CN109012568A - A kind of nanofiber-based hud typed adsorbent material of magnetic silicon oxide and preparation method thereof - Google Patents
A kind of nanofiber-based hud typed adsorbent material of magnetic silicon oxide and preparation method thereof Download PDFInfo
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Abstract
The invention discloses nanofiber-based hud typed adsorbent materials of a kind of magnetic silicon oxide and preparation method thereof, using the silicon oxide nanofiber extracted in choysotile as carrier, using ferric acetyl acetonade as the source of iron substance of the nano particle of synthesis ferroso-ferric oxide, it is slowly decomposed under high temperature anaerobic environment using ferric acetyl acetonade, and load is realized for ferroferric oxide nano granules in silicon oxide nanofiber surface crystallization, then porous silica shell is formed in its surface self-organization by silicon source Substance P hydrolysis, prepare the nanofiber-based hud typed adsorbent material of magnetic silicon oxide.The magnetic core-shell adsorbent material interlayer is clearly demarcated, stable structure, large specific surface area, is easy to Magnetic Isolation, has very strong adsorption effect to cationic organic dyestuff and metal ion.The adsorbed organic pollutant of the adsorbent material can be degraded by the ferroso-ferric oxide of own load by simple class Fenton's reaction, so that it is guaranteed that the multiple regeneration of the material.
Description
Technical field
The present invention relates to functional material preparation technical field, specially a kind of silicon oxide nanofiber, ferroso-ferric oxide with
Composite adsorbing material of porous silica and preparation method thereof.
Background technique
With the continuous improvement of China's industrial level, the industrial discharges such as chemical industry, weaving, mining industry and metallurgy are a large amount of organic
Chemical dyestuff waste water and effluent containing heavy metal ions constitute grave danger to environment and ecology, therefore at present to organic pollution
The important topic of fwaater resources protection is had become with the improvement of heavy metal ion.In many processing methods, physisorphtion by
In its treating capacity, big, simple process, feature applied widely and obvious effect are considered as the improvement of most practical potentiality
Method.The adsorbent applied at present is mainly that specific surface area is larger, the more rich solid of pore structure.The adsorbent in adsorption process
It needs to be dispersed in sewage and come into full contact with pollutant as far as possible, this process makes adsorbent after completing adsorption process
It is difficult to realize effectively be separated by solid-liquid separation.In addition, traditional adsorbent is due to being difficult to carry out regenerative operation, being used repeatedly property compared with
All there is larger defect for economy and environmental in difference.
In recent years, the preparation of magnetic composite and application development are rapid, and are widely used in point of adsorbent, catalyst
From etc. complex processes, enormously simplify process flow.Under the action of externally-applied magnetic field, consolidating for magnetic adsorbent can be fast implemented
Liquid separation, thus largely can solve the separation problem that traditional adsorbent material is faced in practical applications.Currently,
It is modified to the magnetism of adsorbent mainly to introduce the magnetic ferroso-ferric oxide of tool by the modes such as impregnating or loading.Wherein, it bears
The ferriferrous oxide particles for carrying nanometer-sized monodisperse can make modified composite structure stable, magnetic uniform, be current magnetic
Property modified hot spot, have a large amount of research.
Meanwhile for the regeneration for the adsorbent for adsorbing organic matter, current main regeneration method has thermal decomposition regeneration, light
Catalytic regeneration, Fenton regeneration etc., are all the organic matter degradations for making to be adsorbed on adsorbent surface by oxidation reaction, to make to adsorb
Agent restores its adsorption site being occupied.Wherein, Fenton's reaction is due to having the characteristics that degradation capability is strong, high-efficient and a large amount of
Ground report；With further research, discovery has without secondary pollution, degradation by the class Fenton's reaction of catalyst of ferroso-ferric oxide
Effect is good and is attached to the characteristic of magnetic separation of solid and liquid, thus shows huge application potential.It is dedicated to currently, the country has
The modified patent of the magnetism of adsorbent is (such as " magnetic mesoporous silicon oxide surface imprinted polymer adsorbent material and preparation method thereof ",
CN106334537A [P] 2017-01-18), and to such adsorbent material with core-shell structure and class Fenton power of regeneration
It studies still less.
Summary of the invention
Silicon oxide nanofiber is the natural minerals for the high-purity extracted from choysotile, due to its high-specific surface area
With nanometer fibrous pattern by the carrier as nano particle, the spontaneous reunion that can significantly solve nano particle is existing
As improving performance；Porous silica has very high specific surface area, and passes through hydrolysis self assembly system with silicon sources such as ethyl orthosilicates
Standby porous silica out has the order and controllability of height.In order to which solving current adsorbent is difficult to realize solid-liquid simultaneously
The problem for separating and being difficult to multiple regeneration is received the present invention provides a kind of using silicon oxide nanofiber, ferroso-ferric oxide
The composite adsorbing material that rice grain, porous silica are synthesized as matrix.
A kind of nanofiber-based hud typed adsorbent material of magnetic silicon oxide, silicon oxide nanofiber contains in the adsorbent material
Amount is 35 ~ 50%, and ferroso-ferric oxide content is 5 ~ 35%, and porous oxidation silicone content is 20 ~ 60%.
Preferably, silicon oxide nanofiber diameter is 30 ~ 60nm in the adsorbent material, length is greater than 1 μm, and major diameter
Than being greater than 30:1.
Further, the aperture of porous silica is mainly distributed on 2 ~ 5nm in the adsorbent material.
Preferably, ferroso-ferric oxide is attached to silicon oxide nanofiber surface, silica nanometer in the adsorbent material
Fiber and its adhering on surface ferriferrous oxide particles wrapped up by one layer of porous silica.
The present invention further provides a kind of methods for preparing the nanofiber-based hud typed adsorbent material of magnetic silicon oxide, including
Following steps:
(1) the silicon oxide nanofiber suspension dispersed through ethyl alcohol is added in organic solvent and is dispersed with stirring, and be heated to 90
DEG C, the ethyl alcohol in system is evaporated until forming uniform suspension；
(2) step (1) resulting suspension is added in three-necked bottle, ferric acetyl acetonade is then added, and magnetic agitation is with shape
At homogeneous mixture, while being passed through protective gas；
(3) step (2) resulting suspension is heated to 260 ~ 285 DEG C with the speed of 3 DEG C/min, then constant temperature-condensing reflux
For a period of time, then mixture is cooled to room temperature, after separation of solid and liquid, then with ethyl alcohol and deionized water number is washed to solid product
It is secondary and dry under 60 DEG C of vacuum, obtain nanocomposite；
(4) nanocomposite is added in the mixed solution being made of deionized water, concentrated ammonia liquor and dehydrated alcohol, then
Cetyl trimethylammonium bromide is added into the mixed liquor, and is vigorously stirred and to form homogeneous dispersion, then slowly to institute
State in mixture instill 0.1 ~ 0.5mL silicon source, continue 6~12h of stirring at room temperature, then filter, by solid product spend from
It is dried in vacuo at 60 DEG C after sub- water and ethanol washing 3 times；
(5) by step (4) dried product exhibited and NH4NO3Together be added to equipped with ethyl alcohol conical flask in be vigorously stirred, by from
Sub- exchange process removes the dried product exhibited organic matter cetyl trimethylammonium bromide remained on surface, and then vacuum drying is
It can get the nanofiber-based hud typed adsorbent material of magnetic silicon oxide.
Preferably, the solid content of the silicon oxide nanofiber suspension is 10g/L, the silica in step (1)
Nanofiber is to extract in choysotile；The organic solvent is appointing in triethylene glycol, triethylene glycol, glycerol, octadecylene etc.
It anticipates one kind.
As further preferred, in step (2), the mass ratio of silicon oxide nanofiber solid and ferric acetyl acetonade be 1:1 ~
3:8；20~40min of the magnetic agitation time；The protective gas being passed through be high pure nitrogen, gas be passed through the time be 3min with
On.
Preferably, constant temperature-condensing reflux temperature in step (3) is maintained at 258 ~ 278 DEG C, soaking time is 20 ~
40min。
Preferably, the volume ratio of water and ethyl alcohol in mixed solution described in step (4) is 2:3 ~ 3:2, total volume is
120 ~ 160 mL, the volume of concentrated ammonia liquor are 1 ~ 5mL, and the quality that cetyl trimethylammonium bromide is added is 0.1 ~ 0.5g；It is described
Silicon source is the mixture of one or more of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester or butyl silicate.
As further preferred, ethyl alcohol volume is 60 ~ 100mL, NH in step (5)4NO3Quality be 1 ~ 2g, stirring when
Between be 30 ~ 60min.
The present invention has the beneficial effect that:
(1) carrier of this magnetic porous core-shell material is using the amorphous silicon oxide Nanowire extracted in natural minerals choysotile
Dimension, it is from a wealth of sources, nontoxic.Its physical and chemical stability is strong, is suitble to repeatedly use and various modifications.Fiber is straight
Diameter is 30 ~ 60nm, has great specific surface area, and the adsorptivity of itself is extremely strong, and surface is rich in functional groups such as hydroxyls, very suitable
Cooperation is the carrier of nano particle and the substrate of adsorbent material.The magnetic porous core-shell material interlayer is clearly demarcated, stable structure, compares table
Area is big, is easy to Magnetic Isolation, has to cationic dyes molecule (such as methylene blue) and heavy metal ion (such as lead ion)
Very strong adsorption effect.
(2) synthesis thinking of this magnetic porous core-shell material is clear, and synthetic method is simple, and nucleocapsid is well arranged.Outer layer
Porous silica is evenly distributed orderly, while reinforcing material absorption property, can also play guarantor to internal magnetic nanoparticle
Shield effect, keeps the structure of entire composite material more stable.The three-decker is highly stable, is suitble to carry out class in acid condition
Fenton's reaction, the adsorbent material can be fragrant by simple class by the ferroso-ferric oxide of own load after adsorbing organic pollutant
Reaction of pausing is degraded, therefore be can be used as adsorbent and repeatedly regenerated reuse.
(3) magnetic intensity of this magnetic porous core-shell material and outer layer porous oxidation silicon thickness can directly pass through variation source of iron
And the amount realization controllable adjustment of silicon source substance, flexible structure, applicability are wide.This magnetic porous core-shell material has preferable magnetic
Property, effective enrichment can be realized by externally-applied magnetic field, to efficiently separate from liquid phase, this solid-liquid separation method
Have the characteristics that simple, efficient, inexpensive, easy to operate.
(4) this magnetic porous core-shell material can realize quilt by easy class Fenton's reaction after having adsorbed organic pollutant
The degradation of adsorbent also makes the processing of pollutant more thorough to realize the recycling of material, it is furthermore this first will be dirty
It contaminates object to adsorb, then concentrates the environmental improvement method of degradation that also there is environmental protection and dual meaning economically using high-level oxidation technology
Justice.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of magnetic porous core-shell material prepared by the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope picture of magnetic porous core-shell material prepared by the embodiment of the present invention 1；
Fig. 3 is the hysteresis loop and dispersion-Magnetic Isolation in water of magnetic porous core-shell material prepared by the embodiment of the present invention 1
Figure.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.It should be appreciated that specific embodiment described herein is only to explain this hair
It is bright, it is not intended to limit the present invention.
Embodiment 1:
The silicon oxide nanofiber (solid content 10g/L) that 30mL disperses through ethyl alcohol is added in 60mL triethylene glycol and is heated
To 90 DEG C, the ethyl alcohol in system is evaporated, obtains uniform suspension, which is placed in three-necked bottle.To institute
The ferric acetyl acetonade that 500mg is added in solution in three-necked bottle, and magnetic agitation 30min are stated, homogeneous mixture is formed.Gained is equal
Even mixture is vigorously stirred, and is filled with protective gas nitrogen (N2) to ensure oxygen-free environment, gas be passed through the time be 3min with
On.Then after being heated to 278 DEG C with the rate of 3 DEG C/min, then constant temperature-condensing reflux 30min starts to cool down.By mixture
After being cooled to room temperature, magnetic force separation of solid and liquid is carried out to gained mixture using magnet.It solid product ethyl alcohol after separation and goes
Ion water washing is dried in vacuo at 60 DEG C after for several times, obtains nanocomposite.Then, by nano combined material made from 0.1g
Material and 0.3g cetyl trimethylammonium bromide (CTAB) are added to by 80mL deionized water, 2mL concentrated ammonia liquor and the anhydrous second of 60mL
In the mixed solution of alcohol composition, magnetic agitation 30min makes mixed solution homogenize, and forms homogeneous dispersion.What is be vigorously stirred
Under the conditions of, 0.25mL ethyl orthosilicate (TEOS) slowly is added into the mixed solution, continues to stir 8h at room temperature, using magnetic
Iron carries out magnetic force separation of solid and liquid to products therefrom.Solid matter with deionized water after separation and ethanol washing 3 times, after suction filtration
It is dried in vacuo at 60 DEG C.Finally by dried product exhibited and 1.8g NH4NO3Solid is added together to the taper that 100mL ethyl alcohol is housed
In bottle, agitator treating 30min removes dried product exhibited cetyl trimethyl bromine remained on surface by ion-exchange
After changing ammonium (CTAB), vacuum drying can be obtained the nanofiber-based hud typed adsorbent material of magnetic silicon oxide.In the adsorbent material
Silicon oxide nanofiber content is 44.3%, and ferroso-ferric oxide content is 15.5%, and porous oxidation silicone content is 40.1%, adsorption material
The pore-size distribution of porous silica is 2 ~ 5nm in material.
It is the scanning electron microscopic picture of magnetic porous core-shell material prepared by this example 1, the as seen from the figure absorption referring to Fig. 1
Uniform fibrous morphology is presented in material (fibre diameter is 30 ~ 60nm, and length is greater than 1 μm, and draw ratio is greater than 30:1)；Referring to
Fig. 2 is the transmission electron microscope picture of magnetic porous core-shell material prepared by the present embodiment 1, and the adsorbent material is presented bright as seen from the figure
Aobvious three-layer nuclear shell structure, magnetic nanoparticle therein are distributed evenly in silica nano particle that (diameter is about
10nm), the porous silica layer of outer layer is equably covered in core surface (thickness is about 25 ~ 30nm)；Referring to Fig. 3, for this
The hysteresis loop of magnetic porous core-shell material prepared by embodiment 1 and in water dispersion-Magnetic Isolation figure, the as seen from the figure absorption
Material has superparamagnetism, and furthermore the adsorbent material can be realized easily under externally-applied magnetic field and is separated by solid-liquid separation.
Embodiment 2:
The silicon oxide nanofiber (solid content 10g/L) that 30mL disperses through ethyl alcohol is added in 80mL triethylene glycol and is heated to
90 DEG C, the ethyl alcohol in system is evaporated, obtains uniform suspension, which is placed in three-necked bottle.To described
The ferric acetyl acetonade of 1000mg, and magnetic agitation 30min is added in three-necked bottle in solution, forms homogeneous mixture.By gained
Homogeneous mixture is vigorously stirred, and is filled with nitrogen (N2) to ensure oxygen-free environment, the time that is passed through of gas is 3min or more.Then
After being heated to 285 DEG C with the rate of 3 DEG C/min, then constant temperature-condensing reflux 30min starts to cool down.Mixture is cooled to room
Wen Hou carries out magnetic force separation of solid and liquid to gained mixture using magnet.Solid product ethyl alcohol and deionization washing after separation
It is dried in vacuo at 60 DEG C after washing for several times, nanocomposite can be obtained.Then, by nanocomposite made from 0.1g and
0.3g cetyl trimethylammonium bromide (CTAB) is added to by 60mL deionized water, 3mL concentrated ammonia liquor and 60mL dehydrated alcohol group
At mixed solution in, magnetic agitation 30min makes mixed solution homogenize, formed homogeneous dispersion.In the condition being vigorously stirred
Under, 0.1mL methyl orthosilicate is slowly added into the mixture, continues to stir 12h at room temperature, using magnet to products therefrom
Carry out magnetic force separation of solid and liquid.Solid matter with deionized water after separation and ethanol washing 3 times, vacuum is dry at 60 DEG C after suction filtration
It is dry.Finally by dried product exhibited and 2g NH4NO3Solid is added together into the conical flask equipped with 60mL ethyl alcohol, agitator treating
60min, after removing dried product exhibited cetyl trimethylammonium bromide remained on surface (CTAB) by ion-exchange,
Vacuum drying can be obtained the nanofiber-based hud typed adsorbent material of magnetic silicon oxide.Silicon oxide nanofiber in the adsorbent material
Content is 46%, and ferroso-ferric oxide content is 33%, and porous oxidation silicone content is 21%.
Embodiment 3:
The silicon oxide nanofiber (solid content 10g/L) that 50mL disperses through ethyl alcohol is added in 60mL glycerol and is heated to 90
DEG C, the ethyl alcohol in system is evaporated, uniform suspension is obtained, which is placed in three-necked bottle.To described three
The ferric acetyl acetonade of 300mg, and magnetic agitation 30min is added in neck bottle in solution, forms homogeneous mixture.Gained is uniform
Mixture is vigorously stirred, and is filled with nitrogen (N2) to ensure oxygen-free environment, the time that is passed through of gas is 3min or more.Then with 3
DEG C/after the rate of min is heated to 260 DEG C, then constant temperature-condensing reflux 30min starts to cool down.Mixture is cooled to room temperature
Afterwards, magnetic force separation of solid and liquid is carried out to gained mixture using magnet.Solid product after separation is washed with ethyl alcohol and deionized water
It is dried in vacuo at 60 DEG C after for several times, nanocomposite can be obtained.Then, by nanocomposite made from 0.1g and
0.3g cetyl trimethylammonium bromide (CTAB) is added to by 60mL deionized water, 1mL concentrated ammonia liquor and 80mL dehydrated alcohol group
At mixed solution in, magnetic agitation 30min makes mixed solution homogenize, formed homogeneous dispersion.In the condition being vigorously stirred
Under, 0. 5mL positive silicic acid propyl ester is slowly added into the mixture, continues to stir 6h at room temperature, using magnet to products therefrom
Carry out magnetic force separation of solid and liquid.Solid matter with deionized water after separation and ethanol washing 3 times, vacuum is dry at 60 DEG C after suction filtration
It is dry.Finally by dried product exhibited and 2g NH4NO3Solid is added together into the conical flask equipped with 100mL ethyl alcohol, agitator treating
30min, after removing dried product exhibited cetyl trimethylammonium bromide remained on surface (CTAB) by ion-exchange,
Vacuum drying can be obtained the nanofiber-based hud typed adsorbent material of magnetic silicon oxide.Silicon oxide nanofiber in the adsorbent material
Content is 38 %, and ferroso-ferric oxide content is 5%, and porous oxidation silicone content is 57%.
Table one be each embodiment products obtained therefrom to cationic organic dyestuff (methylene blue) and heavy metal ion (lead from
Son) Adsorption effect and respectively using class Fenton process, the regeneration efficiency (note: absorption after acidic cleaning method regeneration treatment
Adsorbent amount is 0.5g/L, methylene blue and lead ion as absorption object in the process, and initial concentration is the Asia 10mg/L
Methyl blue and 20mg/L lead ion)；In regenerative process, Fenton's reaction regeneration is carried out to the adsorbent for adsorbing methylene blue, it will
0.1g used adsorbent to be scattered in 100mL deionized water, and after adjusting pH to 3 ± 0.1,1mL hydrogen peroxide (H is added dropwise2O2,
30%) it can be taken off drying after, stirring 1h, and for adsorption-regeneration cycles next time)；To adsorbed the adsorbent of lead ion into
Row pickling regeneration can be taken off after using adsorbent to be scattered in 100mL nitric acid solution (0.01mol/L) stirring 1h 0.1g
It is dry, and for adsorption-regeneration cycles next time.As shown in Table 1, which all has methylene blue and lead ion excellent
Elegant Adsorption effect, and the regeneration of adsorbent may be implemented in utilization class Fenton process (methylene blue) or acid wash (lead ion)
It reuses.After five times are recycled, adsorption effect still can reach 70% of initial performance or more, have good circulation can
Usability.
The absorption of 1 different instances product of table and regeneration effect comparison
| Embodiment | Removal rate of 60 min to methylene blue | Five Fenton regeneration efficiencies | Removal rate of 60 min to lead ion | Five pickling regeneration efficiencies |
| 1 | 94.3% | 83.0% | 95.7% | 76.9% |
| 2 | 91.1% | 87.4% | 89.4% | 79.4% |
| 3 | 98. 8% | 80.7% | 98.1% | 71.7% |
Basic principles and main features and advantages of the present invention of the invention, the technical staff of the industry has been shown and described above
It should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and
Improvement all fall within the protetion scope of the claimed invention, and the claimed scope of the invention is by appended claims and its equivalent
Object defines.
Claims (10)
1. a kind of nanofiber-based hud typed adsorbent material of magnetic silicon oxide, it is characterised in that: silica in the adsorbent material
Nanofiber content is 35 ~ 50%, and ferroso-ferric oxide content is 5 ~ 35%, and porous oxidation silicone content is 20 ~ 60%.
2. adsorbent material according to claim 1, it is characterised in that: silicon oxide nanofiber diameter in the adsorbent material
For 30 ~ 60nm, length is greater than 1 μm, and draw ratio is greater than 30:1.
3. adsorbent material according to claim 1, it is characterised in that: the aperture of porous silica point in the adsorbent material
Cloth is in 2 ~ 5nm.
4. adsorbent material according to claim 1, it is characterised in that: ferroferric oxide nano granules in the adsorbent material
Be attached to silicon oxide nanofiber surface, silicon oxide nanofiber and its adhering on surface ferriferrous oxide particles by more than one layer
Hole silicon oxide-wrapped.
5. a kind of method for preparing any adsorbent material of Claims 1-4, comprising the following steps:
(1) the silicon oxide nanofiber suspension dispersed through ethyl alcohol is added in organic solvent and is dispersed with stirring, and be heated to 90
DEG C, the ethyl alcohol in system is evaporated until forming uniform suspension；
(2) step (1) resulting suspension is added in three-necked bottle, ferric acetyl acetonade is then added, and magnetic agitation is with shape
At homogeneous mixture, while being passed through protective gas；
(3) step (2) resulting suspension is heated to 260 ~ 285 DEG C with the speed of 3 DEG C/min, then constant temperature-condensing reflux
For a period of time, then mixture is cooled to room temperature, after separation of solid and liquid, then with ethyl alcohol and deionized water number is washed to solid product
It is secondary and dry under 60 DEG C of vacuum, obtain nanocomposite；
(4) nanocomposite is added in the mixed solution being made of deionized water, concentrated ammonia liquor and dehydrated alcohol, then
Cetyl trimethylammonium bromide is added into the mixed liquor, and is vigorously stirred and to form homogeneous dispersion, then slowly to institute
State in mixture instill 0.1 ~ 0.5mL silicon source, continue 6~12h of stirring at room temperature, then filter, by solid product spend from
It is dried in vacuo at 60 DEG C after sub- water and ethanol washing 3 times；
(5) by step (4) dried product exhibited and NH4NO3Together be added to equipped with ethyl alcohol conical flask in be vigorously stirred, by from
Sub- exchange process removes the dried product exhibited organic matter cetyl trimethylammonium bromide remained on surface, and then vacuum drying is
It can get the nanofiber-based hud typed adsorbent material of magnetic silicon oxide.
6. according to the method described in claim 5, in step (1), the solid content of the silicon oxide nanofiber suspension is
10g/L, the silicon oxide nanofiber are to extract in choysotile；The organic solvent is triethylene glycol, triethylene glycol, sweet
Any one in oil, octadecylene etc..
7. according to the method described in claim 5, in step (2), the quality of silicon oxide nanofiber solid and ferric acetyl acetonade
Than for 1:1 ~ 3:8；20~40min of the magnetic agitation time；The protective gas being passed through is high pure nitrogen, and gas is passed through the time
For 3min or more.
8. being protected according to the method described in claim 5, constant temperature-condensing reflux temperature in step (3) is maintained at 258 ~ 278 DEG C
The warm time is 20 ~ 40min.
9. according to the method described in claim 5, the volume ratio of water and ethyl alcohol in mixed solution described in step (4) be 2:3 ~
3:2, total volume are 120 ~ 160mL, and the volume of concentrated ammonia liquor is 1 ~ 5mL, and the quality that cetyl trimethylammonium bromide is added is 0.1
~0.5g；The silicon source is one or more of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester or butyl silicate
Mixture.
10. according to the method described in claim 5, ethyl alcohol volume is 60 ~ 100mL, NH in step (5)4NO3Quality be 1 ~ 2g,
The time of stirring is 30 ~ 60min.
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| CN201810730604.XA Pending CN109012568A (en) | 2018-07-06 | 2018-07-06 | A kind of nanofiber-based hud typed adsorbent material of magnetic silicon oxide and preparation method thereof |
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| KR101068500B1 (en) * | 2010-03-18 | 2011-09-29 | 경상대학교산학협력단 | Ultraefficient separation and sensing of mercury and methylmercury ions in drinking water by using aminonaphthalimide-functionalized fe3o4@sio2 core/shell magnetic nanoparticles |
| CN102389771A (en) * | 2011-10-17 | 2012-03-28 | 江苏大学 | Method for preparing bell type magnetic mesoporous silica-microsphere absorbent |
| CN102688760A (en) * | 2012-06-07 | 2012-09-26 | 北京科技大学 | Fe3O4/CuO/pSiO2 catalyst and preparation method thereof |
| CN102794140A (en) * | 2012-08-30 | 2012-11-28 | 东华大学 | Preparation method of grain size-controllable nuclear shell Fe3O4/SiO2 nanoparticle |
| CN104056633A (en) * | 2014-06-18 | 2014-09-24 | 太原理工大学 | Preparation method of SiO2-coated core-shell structure catalyst |
| CN106861697A (en) * | 2017-02-27 | 2017-06-20 | 中南大学 | New class fenton catalyst that a kind of ferroferric oxide nano granules are combined with silicon oxide nanofiber and preparation method thereof |
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Patent Citations (6)
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| KR101068500B1 (en) * | 2010-03-18 | 2011-09-29 | 경상대학교산학협력단 | Ultraefficient separation and sensing of mercury and methylmercury ions in drinking water by using aminonaphthalimide-functionalized fe3o4@sio2 core/shell magnetic nanoparticles |
| CN102389771A (en) * | 2011-10-17 | 2012-03-28 | 江苏大学 | Method for preparing bell type magnetic mesoporous silica-microsphere absorbent |
| CN102688760A (en) * | 2012-06-07 | 2012-09-26 | 北京科技大学 | Fe3O4/CuO/pSiO2 catalyst and preparation method thereof |
| CN102794140A (en) * | 2012-08-30 | 2012-11-28 | 东华大学 | Preparation method of grain size-controllable nuclear shell Fe3O4/SiO2 nanoparticle |
| CN104056633A (en) * | 2014-06-18 | 2014-09-24 | 太原理工大学 | Preparation method of SiO2-coated core-shell structure catalyst |
| CN106861697A (en) * | 2017-02-27 | 2017-06-20 | 中南大学 | New class fenton catalyst that a kind of ferroferric oxide nano granules are combined with silicon oxide nanofiber and preparation method thereof |
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Application publication date: 20181218 |