CN107617750B - The method for preparing Ag/ redox graphene composite nano materials - Google Patents

The method for preparing Ag/ redox graphene composite nano materials Download PDF

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CN107617750B
CN107617750B CN201710872954.5A CN201710872954A CN107617750B CN 107617750 B CN107617750 B CN 107617750B CN 201710872954 A CN201710872954 A CN 201710872954A CN 107617750 B CN107617750 B CN 107617750B
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CN107617750A (en
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杨梅
陶莎
陈光文
陈会会
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Dalian Institute of Chemical Physics of CAS
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Abstract

The present invention provides the methods 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 and NaOH are each configured to aqueous solution B, C.Water solution A, aqueous solution B, normal octane are then passed through first capillary microreactor simultaneously, water solution A is quickly mixed with aqueous solution B, and drop is independent by normal octane dispersion, reaction mass is after capillary microreactor outflow, it flows directly into second capillary microreactor to be reacted with aqueous solution C, reaction mass reacts under certain temperature.It is centrifuged, washs and be finally prepared Ag/ redox graphene composite nano materials.The present invention has many advantages, such as that process is continuous, simple process, reaction condition are mild, it is high to obtain Ag load capacity in Ag/ redox graphene composite Nano material, partial size is small, particle diameter distribution is narrow, reproducible between batch.

Description

The method for preparing Ag/ redox graphene composite nano materials
Technical field
The invention belongs to Materials Science and Engineering fields, are related to one kind and utilize oil-water two-phase flow system in micro passage reaction The method for preparing standby Ag/ redox graphene composite nano materials.
Background technique
Ag nanoparticle has very strong UV-Visible absorption drawn game area plasma resonance (Localized Surface Plasmon Resonance, LSPR) etc. properties, in Surface enhanced Raman spectroscopy (SERS) and nonlinear optics etc. Aspect is with a wide range of applications.Due to the unique optical property of Ag nanoparticle, Ag nanoparticle and some semiconductors are multiple Composite nanoparticle made of conjunction also has huge contribution in terms of catalytic degradation.The study found that Ag receives The optical property of rice corpuscles has close contact with pattern, partial size.It therefore, is the reunion for avoiding Ag nanoparticle, regulation is received The pattern of rice corpuscles, research worker introduce the carrier that graphene supports Ag nanoparticle as dispersion.Graphene has single Atomic layer level thickness and good electric conductivity are a kind of excellent substrate materials.The study found that preparation Ag- graphene composite Nano Material can disperse Ag nanoparticle on the surface of graphene well, effective that Ag nanoparticle is inhibited to reunite, can be to avoid Because surfactant there are due to cause electric conductivity to be deteriorated, substantially expand the application range of Ag nanoparticle.It is also possible to keep away Exempt from the stacking of graphene, keeps the good dispersibility of graphene.
However, so far, the method for preparing Ag- graphene composite nano material is complex.The research of Xu et al. " Graphene Metal Particle Nanocomposites, J.Phys.Chem.C, 2008,112:19841-19845 ", Graphene oxide, ethylene glycol are mixed with certain density metallic precursor solution first, 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 processing Miscellaneous, time-consuming, limits the extensive use of this method.
Research " the In Situ Synthesis of Metal Nanoparticles on Single- of Zhou et al. Layer Graphene Oxide and Reduced Graphene Oxide Surfaces,J.Phys.Chem.C,2009, Graphene oxide is heated to 75 DEG C in silver nitrate solution, keeps the temperature 30min later, obtains partial size by 113:10842-10846 " In the Ag- graphene composite nanoparticle that several nanometers to 200nm do not wait.This method is intermittent operation, and time-consuming, partial size point Cloth is wide, Ag nano particle diameter is larger, limits the industrialized production of this method.
Research " the A facile and nove synthesis of Ag-graphene-based of Pasricha et al. Ag- graphene composite nanoparticle is synthesized by two-step process in nanocomposites, Small, 2009,5:2253-2259 ".First The mixed solution of graphene oxide, potassium hydroxide and silver sulfate is heated to boiling and is prepared that Ag- graphene oxide is compound to be received Rice corpuscles, then be passed through hydrazine steam reduction and obtain Ag- graphene composite nanoparticle.This method is intermittent operation, two-step reaction, Process is cumbersome, and time-consuming, and non-room temperature increases energy consumption, and this method also cannot achieve continuous production.
To sum up, the preparation process of Ag- graphene composite nanoparticle is mostly the interval behaviour carried out in traditional reactor at present Make, production efficiency is low, and granularity is inhomogenous, and the Ag partial size of load is usually larger, and load capacity is not high, poor repeatability between batch.For gram Disadvantages mentioned above is taken, need to develop one kind not only can continuously produce in enormous quantities, but also make to repeat between gained nano material uniform particle diameter and batch The good method of property.Micro- Chemical Engineering Technology is that a kind of process intensification technology risen the 1990s has compared with traditional technology Small in size, large specific surface area, transfer performance are 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, to reduce reunion, make institute It is reproducible between nano material particle diameter distribution is narrow and batch.In addition, the nano material preparation process based on micro- Chemical Engineering Technology is Continuous operation mode is easy to be mass produced.However, since micro passage reaction channel size is smaller, in preparation nano material It is difficult to avoid blockage problem in the process.It is restored for this purpose, the application is prepared for Ag/ using oil-water two-phase flow in micro passage reaction Nano particle diameter homogeneity can be improved in graphene oxide composite nanoparticle, mixed since microreactor can be strengthened Journey, Ag load capacity is big in the Ag/ redox graphene composite nanoparticle being prepared, and partial size is smaller, average grain diameter control In 5nm hereinafter, but also can avoid micro passage reaction blocking.
Summary of the invention
It is an object of the invention to be based on micro passage reaction, provides and a kind of prepare 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, simple process, reaction condition temperature It is asked with Ag/ redox graphene composite nanoparticle pattern and uniform particle diameter, average grain diameter control in 5nm or less, without blocking Topic.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
The method for preparing Ag/ redox graphene composite nano materials utilizes water-oil phase in micro passage reaction The continuous preparation Ag/ redox graphene composite nano materials of stream, 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 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 Quickly mixing, and drop is independent by normal octane dispersion, being formed by continuous phase, aqueous solution of normal octane is the two-phase of 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 are reacted;
In above-mentioned technical proposal, it is micro- to be directly entered second capillary after capillary microreactor outflow for reaction mass Reactor is reacted with aqueous solution C, and after centrifuge washing, Ag/ redox graphene composite Nano material is finally prepared Material.
In above-mentioned technical proposal, AgNO in water solution A3The molar concentration of Yu Shuizhong 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 0.4:1-0.03:1 with the mass fraction range on graphene oxide, preferably 0.3:1-0.2:1。
In above-mentioned technical proposal, the molar concentration of sodium borohydride Yu Shuizhong is 0.0003-0.003mol/L in aqueous solution B, The molar concentration of NaOH Yu Shuizhong is 0.005-0.05mol/L.
In above-mentioned technical proposal, the molar concentration of sodium borohydride Yu Shuizhong is 0.001-0.01mol/L in aqueous solution B, The molar concentration of NaOH Yu Shuizhong is 0.005-0.05mol/L.
In above-mentioned technical proposal, the flow of water solution A, aqueous solution B and aqueous solution C 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.
In above-mentioned technical proposal, water solution A, aqueous solution B are identical as the flow of aqueous solution C.
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, respectively Fluid inlet channel I, fluid inlet channel II, fluid inlet channel III, three intake channel hydraulic diameters are identical or different, point It Wei not 0.2-1.2mm;The outlet end of three fluid inlet channels is connected to the arrival end of reaction channel respectively, fluid inlet channel I and fluid inlet channel II, fluid inlet channel II it is identical as the angle of fluid inlet channel III, be 30-90 °;Reaction channel Hydraulic diameter and intake channel hydraulic diameter it is identical or different, be 0.2-1.2mm, reaction channel length be 2-10m.Aqueous solution A, the arrival end that aqueous solution B and normal octane pass through three fluid inlet channels respectively enters, and starts to mix in reaction channel arrival end It closes and reacts.
In above-mentioned technical proposal, second capillary microreactor has reaction channel and two intake channels, respectively Fluid inlet channel IV, fluid inlet channel V, the wherein outlet of 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 is connected to 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.The outlet end of aqueous solution C and first capillary microreactor pass through respectively two liquid into The arrival end in mouth channel enters, and starts mixing in reaction channel arrival end and reacts.
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 present invention the substantive distinguishing features outstanding and significant progress that have are as follows:
It is simple process, anti-1. based on micro passage reaction one-step synthesis Ag/ redox graphene composite nano materials Answer mild condition, process continuous, the Ag/ redox graphene composite nano materials pattern and uniform particle diameter being prepared are born The Ag nanoparticle average grain diameter of load is controlled in 5nm hereinafter, reproducible between batch.
2. forming oil-water two-phase flow by introducing normal octane as oily phase, avoiding microchannel blockage problem.
Detailed description of the invention
Fig. 1 is process flow chart of the invention, wherein 1,2,3,4 be the 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.
Specific embodiment
Used microreactor is equal are as follows: and a 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 outlet end of three fluid inlet channels is connected to the arrival end of reaction channel respectively, fluid inlet channel I and liquid Intake channel II, fluid inlet channel II are identical as the angle of fluid inlet channel III, are 90 °;The hydraulic diameter of reaction channel It is identical as 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 to mix and react in reaction channel arrival end.
Second capillary microreactor has reaction channel and two intake channels, respectively fluid inlet channel IV, Fluid inlet channel V, wherein fluid inlet channel IV is connected with the outlet end of first capillary microreactor, two imports Channel hydraulic diameter is identical, is 0.6mm;The outlet end of two fluid inlet channels is connected to the arrival end of reaction channel respectively, Fluid inlet channel IV, fluid inlet channel V are identical as the angle of fluid inlet channel VI, are 90 °;The waterpower of reaction channel Diameter is identical as intake channel hydraulic diameter, is 0.6mm, and reaction channel length is 1m.Aqueous solution C and first capillary are micro- anti- The arrival end for answering the outlet end of device to pass through two fluid inlet channels respectively enters, reaction channel arrival end start mixing with it is anti- It answers.
The present invention is further illustrated below by embodiment.
Embodiment 1
(1) by 0.00425g AgNO under the conditions of being protected from light3It is dissolved in 45mL deionized water, 5mL is added then to it and aoxidizes stone 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 0.15g lauryl sodium sulfate, 0.027g sodium citrate is then added in liquid A thereto, stirs 10 minutes, is allowed to be sufficiently mixed;
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized water, is made into 0.0015mol/L's NaBH4Aqueous solution B;
(3) by 0.04g NaOH, 0.00565g NaBH4It is dissolved in 50mL deionized water, is made into the NaBH of 0.003mol/L4 Aqueous solution C;
(4) by water solution A, aqueous solution B, normal octane respectively with 0.2,0.2, the flow of 0.6mL/min passes through syringe pump and infuses Enter in first capillary microreactor, is reacted in 40 DEG C of water-baths;
(5) aqueous solution C is injected in second capillary microreactor with the flow of 0.2mL/min by syringe pump, It is reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water and ethyl alcohol alternating centrifugal wash, and obtain Ag/ oxygen reduction 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/ reduction Graphene oxide has been completely converted into graphene in graphene oxide composite nano materials, and the load capacity of Ag is 21.3wt%, The average grain diameter of Ag nanoparticle is 3.3nm.
Embodiment 2
(1) by 0.00425g AgNO under the conditions of being protected from light3It is dissolved in 45mL deionized water, 5mL is added then to it and aoxidizes stone 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 0.15g lauryl sodium sulfate, 0.027g sodium citrate is then added in liquid A thereto, stirs 10 minutes, is allowed to be sufficiently mixed;
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized water, is made into 0.0015mol/L's NaBH4Aqueous solution B;
(3) by 0.04g NaOH, 0.196g NaBH4It is dissolved in 50mL deionized water, is made into the NaBH of 0.01mol/L4Water Solution C;
(4) by water solution A, aqueous solution B, normal octane respectively with 0.3,0.3, the flow of 0.4mL/min passes through syringe pump and infuses Enter in first capillary microreactor, is reacted in 40 DEG C of water-baths;
(5) aqueous solution C is injected in second capillary microreactor with the flow of 0.3mL/min by syringe pump, It is reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water and ethyl alcohol alternating centrifugal wash, and obtain Ag/ oxygen reduction Graphite alkene composite nano materials, as shown in Figure 4.The load capacity of Ag is 21.3wt%, and the average grain diameter of Ag nanoparticle is 3.1nm。
Embodiment 3
(1) by 0.00425g AgNO under the conditions of being protected from light3It is dissolved in 45mL deionized water, 5mL is added then to it and aoxidizes stone 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 0.15g lauryl sodium sulfate, 0.027g sodium citrate is then added in liquid A thereto, stirs 10 minutes, is allowed to be sufficiently mixed;
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized water, is made into 0.0015mol/L's NaBH4Aqueous solution B;
(3) by 0.04g NaOH, 0.196g NaBH4It is dissolved in 50mL deionized water, is made into the NaBH of 0.01mol/L4Water Solution C;
(4) by water solution A, aqueous solution B, normal octane respectively with 0.1,0.1, the flow of 0.3mL/min passes through syringe pump and infuses Enter in first capillary microreactor, is reacted in 40 DEG C of water-baths;
(5) aqueous solution C is injected in second capillary microreactor with the flow of 0.1mL/min by syringe pump, It is reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water and ethyl alcohol alternating centrifugal wash, and obtain Ag/ oxygen reduction Graphite alkene composite nano materials, as shown in Figure 5.The load capacity of Ag is 21.3wt%, and the average grain diameter of Ag nanoparticle is 2.6nm。
Comparative example 1
(1) by 0.00425g AgNO under the conditions of being protected from light3It is dissolved in 45mL deionized water, 5mL is added then to it and aoxidizes stone 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 0.15g lauryl sodium sulfate, 0.027g sodium citrate is then added in liquid A thereto, stirs 10 minutes, is allowed to be sufficiently mixed;
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized water, is made into 0.0015mol/L's NaBH4Aqueous solution B;
(3) by 0.04g NaOH, 0.196g NaBH4It is dissolved in 50mL deionized water, is made into the NaBH of 0.01mol/L4Water Solution C;
(4) by water solution A, aqueous solution B, normal octane respectively with 0.2,0.2, the flow of 0.6mL/min passes through syringe pump and infuses Enter in first capillary microreactor, is reacted in 60 DEG C of water-baths;
(5) aqueous solution C is injected in second capillary microreactor with the flow of 0.2mL/min by syringe pump, It is reacted in 60 DEG C of water-baths, capillary microreactor outlet gained samples with water and ethyl alcohol alternating centrifugal wash, and obtain Ag/ oxygen reduction Graphite alkene composite nano materials, as shown in Figure 6.The load capacity of Ag is 21.3wt%, average grain diameter 4.36nm.
Comparative example 2
(1) by 0.00425g AgNO under the conditions of being protected from light3It is dissolved in 45mL deionized water, 5mL is added then to it and aoxidizes stone 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 0.15g lauryl sodium sulfate, 0.027g sodium citrate is then added in liquid A thereto, stirs 10 minutes, is allowed to be sufficiently mixed;
(2) by 0.04g NaOH, 0.00283g NaBH4It is dissolved in 50mL deionized water, 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, the flow of 0.6mL/min passes through syringe pump and infuses Enter in first capillary microreactor, is reacted in 40 DEG C of water-baths;
(4) aqueous solution B is injected in second capillary microreactor with the flow of 0.2mL/min by syringe pump, It is reacted in 40 DEG C of water-baths, capillary microreactor outlet gained samples with water and ethyl alcohol alternating centrifugal wash, and obtain Ag/ oxidation stone 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-nitrophenol prepared by embodiment 1:
(1) 0.0483g p-nitrophenol is dissolved in 100mL deionized water, takes above-mentioned solution 5mL, is diluted to 100mL, 2mL is taken to use as degradation reaction;
(2) by 0.095g NaBH4It is dissolved in 50mL deionized water, obtains the NaBH of 0.05mol/L4Aqueous solution takes 0.7mL It is added in 2mL p-nitrophenol obtained by (1);
(3) 4 × 10 are added into mixed solution obtained by (2)-3Ag/ redox graphene prepared by mg embodiment 1 is multiple Nano material is closed as catalyst, it is uniformly mixed, reaches adsorption equilibrium;
(4) UV-vis detection is carried out every 30s;
(5) it will test result treatment and do p-nitrophenol degradation curve figure, as shown in Figure 8.

Claims (7)

1. the method for preparing Ag/ redox graphene composite nano materials utilizes oil-water two-phase flow in micro passage reaction Continuous preparation Ag/ redox graphene composite nano materials, it is characterised in that:
(1) under the conditions of being protected from light, by AgNO3, sodium citrate, lauryl sodium sulfate, graphene oxide and water be configured to aqueous solution A;Wherein, AgNO3Molar concentration be 0.0003-0.0007mol/L;Sodium citrate and AgNO3Molar ratio be 1:1-5:1;Ten Sodium dialkyl sulfate and AgNO3Molar ratio be 6:1-24:1;AgNO3Than range it is 0.4 with the mass fraction of graphene oxide: 1-0.03:1;
(2) sodium borohydride, NaOH and water are each configured to aqueous solution B and C;Wherein, in aqueous solution B sodium borohydride it is mole dense Degree is 0.0003-0.003mol/L, and the molar concentration of NaOH is 0.005-0.05mol/L;Mole of sodium borohydride in aqueous solution C Concentration is 0.001-0.01mol/L, and the molar concentration of NaOH is 0.005-0.05mol/L;
(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 is independent drop by normal octane dispersion, 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 has the microreactor of transparent window or is Bright capillary microreactor, microreactor or transparent capillary microreactor with transparent window are placed in water-bath and carry out instead It answers;
(4) reaction mass is directly entered second capillary microreactor, with aqueous solution C after capillary microreactor outflow It is reacted, is centrifuged with after washing, Ag/ redox graphene composite nano materials, Ag nanoparticle is finally prepared Particle size range be 1-10nm.
2. according to the method described in claim 1, it is characterized by: water solution A, aqueous solution B are identical as the flow of aqueous solution C, It is 0.1-1.5mL/min;Normal octane flow is 0.3-2.5mL/min.
3. according to the method described in claim 2, it is characterized by: water solution A, aqueous solution B are identical as the flow of aqueous solution C, It is 0.3-0.9mL/min;Normal octane flow is 0.6-1.5mL/min.
4. according to the method described in claim 1, its feature is being 10-60 DEG C with: reaction temperature.
5. according to the method described in claim 4, its feature is being 20-40 DEG C with: reaction temperature.
6. according to the method described in claim 1, it is characterized by: first capillary microreactor has reaction channel and three 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 outlet end of three fluid inlet channels respectively with the arrival end of reaction channel Connection, fluid inlet channel I are straight stick channel with, fluid inlet channel II and fluid inlet channel III, and liquid-inlet is logical Road I and fluid inlet channel II, fluid inlet channel II are identical as the angle of fluid inlet channel III, are 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, water The arrival end that solution A, aqueous solution B and normal octane pass through three fluid inlet channels respectively enters microreactor, in reaction channel Arrival end starts to mix and react.
7. according to the method described in claim 1, it is characterized by: second capillary microreactor has reaction channel and two Intake channel, respectively fluid inlet channel IV, fluid inlet channel V, wherein fluid inlet channel IV and first capillary The outlet end of pipe microreactor is connected, and two intake channel hydraulic diameters are identical or different, respectively 0.2-1.2mm;Two liquid The outlet end of body intake channel is connected to the arrival end of reaction channel respectively, 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 as intake channel hydraulic diameter or not It together, is 0.2-1.2mm, reaction channel length is 0.5-5m;It flows out the outlet end of aqueous solution C and first capillary microreactor The arrival end that object passes through two fluid inlet channels respectively enters microreactor, reaction channel arrival end start mixing with it is anti- It answers.
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