CN108580924A - A kind of nano material liquid phase method for continuously synthesizing - Google Patents
A kind of nano material liquid phase method for continuously synthesizing Download PDFInfo
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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
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- 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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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
A kind of nano material liquid phase method for continuously synthesizing, 1) design nano material continuous reaction apparatus；2) pre-reaction liquid is prepared；3) pre-reaction liquid stream is automatically controlled into the reaction bulb in pre-reaction device by control valve；4) heating furnace is controlled by microcomputer and carries out temperature reaction；5) after the completion of temperature reaction, the reaction solution containing nano material is automatically controlled by control valve and flows out reaction bulb to receiving flask；6) the pre-reaction liquid needed for repeatedly reaction is laid in ample stocks of before continuous growth in pre-reaction bottle to repeat 3)~5 using mounted rectilinear continuous growth experiment equipment is designed), realize the continuous growth of nano material；7) nano material is purified, completes nano material liquid phase and continuously synthesizes.In the thermostatic oven body of small size, the vertical unicom container and pipeline controlled by system realizes that sequencing is continuously grown, the yield of liquid phase synthesis nano material is greatly improved in smaller space, is suitable for laboratory synthesis and industrialized production.
Description
Technical field
The present invention relates to based on liquid phase nano material, more particularly, to a kind of nano material liquid phase method for continuously synthesizing.
Background technology
With the arriving in nano material epoch, the synthetic technology of nano material emerges one after another, according to the object phase being synthetically prepared
State can be divided into vapor phase method, liquid phase method and solid phase method three classes, and wherein chemical liquid phase reaction is very important Macroscale homogenous conjunction
At one of the important method of nano material.Usual liquid phase method prepares nano material, is the one or more kinds of soluble metals of selection
Salt solute is configured to reaction solution with liquid solvent, or the reaction was continued for addition liquid solute during the reaction, each element
In lewis' acid state, one-dimensional (nano wire), two-dimentional (nanometer sheet) or the three-dimensional (nanometer that are precipitated or suspended after reaction
Particle) nano shape material.Liquid phase method is current laboratory and the most widely used preparation method of nano material of industrial circle,
It can be used for synthesizing the nano materials such as metal, oxide.By taking metal nanometer line as an example.In recent years, copper nano-wire research was prominent flies suddenly
Into great potential replaces tin indium oxide to become transparent electrode material of new generation.Currently, the synthetic method mainly used is liquid phase
Synthetic method can obtain diameter and be differed at tens nanometers, various copper nano-wires of the length from tens microns of mm size.Together
When, metal nanometer line can wrap different metal element in its surface in the liquid phase, such as nickel, silver, zinc, platinum other
Metallic element forms metal nanometer line ([1] Wang, H. of nucleocapsid；Wu,C.；Huang,Y.；Sun,F.；Lin,N.；
Abdul,M.；Zhong,Z.；Yang,X.；Chen,X.；Kang,J.；Cai,D.ACS.Appl.Mater,8,28709-28717
(2016))。
Although liquid phase synthesizing method itself is suitble to industrialization large-scale production, conventional thought and technology main still to increase
Add container volume, expands the mode of quantity of solvent to improve yield.It is useful such as there are many growing containers of synthesis metal nanometer line
Three-necked flask growth, according to the difference of capacity, it can disposably grow 25ml, 50ml, 100ml etc.；Useful round-bottomed flask
Growth, 50ml, 100ml, 500ml etc. can disposably be grown according to flask capacity；Also useful pot mouth growth, disposably
500ml, 1L, 2L ([2] Ye, S. such as not can be grown；Stewart,I.；Chen,Z.；Li,B.；Rathmell,A.；
Benjamin J.；Wiley.Acc accounts,49,442-451(2016)).It can be seen that if necessary to raised growth gold
When belonging to nano wire, the container of bigger is needed replacing, occupies the space of bigger, consumes more extra energy.In addition, from laboratory
Horizontal small container synthetic technology, is expanded to bulk container industrially scalable, is usually accompanied by the further complexity of reaction process
Change and the failure of system response conditional parameter, so product quality declines to a great extent.
Invention content
It is an object of the invention to for current nano material synthesis production capacity and space, the contradiction of operation sequence complexity, carry
For a large amount of liquid phase synthesis nano materials in smaller space can be achieved, a kind of nano material liquid phase for meeting industrial applications demand connects
Continuous synthetic method.
The present invention includes the following steps：
1) nano material continuous reaction apparatus is designed；
2) pre-reaction liquid is prepared；
3) pre-reaction liquid stream is automatically controlled into the reaction bulb in pre-reaction device by control valve；
4) heating furnace is controlled by microcomputer and carries out temperature reaction；
5) after the completion of temperature reaction, the reaction solution containing nano material is automatically controlled by control valve and flows out reaction bulb to receipts
Collect bottle；
6) the pre-reaction liquid needed for repeatedly reaction is laid in ample stocks of before continuous growth in pre-reaction bottle, then using design installation
Good rectilinear continuous growth experiment equipment repeats step 3)~5), realize the continuous growth of nano material；
In step 6), the rectilinear continuous growth experiment equipment constantly repeats feed, reaction, emptying, collects product
Cycle, realize the function that automatically continuously synthesizes, do not account for large space, be not necessarily to personnel's operation and control in the process.
7) nano material is purified, completes nano material liquid phase and continuously synthesizes.
In step 1), the nano material continuous reaction apparatus can be rectilinear glass reaction unit, described rectilinear
Glass reaction unit be equipped with feeding container, reaction vessel and collection vessel, between feeding container, reaction vessel and collection vessel with
Control valve connects, to realize that system automatically controls.
In step 4), communication type program heating furnace up and down, the connection up and down can be used in the microcomputer control heating furnace
Constant temperature ceramic fibre stove can be used in formula program heating furnace, is opened there are two the duct being aligned in burner hearth upper and lower ends, channel diameter can
It is designed according to container conduit diameter, preferably channel diameter is 5cm, described vertical to connect rectilinear reaction vessel group
Formula container group be equipped with feeding container, reaction vessel and product collection vessel, rectilinear reaction vessel group can be used glass, quartz,
The corrosion-resistant and high-temperature resistants material such as corundum, stainless steel, pipeline is connected to by autocontrol valve between the container of rectilinear reaction vessel group, institute
It states autocontrol valve and the controls such as solenoid valve, pneumatic operated valve, glass valves, ball valve can be used；Computer control software can be used in control program
(such as Labview) controls heating furnace to valve and microcomputer by PORT COM and is controlled into line program；Reaction vessel is equipped with protection
Gas interface, for being passed through protective gas to reaction vessel.The microcomputer control heating furnace is equipped with microcomputer central control system, described micro-
Machine central control system is set there are two autocontrol valve, computer program and PORT COM to valve and heating furnace into line program control
System；The pre-reaction agent solution matched needed for being added in the feeding container, the solvent of the pre-reaction agent solution can be selected from water,
At least one of alcohol, ether, octadecenyl amine etc. be inorganic or organic solvent.
The top of the reaction vessel can access double-channel gas pipeline simultaneously, can be used for being passed through protectiveness to reaction vessel
Gas participates in reaction gas, and the protective gas includes at least one of nitrogen, argon gas, oxygen, hydrogen, ammonia etc.；
The size of burner hearth that the size of reaction vessel can control heating furnace with microcomputer coordinates, and microcomputer control heating furnace can be controlled by communication interface
Heating schedule；Reaction vessel lower end connects another autocontrol valve, waits after the completion of reacting, and by control terminal, starts control valve,
Solution containing nano materials is put into product collection vessel.
The present invention in the thermostatic oven body of small size, realize by the vertical unicom container and pipeline controlled by system
Sequencing is continuously grown, and the yield of liquid phase synthesis nano material can be greatly improved in smaller space, is suitable for laboratory and is synthesized
And industrialized production.
The present invention to solve the above-mentioned problems, overcome in liquid phase method the mass production of long-term existing nano material synthesis with
The contradiction of small container technology, it is proposed that a kind of completely new liquid phase synthesis concept, the small container for providing a set of creativeness are continuously grown
System, the i.e. continuous growing technology of vertical pipe stove.The present invention is applicable not only to the synthesis of metal (such as copper) nano wire, and is applicable in
It is synthesized in the nano material of any liquid phase method, such as nano silver wire, nanometer sheet, nano particle etc..The present invention's is of low cost, section
About labo r resources, it is simple to operate, meet industrialization demand, to realize light, nano material compound probability just, small, fast
Production steps an important step.Structure is extremely simple, and occupied space is smaller than 1m2, in the case of artificial and large space, energy
The rapid all kinds of nano material liquid phase synthesis for carrying out heavy industrialization.It is with a wide range of applications and potentiality to be exploited.
Description of the drawings
Fig. 1 is the structure composition schematic diagram of nano material continuous reaction apparatus embodiment of the present invention.
Fig. 2 is the structure composition schematic diagram that microcomputer of the present invention controls heating furnace embodiment.
Fig. 3 is the structure composition schematic diagram of pre-reaction device of the present invention.
Fig. 4 is the structure composition schematic diagram of feed pipe of the present invention, nitrogen inlet-outlet and cone mill plug interface.
Fig. 5 is the structure composition schematic diagram of reaction bulb of the present invention, autocontrol valve and product collection vessel.
Specific implementation method
Below for growing copper nano-wire materials synthesis, in conjunction with attached drawing, the present invention is further illustrated.
The structure composition schematic diagram of the embodiment of the present invention is referring to Fig. 1.
1, the continuous growing system of rectilinear tube furnace
1) design can meet the microcomputer control heating furnace of copper nano-wire growth conditions.
Using ceramic fibre stove.Common thermostatic oven is a closure heating cavity, can not achieve metal nanometer line company
Continuous raised growth, the present invention, which uses upper and lower communication type thermostatic oven, design feature, to be carried out up and down in 3 center of burner hearth
It opens up unicom duct and forms burner hearth trepanning 1, bore dia is about 5cm (diameter can be designed according to container conduit diameter), entirely
2 size of furnace body is 80cm × 80cm × 60cm, realizes temperature setting by controlling the space of a whole page 4, as shown in Figure 2.Duct cooperation is heat-insulated
Stove is stifled, is suitable for connection successive reaction container group, and ensure that 3 interior temperature distribution of burner hearth is uniform, and play to the heat-insulated of outside
Effect.
Microcomputer controls heating furnace and uses 20 sections of heated at constant temperature control systems, and with RS232 communication interfaces and microcomputer software phase
Connection, heating rate require, up to 20 DEG C/min, directly to do system control with computer, save manual steps.
2) the continuous growth response container group of Aided design nano material.
In view of needing continuously to be grown, it is therefore desirable to good pre- of pre-reaction feeding container 6 storage pre-coordination
Reaction dissolvent, deployed solution can reach pre-reactor by feed inlet 5, as shown in figure 3, the pre-reactor uses back taper
Bottle structure facilitates solvent to store and quickly convey downwards, and bottleneck includes frosted mouth bottle stopper above pre-reactor, and lower pipeline passes through
Autocontrol valve 7 controls automatic discharging function, is connected with the feed pipe 10 of pre-reactor.Autocontrol valve uses solenoid valve knot
Structure, and there is communication interface to be connected with microcomputer, equally achievable microsystem control.Pre-reaction feeding container 6 is placed in microcomputer control
On heating furnace, lower pipeline connects the reaction vessel 13 in burner hearth 3 by the upper duct of burner hearth 3, and combination uses taper
Mill plug interface 12.
Reaction vessel 13 is placed in burner hearth 3, is designed using spherical structure, is copper nano-wire reaction chamber, is coordinated 3 size of burner hearth
And the uniformity of reaction is kept, as shown in figure 4, diameter is about 20cm, top is connect by cone mill plug interface with pre-reaction bottle.
Feed pipe 10 is designed as binary channels glass tube, and nitrogen inlet 8 and nitrogen outlet 9 are equipped in binary channels glass tube.Feed pipe 10 is used
It, then can be logical via mass flow controller by protecting gas entrance in growth course in supplementing reaction dissolvent to reaction vessel 13
Entering protective gas (such as nitrogen) conduct prevents oxidation protection gas, meanwhile, there are another exhaust emission pipes, exclude reactor off-gas.
Because density of nitrogen is more than air, it is possible to the air in reaction bulb be discharged with air-discharging method, two pipelines are by intermediate steady
Determine the fixation of device 11.There are two function, (control reaction solution flows into reaction bulb and is passed in and out with nitrogen the quartz glass tube tool of middle section
Reaction bulb), reaction unit is not only simplified in this way, and improves instrument utilization rate.Reaction vessel bottom discharge nozzle road 14 passes through stove
The lower duct of thorax 3 is connect by autocontrol valve 15 with the product collection vessel 16 of 2 lower section of furnace body.Autocontrol valve 15 uses
Electromagnetic valve structure, and there is communication interface to be connected with microcomputer, equally achievable microsystem control.
The product collection vessel 16 is connected using the pipeline of ground cone-shaped interface with reaction vessel 13, as shown in figure 5,
For storage reaction product, and it can realize the fast cooling cooling of reaction dissolvent.
3) microcomputer controls heating furnace
The automatic progress entirely reacted in order to control, saves manual steps, and heating all uses microsystem with input and output material
Control.Reaction solution flows into reaction bulb from reactor automatically, and waits that automatic outflow reaction bulb is collected to product after the completion of reacting
In container 16, it is separately added into autocontrol valve.Simple control valve, which can not achieve, to be automatically controlled, logical by computer and middle-end
It interrogates equipment and connects two control valves, installation procedure runs software realizes the flowing of automation control reaction solution on computers.
2, nano material liquid phase method for continuously synthesizing includes the following steps：
1) preparation of pre-reaction liquid
(copper chloride, acetylacetone copper needed for such as copper nano-wire growth is added in pre-reaction bottle in required pre-reaction solvent
Deng)；Secondly the catalyst needed for reaction is added (catalyst can be nickel salt, platinum salt etc.)；It is eventually adding a certain amount of reducing agent
With surfactant (such as hexadecylamine, octadecenyl amine, ethylenediamine).All pre-reaction solvents can press one according to actual conditions
Certainty ratio is added in pre-reaction bottle (such as：Experimental program is 0.1g nickel acetylacetonates to be added per 0.13g copper chlorides and with 10mL oil
Amine).Since solution will not react in pre-reaction bottle at room temperature, so can be laid in a pre-reaction bottle adequately pre-
Reaction solution is without occurring specimen breakdown.
2) the continuous growth course automatically controlled
(1) it is opened by the autocontrol valve under the procedure auto-control pre-reaction bottle of computer terminal, it will be a certain amount of pre- anti-
Solvent is answered to inject in reaction bulb, later closing control valve.
(2) mass flow controller is controlled, the protective gas (such as nitrogen) of certain flow is continuously passed through to reaction vessel, and
It initially enters heating furnace and carries out heating heating response procedures, heating schedule can set at least 20 according to nano material synthesis condition
Section temperature program keeps nano material to grow duration after temperature reaches reaction temperature.
(3) it waits for after reaction, heating schedule being closed, and protective gas is kept to continue to be passed through, into temperature-fall period.
(4) room temperature to be down to, stops supply protective gas, and computer end program control reaction bulb lower part autocontrol valve is beaten
It opens, the product solution containing nano material is discharged into the product collection vessel of lower section, later closing control valve.
(5) above procedure is repeated, realizes continuous growth and output.
3) separating-purifying of nano wire
Reaction product in product collection vessel is transferred to centrifuge tube and is put into centrifuge and carries out centrifugal treating, is centrifuged
Machine rotating speed is 9000r/min, and centrifugation time is set as 5min.After centrifugation, nano wire solid is deposited on centrifugation bottom of the tube, will be upper
After layer waste liquid is outwelled, addition n-hexane carries out centrifugation bottom of the tube nano wire ultrasonic again, and after about 3min, second is carried out to solution
Secondary centrifugal treating.It repeats this centrifugal treating number to be no less than 3 times, finally seals nano wire in n-hexane up for safekeeping.
The midget plant that the present invention is combined using rectilinear glass container group with ceramic fibre stove is, it can be achieved that automatically control down
The technology of efficient continuous a large amount of nano material growths.The present invention use rectilinear pipeline heating furnace structure, including it is a set of by
System is controlled in the glass reaction unit of feeding container, reaction vessel and collection vessel, mating ceramic fibre program heating furnace, microcomputer
System is constituted.Main concept is that pre-reaction solution is contained in feeding container, and quantitative reaction is controlled by an autocontrol valve
Solution flows into reaction vessel bottle, and controls program heating furnace simultaneously and carry out temperature reaction nano materials, after completion of the reaction, leads to
It crosses another autocontrol valve and the nanomaterial solution of synthesis is injected into collection vessel.Meanwhile second feed and response procedures
Continue, realizes continuous nano material synthesis.Structure is extremely simple, and occupied space is smaller than 1m2, without artificial and large space
In the case of, all kinds of nano material liquid phase synthesis of heavy industrialization can be carried out rapidly.It is with a wide range of applications and opens
Send out potentiality.
Claims (10)
1. a kind of nano material liquid phase method for continuously synthesizing, it is characterised in that include the following steps：
1) nano material continuous reaction apparatus is designed；
2) pre-reaction liquid is prepared；
3) pre-reaction liquid stream is automatically controlled into the reaction bulb in pre-reaction device by control valve；
4) heating furnace is controlled by microcomputer and carries out temperature reaction；
5) after the completion of temperature reaction, the reaction solution containing nano material is automatically controlled by control valve and flows out reaction bulb to collection
Bottle；
6) the pre-reaction liquid needed for repeatedly reaction is laid in ample stocks of before continuous growth in pre-reaction bottle, it is then mounted using designing
Rectilinear continuous growth experiment equipment repeats step 3)~5), realize the continuous growth of nano material；
7) nano material is purified, completes nano material liquid phase and continuously synthesizes.
2. a kind of nano material liquid phase method for continuously synthesizing as described in claim 1, it is characterised in that described to receive in step 1)
Rice material continuous reaction apparatus is rectilinear glass reaction unit, and the rectilinear glass reaction unit is equipped with feeding container, anti-
Container and collection vessel are answered, is connected with control valve between feeding container, reaction vessel and collection vessel.
3. a kind of nano material liquid phase method for continuously synthesizing as described in claim 1, it is characterised in that described micro- in step 4)
Machine controls heating furnace and uses upper and lower communication type program heating furnace.
4. a kind of nano material liquid phase method for continuously synthesizing as claimed in claim 3, it is characterised in that the communication type journey up and down
Sequence heating furnace uses constant temperature ceramic fibre stove, is opened there are two the duct being aligned in burner hearth upper and lower ends, channel diameter is according to container
Pipe diameter size designs, and channel diameter 5cm, the duct is connect with rectilinear reaction vessel group.
5. a kind of nano material liquid phase method for continuously synthesizing as claimed in claim 4, it is characterised in that the rectilinear container group
Equipped with feeding container, reaction vessel and product collection vessel, rectilinear reaction vessel group is using glass, quartz, corundum, stainless steel
Corrosion-resistant and high-temperature resistant material, pipeline is connected to by autocontrol valve between the container of rectilinear reaction vessel group, the autocontrol valve
Using solenoid valve, pneumatic operated valve, glass valves, ball valve control；Controlling program uses computer control software by PORT COM to valve
Heating furnace is controlled with microcomputer to control into line program.
6. a kind of nano material liquid phase method for continuously synthesizing as claimed in claim 5, it is characterised in that the reaction vessel is equipped with
Protect gas interface.
7. a kind of nano material liquid phase method for continuously synthesizing as described in claim 1, it is characterised in that described micro- in step 4)
Machine controls heating furnace and is equipped with microcomputer central control system, and the microcomputer central control system is set there are two autocontrol valve, computer program
And PORT COM controls valve and heating furnace into line program.
8. a kind of nano material liquid phase method for continuously synthesizing as claimed in claim 5, it is characterised in that add in the feeding container
The pre-reaction agent solution matched needed for entering, the solvent of the pre-reaction agent solution is in water, alcohol, ether, octadecenyl amine
It is at least one.
9. a kind of nano material liquid phase method for continuously synthesizing as claimed in claim 5, it is characterised in that the reaction vessel it is upper
Portion accesses double-channel gas pipeline, for being passed through protective gas to reaction vessel or participating in reaction gas, the protectiveness gas
Body includes at least one of nitrogen, argon gas, oxygen, hydrogen, ammonia；The stove of the size of reaction vessel and microcomputer control heating furnace
Thorax dimensional fits, microcomputer control heating furnace control heating schedule by communication interface；The connection of reaction vessel lower end is another to be automatically controlled
Valve waits after the completion of reacting, and by control terminal, starts control valve, and the solution containing nano materials, which is put into product, to be collected
Container.
10. a kind of nano material liquid phase method for continuously synthesizing as described in claim 1, it is characterised in that described in step 6)
Rectilinear continuous growth experiment equipment repeats feed, reaction, emptying, the cycle for collecting product, realizes automatically continuously synthesis.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111437790A (en) * | 2020-04-15 | 2020-07-24 | 河南科技大学 | Differential pressure type liquid phase timing reaction device for laboratory |
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