CN107617750A - The method for preparing Ag/ redox graphene composite nano materials - Google Patents
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Abstract
The invention provides the method for preparing Ag/ redox graphene composite nano materials.First by AgNO3, sodium citrate, lauryl sodium sulfate, graphene oxide be configured to water solution A, sodium borohydride is each configured to the aqueous solution B, C with NaOH.Water solution A, aqueous solution B, normal octane are then passed through first capillary microreactor simultaneously, water solution A quickly mixes with aqueous solution B, and independent drop is separated into by normal octane, reaction mass is after capillary microreactor outflow, flow directly into second capillary microreactor to be reacted with aqueous solution C, reaction mass reacts under certain temperature.Ag/ redox graphene composite nano materials finally are prepared through centrifuging, washing.The present invention have the advantages that process is continuous, technique is simple, reaction condition is gentle, obtain in Ag/ redox graphene composite Nano materials Ag load capacity height, particle diameter is small, particle diameter distribution is narrow, reproducible between batch.
Description
Technical field
The invention belongs to Materials Science and Engineering field, is related to one kind and oil-water two-phase flow system is utilized in micro passage reaction
The method for preparing standby Ag/ redox graphene composite nano materials.
Background technology
Ag nano-particles have very strong UV-Visible absorption drawn game area plasma resonance (Localized
Surface Plasmon Resonance, LSPR) etc. property, in SERS (SERS) and nonlinear optics etc.
Aspect is with a wide range of applications.Due to the unique optical property of Ag nano-particles, Ag nano-particles are answered with some semiconductors
Close the composite nanoparticle formed also has huge contribution in catalytic degradation organic pollution etc..Research finds that Ag receives
The optical property of rice corpuscles has close contact with pattern, particle diameter.Therefore, to avoid the reunion of Ag nano-particles, regulation and control are received
The pattern of rice corpuscles, research worker introduce graphene as the scattered carrier for supporting Ag nano-particles.Graphene has single
Atomic layer level thickness and good electric conductivity, it is a kind of excellent backing material.Research is found, prepares Ag- graphene composite Nanos
Material, Ag nano-particles can be dispersed in graphenic surface well, the effective Ag nano-particles that suppress are reunited, and can be avoided
Cause electric conductivity to be deteriorated because of the presence of surfactant, significantly expand the application of Ag nano-particles.It is also possible to keep away
Exempt from the stacking of graphene, keep the good dispersiveness of graphene.
However, so far, the method for preparing Ag- graphene composite nano materials is complex.Xu et al. research
“Graphene Metal Particle Nanocomposites,J.Phys.Chem.C,2008,112:19841-19845 ",
First graphene oxide, ethylene glycol are mixed with certain density metallic precursor solution, 6h is reacted in 100 DEG C of oil baths and is prepared into
To metal (Au, Pt, Pd)-graphene composite nanoparticle.Organic reagent used in this method not environmentally answers subsequent treatment
Miscellaneous, time-consuming, limits the extensive use of this method.
Zhou et al. research " In Situ Synthesis of Metal Nanoparticles on Single-
Layer Graphene Oxide and Reduced Graphene Oxide Surfaces,J.Phys.Chem.C,2009,
113:10842-10846 ", graphene oxide is heated to 75 DEG C in silver nitrate solution, is incubated 30min afterwards, obtains particle diameter
In the Ag- graphene composite nanoparticles that several nanometers to 200nm do not wait.This method is intermittent operation, and time-consuming, particle diameter point
Cloth is wide, Ag nano particle diameters are larger, limits the industrialized production of this method.
Pasricha et al. research " A facile and nove synthesis of Ag-graphene-based
nanocomposites,Small,2009,5:2253-2259 ", Ag- graphene composite nanoparticles are synthesized by two-step process.First
The mixed solution of graphene oxide, potassium hydroxide and silver sulfate is heated to boiling and is prepared that Ag- graphene oxides are compound to be received
Rice corpuscles, then be passed through hydrazine steam reduction and obtain Ag- graphene composite nanoparticles.This method is intermittent operation, two-step reaction,
Process is cumbersome, and time-consuming, and non-normal temperature increases energy consumption, and this method can not also realize continuous production.
To sum up, the preparation process of Ag- graphenes composite nanoparticle is mostly the interval behaviour carried out in traditional reactor at present
Make, low production efficiency, granularity heterogeneity, the Ag particle diameters of load are generally larger, and load capacity is not high, poor repeatability between batch.For gram
Disadvantages mentioned above is taken, need to develop one kind both can continuously produce in enormous quantities, make to repeat between gained nano material uniform particle diameter and batch again
The good method of property.Micro- Chemical Engineering Technology is a kind of process intensification technology risen the 1990s, compared with conventional art, is had
Small volume, specific surface area are big, transfer performance is good, the advantages that being easily integrated.There is unique advantage in field of inorganic material preparing technology,
Microreactor can strengthen mixing, form the reaction environment of stable uniform, and product can remove in time, reunite so as to reduce, make institute
Nano material particle diameter distribution is narrow and batch between it is reproducible.In addition, the nano material preparation process based on micro- Chemical Engineering Technology is
Continuous operation mode, it is easy to mass produce.However, because micro passage reaction channel size is smaller, nano material is being prepared
During be difficult avoid blockage problem.Therefore, the application is prepared for Ag/ reduction in micro passage reaction using oil-water two-phase flow
Graphene oxide composite nanoparticle, you can improve nano particle diameter homogeneity, mixed because microreactor can be strengthened
Journey, Ag load capacity is big in the Ag/ redox graphene composite nanoparticles being prepared, and particle diameter is smaller, average grain diameter control
In below 5nm, but also the blocking of micro passage reaction can be avoided.
The content of the invention
It is an object of the invention to based on micro passage reaction, there is provided one kind prepares sea urchin shape Ag/ using oil-water two-phase flow
The method of redox graphene composite nano materials.It is an advantage of the invention that process is continuous, technique is simple, reaction condition temperature
Asked with, Ag/ redox graphene composite nanoparticle patterns and uniform particle diameter, average grain diameter control in below 5nm, without blocking
Topic.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
The method for preparing Ag/ redox graphene composite nano materials, water-oil phase is utilized in micro passage reaction
Stream is continuous to prepare Ag/ redox graphene composite nano materials, it is characterised in that：
(1) by AgNO3, sodium citrate, lauryl sodium sulfate, graphene oxide and water be configured to water solution A；
(2) sodium borohydride and NaOH and water are each configured to the aqueous solution B, C；
(3) water solution A, aqueous solution B, normal octane are passed through first capillary microreactor, water solution A and aqueous solution B
Quick mixing, and independent drop is separated into by normal octane, formed using two-phase of the normal octane as continuous phase, the aqueous solution for dispersed phase
Flowing；The microreactor or be the micro- reaction of transparent capillary that capillary microreactor is reaction channel side with transparent window
Device, the transparent window or transparent capillary microreactor of reaction channel are placed in water-bath and reacted；
In above-mentioned technical proposal, it is micro- to be directly entered second capillary after capillary microreactor outflow for reaction mass
Reactor, reacted with aqueous solution C, after centrifuge washing, Ag/ redox graphene composite Nano materials are finally prepared
Material.
In above-mentioned technical proposal, AgNO in water solution A3Molar concentration in water is 0.0001-0.001mol/L, preferably
0.0003-0.0007mol/L；Sodium citrate and AgNO3Molar ratio range be 1:1-5:1, preferably 1.2:1-3.5:1；12
Sodium alkyl sulfate and AgNO3Molar ratio range be 6:1-24:1, preferably 8:1-15:1.
In above-mentioned technical proposal, AgNO3It is 0.4 with the mass fraction scope on graphene oxide:1-0.03:1, preferably
0.3:1-0.2:1。
In above-mentioned technical proposal, molar concentration of the sodium borohydride in water is 0.0003-0.003mol/L in aqueous solution B,
Molar concentrations of the NaOH in water is 0.005-0.05mol/L.
In above-mentioned technical proposal, molar concentration of the sodium borohydride in water is 0.001-0.01mol/L in aqueous solution B,
Molar concentrations of the NaOH in water is 0.005-0.05mol/L.
In above-mentioned technical proposal, water solution A, aqueous solution B and aqueous solution C flow are 0.1-1.5mL/min, are preferably
0.3-0.9mL/min；Normal octane flow is 0.3-2.5mL/min, preferably 0.6-1.5mL/min.
In above-mentioned technical proposal, water solution A, aqueous solution B are identical with aqueous solution C flow.
In above-mentioned technical proposal, reaction temperature is 10-60 DEG C, preferably 20-40 DEG C.
In above-mentioned technical proposal, first capillary microreactor has reaction channel and three intake channels, is respectively
Fluid inlet channel I, fluid inlet channel II, fluid inlet channel III, three intake channel hydraulic diameters are identical or different, point
Wei not 0.2-1.2mm；The port of export of three fluid inlet channels connects with the arrival end of reaction channel respectively, fluid inlet channel
I is identical with the angle of fluid inlet channel III with fluid inlet channel II, fluid inlet channel II, is 30-90 °；Reaction channel
Hydraulic diameter and intake channel hydraulic diameter it is identical or different, be 0.2-1.2mm, reaction channel length is 2-10m.The aqueous solution
A, aqueous solution B is entered by the arrival end of three fluid inlet channels respectively with normal octane, starts to mix in reaction channel arrival end
Close and react.
In above-mentioned technical proposal, second capillary microreactor has reaction channel and two intake channels, is respectively
The outlet of fluid inlet channel IV, wherein fluid inlet channel V, fluid inlet channel IV and first capillary microreactor
End is connected, and two intake channel hydraulic diameters are identical or different, respectively 0.2-1.2mm；The outlet of two fluid inlet channels
End connects with the arrival end of reaction channel respectively, fluid inlet channel IV, fluid inlet channel V and fluid inlet channel VI
Angle is identical, is 30-90 °；The hydraulic diameter of reaction channel and intake channel hydraulic diameter are identical or different, are 0.2-1.2mm,
Reaction channel length is 0.5-5m.Aqueous solution C and first capillary microreactor port of export are entered by two liquid respectively
The arrival end of mouth passage enters, and starts mixing and reaction in reaction channel arrival end.
The particle size range of the loaded Ag of Ag/ redox graphene composite nano materials prepared by the present invention is 1-10nm.
Compared with prior art, the substantive distinguishing features of the protrusion possessed and significant progress are the present invention：
1. being based on micro passage reaction one-step synthesis Ag/ redox graphene composite nano materials, technique is simple, anti-
Answer mild condition, process continuous, the Ag/ redox graphene composite nano materials patterns and uniform particle diameter being prepared, bear
The Ag nano-particles average grain diameter control of load is reproducible between below 5nm, batch.
2. being used as oil phase by introducing normal octane, oil-water two-phase flow is formed, avoids microchannel blockage problem.
Brief description of the drawings
Fig. 1 is the process chart of the present invention, wherein, 1,2,3,4 be first, second, third, fourth syringe pump, and 5 be the
One capillary microreactor, 6 be fluid inlet channel I, and 7 be fluid inlet channel II, and 8 be fluid inlet channel III, and 9 be liquid
Body intake channel VI, 10 be second capillary microreactor, and 11 be water bath device.
Fig. 2 is the XRD spectra of Ag/ redox graphene composite nano materials prepared by embodiment 1.
Fig. 3 is the transmission electron microscope photo of Ag/ redox graphene composite nano materials prepared by embodiment 1.
Fig. 4 is the transmission electron microscope photo of Ag/ redox graphene composite nano materials prepared by embodiment 2.
Fig. 5 is the transmission electron microscope photo of Ag/ redox graphene composite nano materials prepared by embodiment 3.
Fig. 6 is the transmission electron microscope photo of Ag/ redox graphene composite nano materials prepared by comparative example 1.
Fig. 7 is the XRD spectra of Ag/ graphene oxide composite nano materials prepared by comparative example 2.
Fig. 8 is the degradation curve of p-nitrophenol.
Embodiment
Used microreactor is：One capillary microreactor has reaction channel and three intake channels, point
Not Wei fluid inlet channel I, fluid inlet channel II, fluid inlet channel III, three intake channel hydraulic diameters are identical, are
0.6mm；The port of export of three fluid inlet channels connects with the arrival end of reaction channel respectively, fluid inlet channel I and liquid
Intake channel II, fluid inlet channel II are identical with the angle of fluid inlet channel III, are 90 °；The hydraulic diameter of reaction channel
It is identical with intake channel hydraulic diameter, it is 0.6mm, reaction channel length is 4m.Water solution A, aqueous solution B and normal octane lead to respectively
The arrival end for crossing three fluid inlet channels enters, and starts mixing and reaction in reaction channel arrival end.
Second capillary microreactor has a reaction channel and two intake channels, respectively fluid inlet channel IV,
Fluid inlet channel V, wherein fluid inlet channel IV are connected with the port of export of first capillary microreactor, two imports
Passage hydraulic diameter is identical, is 0.6mm；The port of export of two fluid inlet channels connects with the arrival end of reaction channel respectively,
Fluid inlet channel IV, fluid inlet channel V are identical with the angle of fluid inlet channel VI, are 90 °；The waterpower of reaction channel
Diameter is identical with intake channel hydraulic diameter, is 0.6mm, and reaction channel length is 1m.Aqueous solution C and first capillary are micro- anti-
Answer the port of export of device to enter respectively by the arrival end of two fluid inlet channels, reaction channel arrival end start mixing with it is anti-
Should.
The present invention is further illustrated below by embodiment.
Embodiment 1
(1) by 0.00425g AgNO under the conditions of lucifuge3It is dissolved in 45mL deionized waters, 5mL oxidation stones is added then to it
Black alkene solution (2mg/mL) is made into AgNO3Molar concentration is 0.0005mol/L, graphene oxide concentration is the water-soluble of 0.2mg/mL
Liquid A, 0.15g lauryl sodium sulfate, 0.027g sodium citrates are then added thereto, stir 10 minutes, be allowed to be sufficiently mixed；
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized waters, is made into 0.0015mol/L's
NaBH4Aqueous solution B；
(3) by 0.04g NaOH, 0.00565g NaBH4It is dissolved in 50mL deionized waters, is made into 0.003mol/L NaBH4
Aqueous solution C；
(4) by water solution A, aqueous solution B, normal octane respectively with 0.2,0.2,0.6mL/min flow is by injecting infusion
Enter in first capillary microreactor, reacted in 40 DEG C of water-baths；
(5) aqueous solution C is injected in second capillary microreactor with 0.2mL/min flow by syringe pump,
Reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water is washed with ethanol alternating centrifugal, obtains Ag/ oxygen reductions
Graphite alkene composite nano materials, as shown in Figure 3.The XRD spectra of gained sample is as shown in Figure 2, it can be seen that gained Ag/ is reduced
Graphene oxide has been completely converted into graphene in graphene oxide composite nano materials, and Ag load capacity is 21.3wt%,
The average grain diameter of Ag nano-particles is 3.3nm.
Embodiment 2
(1) by 0.00425g AgNO under the conditions of lucifuge3It is dissolved in 45mL deionized waters, 5mL oxidation stones is added then to it
Black alkene solution (2mg/mL) is made into AgNO3Molar concentration is 0.0005mol/L, graphene oxide concentration is the water-soluble of 0.2mg/mL
Liquid A, 0.15g lauryl sodium sulfate, 0.027g sodium citrates are then added thereto, stir 10 minutes, be allowed to be sufficiently mixed；
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized waters, is made into 0.0015mol/L's
NaBH4Aqueous solution B；
(3) by 0.04g NaOH, 0.196g NaBH4It is dissolved in 50mL deionized waters, is made into 0.01mol/L NaBH4Water
Solution C；
(4) by water solution A, aqueous solution B, normal octane respectively with 0.3,0.3,0.4mL/min flow is by injecting infusion
Enter in first capillary microreactor, reacted in 40 DEG C of water-baths；
(5) aqueous solution C is injected in second capillary microreactor with 0.3mL/min flow by syringe pump,
Reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water is washed with ethanol alternating centrifugal, obtains Ag/ oxygen reductions
Graphite alkene composite nano materials, as shown in Figure 4.Ag load capacity is 21.3wt%, and the average grain diameter of Ag nano-particles is
3.1nm。
Embodiment 3
(1) by 0.00425g AgNO under the conditions of lucifuge3It is dissolved in 45mL deionized waters, 5mL oxidation stones is added then to it
Black alkene solution (2mg/mL) is made into AgNO3Molar concentration is 0.0005mol/L, graphene oxide concentration is the water-soluble of 0.2mg/mL
Liquid A, 0.15g lauryl sodium sulfate, 0.027g sodium citrates are then added thereto, stir 10 minutes, be allowed to be sufficiently mixed；
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized waters, is made into 0.0015mol/L's
NaBH4Aqueous solution B；
(3) by 0.04g NaOH, 0.196g NaBH4It is dissolved in 50mL deionized waters, is made into 0.01mol/L NaBH4Water
Solution C；
(4) by water solution A, aqueous solution B, normal octane respectively with 0.1,0.1,0.3mL/min flow is by injecting infusion
Enter in first capillary microreactor, reacted in 40 DEG C of water-baths；
(5) aqueous solution C is injected in second capillary microreactor with 0.1mL/min flow by syringe pump,
Reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water is washed with ethanol alternating centrifugal, obtains Ag/ oxygen reductions
Graphite alkene composite nano materials, as shown in Figure 5.Ag load capacity is 21.3wt%, and the average grain diameter of Ag nano-particles is
2.6nm。
Comparative example 1
(1) by 0.00425g AgNO under the conditions of lucifuge3It is dissolved in 45mL deionized waters, 5mL oxidation stones is added then to it
Black alkene solution (2mg/mL) is made into AgNO3Molar concentration is 0.0005mol/L, graphene oxide concentration is the water-soluble of 0.2mg/mL
Liquid A, 0.15g lauryl sodium sulfate, 0.027g sodium citrates are then added thereto, stir 10 minutes, be allowed to be sufficiently mixed；
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized waters, is made into 0.0015mol/L's
NaBH4Aqueous solution B；
(3) by 0.04g NaOH, 0.196g NaBH4It is dissolved in 50mL deionized waters, is made into 0.01mol/L NaBH4Water
Solution C；
(4) by water solution A, aqueous solution B, normal octane respectively with 0.2,0.2,0.6mL/min flow is by injecting infusion
Enter in first capillary microreactor, reacted in 60 DEG C of water-baths；
(5) aqueous solution C is injected in second capillary microreactor with 0.2mL/min flow by syringe pump,
Reacted in 60 DEG C of water-baths, capillary microreactor outlet gained samples with water is washed with ethanol alternating centrifugal, obtains Ag/ oxygen reductions
Graphite alkene composite nano materials, as shown in Figure 6.Ag load capacity is 21.3wt%, average grain diameter 4.36nm.
Comparative example 2
(1) by 0.00425g AgNO under the conditions of lucifuge3It is dissolved in 45mL deionized waters, 5mL oxidation stones is added then to it
Black alkene solution (2mg/mL) is made into AgNO3Molar concentration is 0.0005mol/L, graphene oxide concentration is the water-soluble of 0.2mg/mL
Liquid A, 0.15g lauryl sodium sulfate, 0.027g sodium citrates are then added thereto, stir 10 minutes, be allowed to be sufficiently mixed；
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized waters, is made into 0.0015mol/L's
NaBH4Aqueous solution B；
(3) by water solution A, aqueous solution B, normal octane respectively with 0.2,0.2,0.6mL/min flow is by injecting infusion
Enter in first capillary microreactor, reacted in 40 DEG C of water-baths；
(4) aqueous solution B is injected in second capillary microreactor with 0.2mL/min flow by syringe pump,
Reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water is washed with ethanol alternating centrifugal, obtains Ag/ oxidation stones
Black alkene composite nano materials, XRD are as shown in Figure 7.Graphene oxide is not fully converted to graphene.
Application examples
Ag/ redox graphene composite nano materials catalytic degradation p-nitrophenols prepared by embodiment 1：
(1) 0.0483g p-nitrophenols are dissolved in 100mL deionized waters, take above-mentioned solution 5mL, be diluted to 100mL,
2mL is taken to be used as degradation reaction；
(2) by 0.095g NaBH4It is dissolved in 50mL deionized waters, obtains 0.05mol/L NaBH4The aqueous solution, take 0.7mL
Add in 2mL p-nitrophenols obtained by (1)；
(3) 4 × 10 are added into mixed solution obtained by (2)-3Ag/ redox graphenes prepared by mg embodiments 1 are answered
Nano material is closed as catalyst, makes it well mixed, reaches adsorption equilibrium；
(4) UV-vis detections are carried out every 30s；
(5) testing result is handled and does p-nitrophenol degradation curve figure, as shown in Figure 8.
Claims (10)
1. preparing the method for Ag/ redox graphene composite nano materials, oil-water two-phase flow is utilized in micro passage reaction
It is continuous to prepare Ag/ redox graphene composite nano materials, it is characterised in that：
(1) under the conditions of lucifuge, by AgNO3, sodium citrate, lauryl sodium sulfate, graphene oxide and water be configured to the aqueous solution
A；
(2) sodium borohydride and NaOH and water are each configured to the aqueous solution B, C；
(3) water solution A, aqueous solution B, normal octane are passed through first capillary microreactor, in first micro- reaction of capillary
Water solution A is mixed with aqueous solution B in device, and independent drop is separated into by normal octane, is formed using normal octane as continuous phase, water-soluble
Liquid is the two-phase flow of dispersed phase；Capillary microreactor is that reaction channel side carries the microreactor of transparent window or is
Bright capillary microreactor, microreactor or transparent capillary microreactor with transparent window are placed in water-bath and carried out instead
Should；
(4) reaction mass is directly entered second capillary microreactor, with aqueous solution C after capillary microreactor outflow
Reacted, through centrifuging with after washing, Ag/ redox graphene composite nano materials are finally prepared.
2. according to the method for claim 1, it is characterised in that：AgNO in water solution A3Molar concentration in water is
0.0001-0.001mol/L, preferably 0.0003-0.0007mol/L；Sodium citrate and AgNO3Molar ratio range be 1:1-5:
1, preferably 1.2:1-3.5:1；Lauryl sodium sulfate and AgNO3Molar ratio range be 6:1-24:1, preferably 8:1-15:1；
AgNO3Than scope it is 0.4 with the mass fraction of graphene oxide:1-0.03:1, preferably 0.3:1-0.2:1.
3. according to the method for claim 1, it is characterised in that：Molar concentration of the sodium borohydride in water is in aqueous solution B
Molar concentrations of the NaOH in water is 0.005-0.05mol/L in 0.0003-0.003mol/L, aqueous solution C.
4. according to the method for claim 1, it is characterised in that：Molar concentration of the sodium borohydride in water is in aqueous solution B
Molar concentrations of the NaOH in water is 0.005-0.05mol/L in 0.001-0.01mol/L, aqueous solution C.
5. according to the method described in claim 1,2 or 3, it is characterised in that：The flow of water solution A, aqueous solution B and aqueous solution C
It is 0.1-1.5mL/min, preferably 0.3-0.9mL/min；Normal octane flow is 0.3-2.5mL/min, preferably 0.6-
1.5mL/min。
6. according to the method for claim 5, it is characterised in that：Water solution A, aqueous solution B are identical with aqueous solution C flow.
7. according to the method for claim 1, its feature with：Reaction temperature is 10-60 DEG C, preferably 20-40 DEG C.
8. according to the method for claim 1, it is characterised in that：First capillary microreactor has reaction channel and three
Bar intake channel, respectively fluid inlet channel I, fluid inlet channel II, fluid inlet channel III, three intake channel waterpower
Diameter is identical or different, respectively 0.2-1.2mm；The port of export of the three fluid inlet channels arrival end with reaction channel respectively
Connection, fluid inlet channel I are straight stick channel with, fluid inlet channel II and fluid inlet channel III, and liquid-inlet leads to
Road I is identical with the angle of fluid inlet channel III with fluid inlet channel II, fluid inlet channel II, is 30-90 °；Reaction is logical
The hydraulic diameter in road and intake channel hydraulic diameter are identical or different, are 0.2-1.2mm, and reaction channel length is 2-10m；It is water-soluble
Liquid A, aqueous solution B enter microreactor by the arrival end of three fluid inlet channels respectively with normal octane, enter in reaction channel
Mouth end starts mixing and reaction.
9. according to the method for claim 1, it is characterised in that：Second capillary microreactor has reaction channel and two
Bar intake channel, respectively fluid inlet channel IV, fluid inlet channel V, wherein fluid inlet channel IV and first capillary
The port of export of pipe microreactor is connected, and two intake channel hydraulic diameters are identical or different, respectively 0.2-1.2mm；Two liquid
The port of export of body intake channel connects with the arrival end of reaction channel respectively, and they are straight stick channel, fluid inlet channel
IV and the angle of fluid inlet channel V are 30-90 °；The hydraulic diameter of reaction channel is identical with intake channel hydraulic diameter or not
Together, it is 0.2-1.2mm, reaction channel length is 0.5-5m；The port of export of aqueous solution C and first capillary microreactor flows out
Thing enters microreactor by the arrival end of two fluid inlet channels respectively, reaction channel arrival end start mixing with it is anti-
Should.
10. according to the method for claim 1, it is characterised in that：The Ag/ redox graphene composite Nanos being prepared
The particle size range of Ag nano-particles is 1-10nm in material.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009013490A (en) * | 2007-07-09 | 2009-01-22 | Sumitomo Metal Mining Co Ltd | Nickel powder, and method for producing the same |
| CN103250739A (en) * | 2012-08-20 | 2013-08-21 | 苏州大学 | Preparation method of oxidized grapheme/silver particle nanometer compound and application thereof |
| CN106270543A (en) * | 2015-06-12 | 2017-01-04 | 中国科学院大连化学物理研究所 | The method preparing the controlled Triangular nanoplates of arrangement mode continuously |
| CN106563811A (en) * | 2015-10-13 | 2017-04-19 | 中国科学院大连化学物理研究所 | Method for continuously preparing urchin-like Ag-ZnO nano particles by using microchannel reactor |
| CN106824234A (en) * | 2017-01-22 | 2017-06-13 | 中国科学院大连化学物理研究所 | The method for preparing sea urchin shape Ag/AgCl/ZnO nano composite materials |
-
2017
- 2017-09-25 CN CN201710872954.5A patent/CN107617750B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009013490A (en) * | 2007-07-09 | 2009-01-22 | Sumitomo Metal Mining Co Ltd | Nickel powder, and method for producing the same |
| CN103250739A (en) * | 2012-08-20 | 2013-08-21 | 苏州大学 | Preparation method of oxidized grapheme/silver particle nanometer compound and application thereof |
| CN106270543A (en) * | 2015-06-12 | 2017-01-04 | 中国科学院大连化学物理研究所 | The method preparing the controlled Triangular nanoplates of arrangement mode continuously |
| CN106563811A (en) * | 2015-10-13 | 2017-04-19 | 中国科学院大连化学物理研究所 | Method for continuously preparing urchin-like Ag-ZnO nano particles by using microchannel reactor |
| CN106824234A (en) * | 2017-01-22 | 2017-06-13 | 中国科学院大连化学物理研究所 | The method for preparing sea urchin shape Ag/AgCl/ZnO nano composite materials |
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| CN110479348A (en) * | 2019-09-04 | 2019-11-22 | 西南石油大学 | A kind of preparation method and applications of the monatomic catalyst of metal |
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| CN110935444A (en) * | 2019-12-14 | 2020-03-31 | 中国科学院大连化学物理研究所 | Method for preparing precious metal alloy/reduced graphene oxide composite material |
| CN113042037A (en) * | 2021-03-03 | 2021-06-29 | 中国科学院大连化学物理研究所 | Method for preparing metal/titanium dioxide composite material continuously based on micro-reaction technology |
| CN113470986A (en) * | 2021-07-19 | 2021-10-01 | 重庆文理学院 | Flexible linear supercapacitor and preparation method thereof |
| CN113470986B (en) * | 2021-07-19 | 2022-04-12 | 重庆文理学院 | Flexible linear supercapacitor and preparation method thereof |
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