CN108526478A - Nanogold-mesoporous silicon oxide composite material and preparation method - Google Patents
Nanogold-mesoporous silicon oxide composite material and preparation method Download PDFInfo
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- CN108526478A CN108526478A CN201710115884.9A CN201710115884A CN108526478A CN 108526478 A CN108526478 A CN 108526478A CN 201710115884 A CN201710115884 A CN 201710115884A CN 108526478 A CN108526478 A CN 108526478A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to nanometer mesoporous gold silicon dioxide composite materials and preparation method thereof, this method is using nanogold as raw material, using Quaternary ammonium bromide as template, a certain amount of 1 is added into the reaction solution containing a certain proportion of Quaternary ammonium bromide, water, alcohol and alkali, 2 two (triethoxysilyl) ethane, template is removed after reaction, to obtain nanometer mesoporous gold silicon dioxide composite material.The preparation method of the present invention is simple, and the nanometer mesoporous gold silicon dioxide composite material obtained has " two-sided god " structure, and the pattern of nanometer mesoporous gold silicon dioxide composite material is uniform, stability is excellent, its pattern is controllable.
Description
Technical field
The present invention relates to field of nanometer material technology, more particularly to nanogold-mesoporous silicon oxide with " two-sided god " structure
Composite material and preparation method.
Background technology
Nano material be in current new material research field it is most dynamic, have very to the future economy and social development
Important component the most active in the research object and nanosecond science and technology of great influence, closest to application.With block materials
It compares, the particle of nanoscale has unique physics, chemical property.Gold nanoparticle is most stable of in metal nanoparticle
One of nano-particle has unique physical and chemical performance, gets more and more people's extensive concerning.
However, simple nanogold particle is unstable when environment changes under normal conditions, easily reuniting generates precipitation, these
The presence of destabilizing factor promotes people to go to try to explore more effective nanogold particle surface modification method.Due to mesoporous state
Silica (mSiO2) on mesoporous and huge specific surface area can effectively load it is various treatment diseases Medicine small molecules
Or imaging probe, it can be further developed into as multifunctional nanocomposites for being imaged, diagnosing, treat, therefore mSiO2Packet
Nanogold particle (the Au@mSiO covered2) there is good application advantage.
The appearance and size of nano material determines the physics and chemical property of nano material, in the pattern of a variety of nano materials
On, based on the excellent property of " two-sided god " structure and its in multiple fields, such as catalysis, self assembly, imaging, signal detection and medicine
The extensive use of the multiple fields such as object conduction so that " two-sided god " structure is got the attention.The nanometer of " two-sided god " structure
Material has carried out asymmetric modification due to its surface so that it becomes anisotropy from isotropism, and then can carry out more multiple
Miscellaneous, controllable and orientation assembling.
The preparation method of nanogold-silicon dioxide composite material in the prior art, the structure of the composite material prepared
Generally nucleocapsid, i.e. mesoporous silicon oxide are completely encapsulated in as shell outside nanogold material, during nanogold material is used as
Heart core, the composite material of this nucleocapsid is due to for isotropism, greatly limiting nanogold-silica composite wood
The versatile of material.
Based on above-mentioned analysis, nanogold-silica composite wood with " two-sided god " structure of high yield how is prepared
Expect and carry out the regulation and control of selectivity to the shape characteristic of the composite material to be one of current problem to be solved.In addition, mesh
The synthetic method of preceding major part nanogold-silicon dioxide composite material can only all prepare spherical structure, be difficult to realize different component
Pattern accurately control.
Invention content
For the above problem of the prior art, the present invention provides a kind of nanogold-with " two-sided god " structure is mesoporous
Silicon dioxide composite material and preparation method thereof, the preparation method is simple, the nanogold-with " two-sided god " structure obtained
The pattern of meso-porous titanium dioxide silicon composite is uniform, stability is excellent and its pattern is controllable.
To solve the above problems, the preparation method of nanogold-meso-porous titanium dioxide silicon composite of the present invention, including it is as follows
Step：
A) nanogold material is prepared, and the nanogold material is dispersed in quaternary ammonium bromide salting liquid, obtains nanogold
Solution；
B) nano-Au solution obtained in the step a) is added to containing the Quaternary ammonium bromide, water, alcohol and alkali
In aqueous solution, and certain time is stirred, obtains reaction solution；Wherein, the Quaternary ammonium bromide is template；
C) a certain amount of 1,2- bis- (triethoxysilyl) ethane is added to reaction obtained in the step b)
Solution, and quickly stir, then under 10~60 DEG C of temperature condition, react 1~4 hour；
D) Primary product is obtained by centrifugation, and the Primary product is distributed in a certain amount of alcohol, then remove institute
Quaternary ammonium bromide template is stated, to obtain nanogold-meso-porous titanium dioxide silicon composite.
Preferably, the nano-Au solution in the step b) and step c), the Quaternary ammonium bromide, the water, institute
State alcohol, the alkali, the 1,2- bis- (triethoxysilyl) ethane volume ratio be 1~5:1~5:10~50:1~5:
0.1~3:0.01~1.
Preferably, the Quaternary ammonium bromide is cetyl trimethylammonium bromide, and the alcohol is ethyl alcohol, and the alkali is ammonia
Water.
Preferably, a concentration of 20~50mg/ml of the cetyl trimethylammonium bromide, the quality percentage of the ammonium hydroxide
Than being 10~30%.
Preferably, the reaction solution in the step c) first reacts 1~2 hour under 15~30 DEG C of temperature conditions,
It then proceedes to react 1~2 hour under 50~60 DEG C of temperature conditions.
Preferably, contain cetyl trimethyl in the reaction system of the preparation nanogold material in the step a)
One or more aqueous solutions in ammonium bromide, hexadecyltrimethylammonium chloride and enuatrol are as growth-promoting media, the reactant
Contain ascorbic acid in system as reducing agent, three hydration gold chlorides are contained in the reaction system as presoma.
Preferably, the Quaternary ammonium bromide template is removed by ethyl alcohol extraction in the step d).
Preferably, the Primary product in the step d) is distributed in 1~10ml ethyl alcohol, obtains dispersion solution；Then
The dispersion solution is added in ammonium nitrate ethanol solution, wherein the ammonium nitrate ethanol solution concentration is 5~8mg/ml；
It is extracted 15~30 hours under 50~80 DEG C of temperature conditions, and condensing reflux obtains nanogold-meso-porous titanium dioxide silicon composite.
The present invention also provides the nanometers that a kind of preparation method of above-mentioned nanogold-meso-porous titanium dioxide silicon composite obtains
Gold-meso-porous titanium dioxide silicon composite, the nanogold-meso-porous titanium dioxide silicon composite have " two-sided god " structure.
Preferably, the form of nanogold is nanometer gold bar or nanometer in the nanogold-meso-porous titanium dioxide silicon composite
Any one in Golden Triangle piece or nanogold particle.
Compared with prior art, the present invention has the advantages that：
1) preparation method of nanogold provided by the invention-meso-porous titanium dioxide silicon composite is simple, yield is high, avoids
Complicated, cumbersome operation.
2) shape (such as nanometer gold bar, nanogold of the shape of the mesoporous silicon oxide in the present invention by nanogold material
Grain and nanogold triangular plate) influence.It can be accurate such as reaction temperature and surfactant concentration by adjusting response parameter
Control the general morphology and relative position of each component.
3) good dispersion property, the size uniformity of the nanogold-meso-porous titanium dioxide silicon composite prepared using the present invention,
Energy with good stability.
Description of the drawings
Fig. 1：
(a) transmission electron microscope photo of the nanometer gold bar prepared for the embodiment of the present invention 1；
(b) transmission electron microscope photo of the nanogold-meso-porous titanium dioxide silicon composite prepared for the embodiment of the present invention 1；
(c) scanning transmission electron microscope of the nanogold-meso-porous titanium dioxide silicon composite prepared for the embodiment of the present invention 1 shines
Piece；
(d) it is that nanogold-angle of elevation annular dark field of meso-porous titanium dioxide silicon composite-prepared by the embodiment of the present invention 1 is swept
Retouch transmission electron microscope photo and corresponding X-ray energy disperse spectrogram；
(e)~(h) is nanogold-meso-porous titanium dioxide silicon composite of the embodiment of the present invention 1 under the differential responses time
Transmission electron microscope photo；
(i) growth for the nanogold-meso-porous titanium dioxide silicon composite with " two-sided god " structure simulated for the present invention
Mechanism figure；
Wherein, the scale of (d)~(h) is 100nm；
Fig. 2：
(a)~(c) is nanogold-meso-porous titanium dioxide silicon composite of the embodiment of the present invention 1 at a temperature of differential responses
The transmission electron microscope photo of growth morphology situation；
(d)~(f) is that nanogold-mesoporous silicon oxide of the embodiment of the present invention 1 under different surfaces surfactant concentration is multiple
The transmission electron microscope photo of condensation material growth morphology situation；
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art obtained without making creative work it is all its
His embodiment, shall fall within the protection scope of the present invention.
The present invention provides a kind of nanogold-mesoporous silicon oxide composite material and preparation method, the preparation method packets
Include following steps：
A) nanogold material is prepared, and the nanogold material is dispersed in quaternary ammonium bromide salting liquid, obtains nanogold
Solution；
B) nano-Au solution obtained in the step a) is added to containing the Quaternary ammonium bromide, water, alcohol and alkali
In aqueous solution, and certain time is stirred, obtains reaction solution；Wherein, the Quaternary ammonium bromide is template；
C) a certain amount of 1,2- bis- (triethoxysilyl) ethane is added to reaction obtained in the step b)
Solution, and quickly stir, then under 10~60 DEG C of temperature condition, react 1~4 hour；
D) Primary product is obtained by centrifugation, and the Primary product is distributed in a certain amount of alcohol, then remove institute
Quaternary ammonium bromide template is stated, to obtain nanogold-meso-porous titanium dioxide silicon composite.
Wherein, the Quaternary ammonium bromide is preferably cetyl trimethylammonium bromide；The alcohol is preferably ethyl alcohol；The alkali
Preferably concentrated ammonia liquor.
Specifically, the nano-Au solution, the Quaternary ammonium bromide in the step b) and step c), the water, institute
State alcohol, the alkali, the 1,2- bis- (triethoxysilyl) ethane volume ratio be 1~5:1~5:10~50:1~5:
0.1~3:0.01~1.Preferably, a concentration of 20~50mg/ml of cetyl trimethylammonium bromide, the quality of the ammonium hydroxide
Percentage is 10~30%.
Preferably, the reaction solution in the step c) first reacts 1~2 hour under 15~30 DEG C of temperature conditions,
It then proceedes to react 1~2 hour under 50~60 DEG C of temperature conditions.
Preferably, contain cetyl trimethyl in the reaction system of the preparation nanogold material in the step a)
One or more aqueous solutions in ammonium bromide, hexadecyltrimethylammonium chloride and enuatrol are as growth-promoting media, the reactant
Contain ascorbic acid in system as reducing agent, three hydration gold chlorides are contained in the reaction system as presoma.
Preferably, the Quaternary ammonium bromide template is removed by ethyl alcohol extraction in the step d).
Preferably, the Primary product in the step d) is distributed in 1~10ml ethyl alcohol, obtains dispersion solution；Then
The dispersion solution is added in ammonium nitrate ethanol solution, wherein the ammonium nitrate ethanol solution concentration is 5~8mg/ml；
It is extracted 15~30 hours under 50~80 DEG C of temperature conditions, and condensing reflux obtains nanogold-meso-porous titanium dioxide silicon composite.
In order to further illustrate the present invention, with reference to embodiments to nanogold-mesoporous silicon oxide provided by the invention
The preparation method of composite material is described in detail.
Reagent used in following embodiment is commercially available.
Embodiment 1
The preparation of nanometer gold bar-meso-porous titanium dioxide silicon composite.
The cetyl trimethylammonium bromide solution 10mL of 0.1mol/L is configured, three water of 25.4mmol/L are added thereto
100 μ L of chlorauric acid solution are closed, 10min is stirred with the rotating speed of 400rmp at room temperature.The boron of 0.01mol/L is first drawn with syringe
Sodium hydride solution 0.6mL, then deionized water 0.4mL is drawn, and be rapidly injected in the solution of aforementioned stirring, to which seed be made
Liquid places 2 hours for use.
It weighs 0.7g cetyl trimethylammonium bromides and 0.1243g enuatrols and is added in 50mL deionized waters, wait for
Silver hydroxide (AgOH) solution 2mL of 4mmol/L is added in it after being completely dissolved, the three of 25.4mmol/L is added after stirring 15min
It is hydrated chlorauric acid solution 0.984mL, the concentrated hydrochloric acid of 0.3mL is added after solution fades completely, is vigorously stirred and is added after 20min
The ascorbic acid 0.125mL of 64mmol/L and 40 μ L seed liquors.
After above-mentioned reaction 5~6 hours, 10min is centrifuged under the rotating speed of 8000rpm, sucks supernatant liquor, obtains nanogold
Stick.The nanometer gold bar of acquisition is analyzed using transmission electron microscope, obtains its transmission electron microscope photo, in Fig. 1 shown in (a).
The nanometer gold bar of gained is dispersed in cetyl trimethylammonium bromide, the ten of the nanometer gold bar of about 2mL are made into
Six alkyl trimethyl ammonium bromide aqueous solutions, ultrasound make above-mentioned aqueous solution be completely dispersed, for use.
The cetyl trimethylammonium bromide aqueous solution of the nanometer gold bar of 1mL is added in conical flask, wherein conical flask
In include 20mL pure water, 1.5mL (45mg/mL) cetyl trimethylammonium bromide, 1.5mL ethyl alcohol and 0.55mL (28 wt.%)
Ammonium hydroxide.After forty minutes, by 30 μ L 1,2- bis- (triethoxysilyl) ethane is rapidly injected in conical flask simultaneously acutely for stirring
Stirring 30 seconds, is then reduced to 400rmp by rotating speed, and after being reacted 1.5 hours at 26 DEG C, it is small to be heated to 55 DEG C the reaction was continued 1.5
When.
Obtained Primary product is centrifuged 8 minutes under the rotating speed of 10000rmp, 5mL is dispersed in after being cleaned once with ethyl alcohol
Ethyl alcohol in, obtain dispersion solution.The above-mentioned dispersion solution of 5mL is added in ammonium nitrate ethanol solution, wherein ammonium nitrate ethyl alcohol
Contain 1.2g ammonium nitrate and 200mL ethyl alcohol in solution；It is extracted 24 hours under 70 DEG C of temperature conditions, and condensing reflux obtains nanometer
Golden stick-meso-porous titanium dioxide silicon composite.
Nanometer gold bar-meso-porous titanium dioxide the silicon composite obtained is carried out using transmission electron microscope and scanning transmission electron microscope
Analysis, respectively obtains transmission electron microscope photo and the scanning transmission electron microscope photo as shown in Fig. 1 (c) as shown in Fig. 1 (b).Into one
Step, it is compound to the nanometer gold bar-mesoporous silicon oxide obtained using angle of elevation annular dark field-scanning transmission electron microscope and energy disperse spectroscopy
Material is analyzed, and angle of elevation annular dark field-scanning transmission electron microscope photo and corresponding X-ray as shown in Fig. 1 (d) are obtained
Energy dispersion spectrogram.By above-mentioned phenetic analysis it is found that nanogold manufactured in the present embodiment-meso-porous titanium dioxide silicon composite tool
There is " two-sided god " structure.
The present embodiment is further, to the different experiments reaction time to nanometer gold bar-meso-porous titanium dioxide silicon composite
The influence of pattern is studied, and is analyzed using transmission electron microscope, is obtained as shown in Fig. 1 (e)~(h) in differential responses
Between under nanogold-meso-porous titanium dioxide silicon composite transmission electron microscope photo, wherein (e) reaction time be 3min, (f) react
Time is 5min, and (g) reaction time is 10min, and (h) reaction time is 3h.
The present embodiment is also to different experiments reaction temperature to the shadow of the pattern of nanometer gold bar-meso-porous titanium dioxide silicon composite
Sound is studied, and is analyzed using transmission electron microscope, and the receiving at a temperature of differential responses as shown in Fig. 2 (a)~(c) is obtained
The transmission electron microscope photo of meter Jin-meso-porous titanium dioxide silicon composite growth morphology situation, wherein (a) reaction temperature is 26 DEG C,
(b) reaction temperature is 22 DEG C, and (c) reaction temperature is 18 DEG C.
The present embodiment is further, to the concentration of different surfaces lammonium bromide to nanogold
The influence of the pattern of stick-meso-porous titanium dioxide silicon composite is studied, and is analyzed using transmission electron microscope, is obtained such as Fig. 2
(d) nanogold-meso-porous titanium dioxide silicon composite growth morphology situation shown in~(f) under different surfaces surfactant concentration
Transmission electron microscope photo, wherein a concentration of 45mg/mL of (d), (e) and the concentration of (f) gradually increase.
The growth mechanism of nanogold-meso-porous titanium dioxide silicon composite with " two-sided god " structure prepared by the present invention
See shown in Fig. 1 (i), for the nanogold-meso-porous titanium dioxide silicon composite with " two-sided god " structure of the invention simulated
Growth mechanism figure.
Embodiment 2
The preparation of nanogold triangular plate-mesoporous silicon oxide composite material.
It is added under 0.1mol/L hexadecyltrimethylammonium chlorides 16mL, 200rpm rotating speed and stirs in 80mL deionized waters
Mix, be then added three hydration chlorauric acid solution 800 μ L of 25.4mmol/L, 750 μ L of liquor kalii iodide of 0.01mol/L,
The 800 μ L of ascorbic acid solution of 100 μ L of 0.1mol/L sodium hydroxide solutions, 64mmol/L, are eventually adding 0.1mol/L hydroxides
100 μ L of sodium solution.
By above-mentioned solution left standstill 15 minutes, is centrifuged 8 minutes with the rotating speed of 8000rpm, suck supernatant, obtain nanogold three
Cornual plate.The nanogold triangular plate of gained is dispersed in cetyl trimethylammonium bromide, the nanogold triangular plate of about 2mL is made into
Cetyl trimethylammonium bromide aqueous solution, ultrasound makes above-mentioned aqueous solution be completely dispersed, for use.
The cetyl trimethylammonium bromide aqueous solution of 1mL nanogold triangular plates is added in conical flask, wherein taper
Include 20mL pure water, 1.5mL (45mg/mL) cetyl trimethylammonium bromide, 1.5mL ethyl alcohol and 0.55mL (28 in bottle
Wt.%) ammonium hydroxide.After forty minutes, by 30 μ L 1,2- bis- (triethoxysilyl) ethane is rapidly injected in conical flask for stirring
And be vigorously stirred 30 seconds, rotating speed is then reduced to 400rmp, after being reacted 1.5 hours at 26 DEG C, 55 DEG C is heated to and continues instead
It answers 1.5 hours.
Obtained Primary product is centrifuged 8 minutes under the rotating speed of 10000rmp, 5mL is dispersed in after being cleaned once with ethyl alcohol
Ethyl alcohol in, obtain dispersion solution.The above-mentioned dispersion solution of 5mL is added in ammonium nitrate ethanol solution, wherein ammonium nitrate ethyl alcohol
Contain 1.2g ammonium nitrate and 200mL ethyl alcohol in solution；It is extracted 24 hours under 70 DEG C of temperature conditions, and condensing reflux obtains nanometer
Golden Triangle piece-meso-porous titanium dioxide silicon composite.
Embodiment 3
The preparation of nanogold particle-meso-porous titanium dioxide silicon composite.
0.1mol/L cetyl trimethylammonium bromide 16mL are added in 80mL deionized waters, are then added
Three 800 μ L of hydration chlorauric acid solution of 25.4mmol/L, the ascorbic acid solution 1mL of 64mmol/L, are slowly added to 0.2mol/L
Sodium hydroxide solution 1mL.
15 minutes are stood, is centrifuged 20 minutes with the rotating speed of 11000rpm, is sucked supernatant, obtain nanogold particle.By institute
The nanogold particle obtained is dispersed in cetyl trimethylammonium bromide, is made into the cetyl three of the nanogold particle of about 2mL
Methyl bromide aqueous ammonium, ultrasound make above-mentioned aqueous solution be completely dispersed, for use.
The cetyl trimethylammonium bromide aqueous solution of 1mL nanogold particles is added in conical flask, wherein conical flask
In include 20mL pure water, 1.5mL (45mg/mL) cetyl trimethylammonium bromide, 1.5mL ethyl alcohol and 0.55mL (28 wt.%)
Ammonium hydroxide.After forty minutes, by 30 μ L 1,2- bis- (triethoxysilyl) ethane is rapidly injected in conical flask simultaneously acutely for stirring
Stirring 30 seconds, is then reduced to 400rmp by rotating speed, and after being reacted 1.5 hours at 26 DEG C, it is small to be heated to 55 DEG C the reaction was continued 1.5
When.
Obtained Primary product is centrifuged 8 minutes under the rotating speed of 10000rmp, 5mL is dispersed in after being cleaned once with ethyl alcohol
Ethyl alcohol in, obtain dispersion solution.The above-mentioned dispersion solution of 5mL is added in ammonium nitrate ethanol solution, wherein ammonium nitrate ethyl alcohol
Contain 1.2g ammonium nitrate and 200mL ethyl alcohol in solution；It is extracted 24 hours under 70 DEG C of temperature conditions, and condensing reflux obtains nanometer
Gold particle-meso-porous titanium dioxide silicon composite.
Compared with prior art, the present invention has the advantages that：
1) preparation method of nanogold provided by the invention-meso-porous titanium dioxide silicon composite is simple, yield is high, avoids
Complicated, cumbersome operation.
2) shape (such as nanometer gold bar, nanogold of the shape of the mesoporous silicon oxide in the present invention by nanogold material
Grain and nanogold triangular plate) influence.It can be accurate such as reaction temperature and surfactant concentration by adjusting response parameter
Control the general morphology and relative position of each component.
3) good dispersion property, the size uniformity of the nanogold-meso-porous titanium dioxide silicon composite prepared using the present invention,
Energy with good stability.
Above description has fully disclosed the specific implementation mode of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change for being done of specific implementation mode of the present invention all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (10)
1. the preparation method of nanogold-meso-porous titanium dioxide silicon composite, which is characterized in that described method includes following steps：
A) nanogold material is prepared, and the nanogold material is dispersed in quaternary ammonium bromide salting liquid, obtains nano-Au solution；
B) nano-Au solution obtained in the step a) is added to containing the water-soluble of the Quaternary ammonium bromide, water, alcohol and alkali
In liquid, and certain time is stirred, obtains reaction solution；Wherein, the Quaternary ammonium bromide is template；
C) a certain amount of 1,2- bis- (triethoxysilyl) ethane is added to reaction solution obtained in the step b),
And quickly stir, then under 10~60 DEG C of temperature condition, react 1~4 hour；
D) Primary product is obtained by centrifugation, and the Primary product is distributed in a certain amount of alcohol, then remove the bromine
Change quaternary ammonium salt template, to obtain nanogold-meso-porous titanium dioxide silicon composite.
2. the preparation method of nanogold according to claim 1-meso-porous titanium dioxide silicon composite, which is characterized in that institute
The nano-Au solution in step b) and step c), the Quaternary ammonium bromide, the water, the alcohol, the alkali, described 1 are stated,
The volume ratio of 2- bis- (triethoxysilyl) ethane is 1~5:1~5:10~50:1~5:0.1~3:0.01~1.
3. the preparation method of nanogold according to claim 2-meso-porous titanium dioxide silicon composite, which is characterized in that institute
It is cetyl trimethylammonium bromide to state Quaternary ammonium bromide, and the alcohol is ethyl alcohol, and the alkali is ammonium hydroxide.
4. the preparation method of nanogold according to claim 3-meso-porous titanium dioxide silicon composite, which is characterized in that institute
A concentration of 20~50mg/ml of cetyl trimethylammonium bromide is stated, the mass percent of the ammonium hydroxide is 10~30%.
5. the preparation method of nanogold according to claim 1-meso-porous titanium dioxide silicon composite, which is characterized in that institute
It states the reaction solution in step c) first to react 1~2 hour under 15~30 DEG C of temperature conditions, then proceed at 50~60 DEG C
It is reacted 1~2 hour under temperature condition.
6. the preparation method of nanogold according to claim 1-meso-porous titanium dioxide silicon composite, which is characterized in that institute
It states in the reaction system of the preparation nanogold material in step a) containing cetyl trimethylammonium bromide, cetyl three
One or more aqueous solutions in ammonio methacrylate and enuatrol are made in the reaction system containing ascorbic acid as growth-promoting media
For reducing agent, three hydration gold chlorides are contained in the reaction system as presoma.
7. the preparation method of nanogold according to claim 1-meso-porous titanium dioxide silicon composite, which is characterized in that institute
It states in step d) and the Quaternary ammonium bromide template is removed by ethyl alcohol extraction.
8. the preparation method of nanogold according to claim 7-meso-porous titanium dioxide silicon composite, which is characterized in that will
Primary product in the step d) is distributed in 1~10ml ethyl alcohol, obtains dispersion solution；Then the dispersion solution is added
Into ammonium nitrate ethanol solution, wherein the ammonium nitrate ethanol solution concentration is 5~8mg/ml；Under 50~80 DEG C of temperature conditions
Extraction 15~30 hours, and condensing reflux obtains nanogold-meso-porous titanium dioxide silicon composite.
9. the preparation method of nanogold-meso-porous titanium dioxide silicon composite as described in claim 1~8 any one obtains
Nanogold-meso-porous titanium dioxide silicon composite, which is characterized in that the nanogold-meso-porous titanium dioxide silicon composite has " double
Face god " structure.
10. nanogold according to claim 9-meso-porous titanium dioxide silicon composite, which is characterized in that the nanogold-
The form of nanogold is times in nanometer gold bar or nanogold triangular plate or nanogold particle in meso-porous titanium dioxide silicon composite
Meaning is a kind of.
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| CN201710115884.9A CN108526478A (en) | 2017-03-01 | 2017-03-01 | Nanogold-mesoporous silicon oxide composite material and preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110104654A (en) * | 2019-05-14 | 2019-08-09 | 安徽大学 | A kind of Janus type porous silica composite nanoparticle and preparation method thereof |
| CN110903846A (en) * | 2019-11-27 | 2020-03-24 | 安徽启东热能科技有限公司 | Desulfurizing agent for improving sulfur removal efficiency in petroleum industry |
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| CN102319435A (en) * | 2011-06-20 | 2012-01-18 | 复旦大学 | Mesoporous silica compound particles containing gold nanorods, preparation method and application thereof |
| CN104525941A (en) * | 2014-12-11 | 2015-04-22 | 华中科技大学 | Preparation method for cladding gold nanoparticles with mesoporous silica |
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| CN102319435A (en) * | 2011-06-20 | 2012-01-18 | 复旦大学 | Mesoporous silica compound particles containing gold nanorods, preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110104654A (en) * | 2019-05-14 | 2019-08-09 | 安徽大学 | A kind of Janus type porous silica composite nanoparticle and preparation method thereof |
| CN110903846A (en) * | 2019-11-27 | 2020-03-24 | 安徽启东热能科技有限公司 | Desulfurizing agent for improving sulfur removal efficiency in petroleum industry |
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