it successively distinguishes 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 55 DEG C, and dry vacuum degree is generally 3000pa, and drying time is generally 40 hours, obtain carbon nanotube/angstrom
The multiple dimensioned carrier aeroge of Lip river stone.
Embodiment 7
12g 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 12g sodium styrene sulfonate, 1.6g poly- divinylsiloxanes (number-average molecular weight 5000, contents of ethylene
The poly dimethyl divinylsiloxanes of the amino list sealing end of mole percent 0.1%), 0.3g azodiisobutyronitrile (ABIN),
8g deca-BDE is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 40min, is added to galapectite dispersion liquid
In, ultrasonic disperse 26min 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 70 DEG C of water bath condition after prepolymerization 60min in 40 DEG C of constant temperature
It polymerize 24 hours in water-bath, after it is successively then polymerize 8h 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 support dispersion；It takes 12g lauryl sodium sulfate to be added in 100g water, surpasses
After sound oscillation 30h, the carbon nanotube of 12g is added, ultrasonic disperse for 24 hours, 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 carrier wet gel；By 12g galapectite carrier point
Dispersion liquid is mixed with 22g carbon nanotube carrier wet gel, is added 1.2g azodiisobutyronitrile (ABIN), 7g ammonium polyphosphate, then ultrasound
Disperse 4h, is placed under 70 DEG C of water bath condition after prepolymerization 60min and polymerize 16 hours in 40 DEG C of water bath with thermostatic control, then by it
After successively polymerizeing 2h respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control, product is freeze-dried, cryogenic temperature is -80 DEG C,
Dry humidity is 40 DEG C, and dry vacuum degree is generally 1000pa, and drying time is generally 20 hours, obtains carbon nanotube/Ai Luo
The multiple dimensioned carrier aeroge of stone.
Embodiment 8
0.7g 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 0.7g sodium styrene sulfonate, 0.06g poly- divinylsiloxanes (number-average molecular weight 500, vinyl
The poly dimethyl divinylsiloxanes of the amino bi-end-blocking of content mole percent 5%), 0.01g dibenzoyl peroxide
(BPO), 0.08g deca-BDE is added in the mixed liquor of 50g deionized water and 50g ethyl alcohol, is stirred 10min, is added to angstrom
In the stone dispersion liquid of Lip river, ultrasonic disperse 30min keeps 1h after vacuumizing above-mentioned mixed liquor, is then restored to normal pressure, repeats to take out true
Empty 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 35min
It polymerize in 60 DEG C of water bath with thermostatic control 12 hours, then successively polymerize it respectively in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control
After 4h, after product is washed, it is scattered in 100g water, obtains galapectite support dispersion；0.6g lauryl sodium sulfate is taken to add
Enter in 100g water, after sonic oscillation 2h, the carbon nanotube of 0.6g is added, ultrasonic disperse 1h obtains dispersion liquid；By above-mentioned dispersion liquid
1h is kept after vacuumizing, is then restored to normal pressure, is repeated vacuum step three times, is obtained carbon nanotube carrier wet gel；It will
0.8g galapectite support dispersion is mixed with 0.7g carbon nanotube carrier wet gel, and 0.01g dibenzoyl peroxide is added
(BPO), 0.03g ammonium polyphosphate, re-ultrasonic dispersion 2h are placed under 80 DEG C of water bath condition after prepolymerization 30min in 60 DEG C of perseverance
It polymerize 14 hours in tepidarium, after it is successively then polymerize 4h 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 -6 DEG C, and dry humidity is 19 DEG C, and dry vacuum degree is generally 2000pa, and drying time is general
It is 2 hours, obtains the multiple dimensioned carrier aeroge of carbon nanotube/galapectite.
Flame retardant property test:
The material and EVA (mass ratio 1:4) for taking the method for the invention to prepare, are warming up to 140 DEG C for mixer, 45
EVA is added under conditions of rev/min, the material of invention the method preparation is added after constant torque, keeps 10min to mixing
Uniformly.Composite material after mixing is put into vulcanizing press, sample processed is molded with 140 DEG C of 10MPa, is placed on dry and ventilated
Place is for 24 hours.According to GB/T2406.2-2009, GB8624-2006 and document (Li Bin, Wang Jianqi, polymer material flammability and resistance
Evaluation --- cone calorimetry (CONE) method of combustion property, polymer material science and engineering, 1998,14:15) the method measurement
Composite material limit oxygen index, maximum heatrelease rate and ignitor firing time, the results are shown in Table 1.
1 flame retardant property of table
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. with mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite, it is characterised in that: carbon nanotube-
Galapectite aerogel composite average specific surface area is 600-603m2g-1, in carbon nanotube-galapectite aerogel composite
Exist simultaneously nanoscale and micro-meter scale hole, nanoscale hole average out to 9-13nm, micro-meter scale hole average out to 4-8
μm, it carries out as steps described below:
Step 1,0.7-12 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 0.7-12 parts by weight of styrene sodium sulfonate, 0.06-1.6 weight
The poly- divinylsiloxanes of part, 0.01-0.3 parts by weight initiator, 0.08-8 parts by weight deca-BDE are 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 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 0.6-12 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 0.6-12 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 0.8-12 parts by weight step 1 is mixed with the wet gel of 0.7-22 parts by weight step 2, thereto plus
Enter 0.01-1.2 parts by weight initiator, 0.03-7 parts by weight ammonium polyphosphate, after ultrasonic disperse is uniform, warming-in-water is to 70-80 DEG C
Lower initiated polymerization after polymerization reaction time at least 50h, product is freeze-dried, drying time at least 2h, is obtained having and is situated between
The mesh carbon nanotube of hole and micropore-galapectite aerogel composite.
2. according to claim 1 have mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite,
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 deca-BDE is added in the mixed solution of water and ethyl alcohol, and above-mentioned solution is added after stirring 10-60min
Into galapectite dispersion liquid, ultrasonic disperse 25-35min keeps vacuum 0.5-1.5h, the choosing when carrying out polymerization reaction after vacuumizing
It selects and 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 will
It successively polymerize 2-8h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control respectively.
3. according to claim 1 have mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite,
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.
4. according to claim 1 have mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite,
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 ammonium polyphosphate 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 -6 DEG C of temperature --
105 DEG C, 2-55 DEG C of humidity, vacuum degree 10-50000pa, time 2-48h.
5. according to claim 1 have mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite,
Be characterized in that: initiator selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
6. with mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite preparation method, it is characterised in that:
It carries out as steps described below:
Step 1,0.7-12 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 0.7-12 parts by weight of styrene sodium sulfonate, 0.06-1.6 weight
The poly- divinylsiloxanes of part, 0.01-0.3 parts by weight initiator, 0.08-8 parts by weight deca-BDE are 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 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 0.6-12 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 0.6-12 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 0.8-12 parts by weight step 1 is mixed with the wet gel of 0.7-22 parts by weight step 2, thereto plus
Enter 0.01-1.2 parts by weight initiator, 0.03-7 parts by weight ammonium polyphosphate, after ultrasonic disperse is uniform, warming-in-water is to 70-80 DEG C
Lower initiated polymerization after polymerization reaction time at least 50h, product is freeze-dried, drying time at least 2h, is obtained having and is situated between
The mesh carbon nanotube of hole and micropore-galapectite aerogel composite.
7. according to claim 6 with mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite
Preparation method, it is characterised in that: in step 1, the mixing that 1-10 parts by weight halloysite nanotubes are added to water and ethyl alcohol is molten
Ultrasonic disperse 1h in liquid, 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 deca-BDE are added in the mixed solution of water and ethyl alcohol, will after stirring 10-60min
Above-mentioned solution is added in galapectite dispersion liquid, ultrasonic disperse 25-35min, and vacuum 0.5-1.5h is kept after vacuumizing, is being carried out
Selection polymerize in 40-60 DEG C of water bath with thermostatic control after prepolymerization 30-60min under 70-80 DEG C of water bath condition when polymerization reaction
It is then successively polymerize 2-8h in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control by 12-24h respectively.
8. according to claim 6 with mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite
Preparation method, it is characterised in that: in step 2,1-10 parts by weight lauryl sodium sulfate is added to the water, sonic oscillation 2-
After 48h, the carbon nanotube of 1-10 parts by weight is added thereto, after the uniform 1-24h of ultrasonic disperse, vacuum 1h is kept after vacuumizing.
9. according to claim 6 with mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite
Preparation method, it is characterised in that: in step 3, by the wet of the dispersion liquid of 1-10 parts by weight step 1 and 1-20 parts by weight step 2
Gel mixes, thereto addition 0.01-1 parts by weight initiator, 0.05-5 parts by weight ammonium polyphosphate, after ultrasonic disperse is uniform,
Carry out polymerization reaction when selection under 70-80 DEG C of water bath condition after prepolymerization 30-60min in 40-60 DEG C of water bath with thermostatic control
It polymerize 12-24h, it is then successively polymerize in 80 DEG C, 90 DEG C, 100 DEG C of water bath with thermostatic control to 2-8h respectively, is freeze-dried condition
It is -6 DEG C of temperature -- 105 DEG C, 2-55 DEG C of humidity, vacuum degree 10-50000pa, time 2-48h.
10. according to claim 6 with mesoporous and micropore mesh carbon nanotube-galapectite aerogel composite
Preparation method, it is characterised in that: initiator selects dibenzoyl peroxide (BPO) or azodiisobutyronitrile (ABIN).
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