CN108745252A - A kind of micro Nano material preparation facilities - Google Patents
A kind of micro Nano material preparation facilities Download PDFInfo
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- CN108745252A CN108745252A CN201810746858.0A CN201810746858A CN108745252A CN 108745252 A CN108745252 A CN 108745252A CN 201810746858 A CN201810746858 A CN 201810746858A CN 108745252 A CN108745252 A CN 108745252A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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Abstract
The present invention relates to a kind of micro Nano material preparation facilities, including reaction kettle, blender, charge door, condenser pipe, peristaltic pump and master controller, peristaltic pump is electrically connected with master controller, it is connected inside the hose of peristaltic pump and reaction kettle, for the pumping of acid & alkali liquid, to adjust the pH value of reaction mass in reaction kettle；It is additionally provided with ultrasonic probe, temperature sensor, pH electrodes and conductivity sensor in reaction kettle, is electrically connected respectively with master controller, master controller is monitored and controls to ultrasonic generation, temperature, pH value and the conductivity in reaction kettle respectively.The present invention is easy to operate, the degree of automation is higher, add the design for being stirred, automatically controlling adjustment pH value, measuring conductivity in real time by using controllable ultrasound is carried out to mixture, so that mixture enters, kettle mixing velocity is fast, dispersibility is good, pH value control is accurate, product grain good evenness, good sphericity improve the controllability of synthetizing micro-nano material.
Description
Technical field
The present invention relates to field of micro-nano material technology, and in particular to a kind of micro Nano material preparation facilities.
Background technology
Nano material is sent out in fields such as semicon industry, sophisticated manufacturing, the energy, chemical industry, environment, medicine, national defense safeties
Wave important function.The pattern and size of micro Nano material are in coating, catalyst, material, medicine and other fields to material
There can be great influence with quality.The patterns such as microballoon of shape specification, homogeneous grain diameter nano material and core-shell structured nanomaterials
It is widely used, is one of the hot and difficult issue of nano material synthesis.
Shape specification, the nano material of homogeneous grain diameter have extensive use.Such as monodisperse silica since its granularity is equal
One, the features such as stability is good rubber, coating, catalyst, chromatographic column filler, biology, drug and cosmetics, standard metering, from
Assembling photonic crystal etc. is widely used.Monodisperse silica microspheres useMethod, the colloidal sol seed law, microemulsion
It is prepared by the methods of method.Monodisperse polymer micro-sphere is as functional high molecule material in analytical chemistry, standard metering, self assembly light
Sub- crystal etc. is widely used.Monodisperse polystyrene (PS), crosslinked polystyrene etc. are using emulsion polymerization, soap-free emulsion
Polymerization, suspension polymerization, dispersion copolymerization method, seeded polymerization.The materials such as mono-dispersion microballoon are equal to regular appearance, size
One and the high request of monodispersity make the control to preparation condition and preparation facilities requirement higher.
To ensure that the control of nano material product quality, micro-nano reference materials for particle size analysis are nano particle size measurement standard mistakes
An important ring in journey.In the world, reference materials for particle size analysis is usually divided into monodisperse and polydispersion two types.Monodisperse is logical
The geometric standard deviation for referring to particle diameter distribution is less than 1.2%.At present, the material for being used to prepare monodisperse spherical particle mainly has
Polystyrene, crosslinked polystyrene (styrene-divinylbenzene copolymer PSDVB) etc..The preparation of micro-nano reference materials for particle size analysis
Control and preparation facilities to preparation condition require higher.
In acidity condition, the liquid feeding rate of raw material and delivery rate, stir speed (S.S.) in the preparation process of micro Nano material
Deng all being had a major impact to the pattern of nano-particle, size and quality, generally prepared frequently with multiple process multisteps, equipment
Quantity is more, using multiple independent equipment and manual operation control adjustment reaction condition, prepares receiving for different-shape and size
Rice corpuscles, the degree of automation are low.Process is relatively more in process of production for the preparation facilities of existing micro Nano material, preparation condition
It is not easy to be precisely controlled, is easy the uneven poor dispersion of stirring and generates reunion, labor intensive is also easy to produce human error, preparation process
The pollution of middle generation easily influences the health of operator；The easy granular size of micro Nano material prepared is uneven, and sphericity is poor,
Using with limitation.
Invention content
It is insufficient present in above-mentioned background technology it is an object of the invention to solve, a kind of novel micro Nano material is provided
Preparation facilities by ultrasound plus stirring, automatically controls adjustment pH value, the real-time design for measuring conductivity, real-time automatic sampling prison
It surveys, improves the controllability of synthetizing micro-nano material.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of micro Nano material preparation facilities, including reaction kettle, blender, charge door, the condenser pipe with receiving flask, wriggling
Pump and master controller, the charge door and condenser pipe are arranged above the reaction kettle, be respectively used to reaction mass addition and
The liquid that product distills out is collected, and the agitating paddle of the blender gos deep into the reaction kettle, is used for the stirring of reaction mass, institute
It states peristaltic pump to be electrically connected with the master controller, the peristaltic pump is used for by inside hose and the reaction kettle being connected
The pumping of acid & alkali liquid, to adjust the pH value of reaction mass in the reaction kettle；
The ultrasonic probe for being cleaned and being disperseed to reaction mass, monitoring reaction mass temperature are additionally provided in the reaction kettle
Temperature sensor, monitor reaction mass pH value pH electrodes and monitor extent of reaction conductivity sensor, the ultrasonic probe,
Temperature sensor, pH electrodes and conductivity sensor are electrically connected with the master controller respectively, and the master controller is respectively to institute
Ultrasonic generation, temperature, pH value and the conductivity stated in reaction kettle are monitored and control.
The reaction kettle includes autoclave body, kettle cover and bottom, between the autoclave body and kettle cover, detachable between autoclave body and bottom
Fixed seal connection, be respectively equipped on the kettle cover charge door, inlet, installing port, ultrasonic probe mouth, temperature sensor mouth,
PH electrode ports, conductivity sensor mouth and air inlet, wherein the installing port is arranged at the center of the kettle cover, the inlet
It is connected with the peristaltic pump through hose, the ultrasonic probe, temperature sensor, pH electrodes and conductivity sensor difference are detachable
On the ultrasonic probe mouth of the kettle cover, temperature sensor mouth, pH electrode ports and conductivity sensor mouth, the blender
At the installing port of the kettle cover, the air inlet is connected by hose with the gas tank being arranged outside the reaction kettle.
It is corresponded in the upper surface of the kettle cover and is equipped with charge pipe at the charge door, charging is equipped on the charge pipe
Device, the feeding device are electrically connected with the master controller, and the master controller is to the feeding device to the reaction
The auto feed action of kettle is monitored and controls.
When added material is liquid, the feeding device can wriggle according to application and reaction kettle operating pressure apolegamy normal pressure
One in pump, high-pressure piston pump, normal pressure/high pressure syringe pump, efficient liquid phase pump, large volume high-pressure pump, high pressure volatile liquid pump
Kind；The feeding device can be one or more equipment, it can be achieved that multichannel liquid feeding, not by the main controller controls multichannel
With liquid rate liquid feeding by a certain percentage；When added material is solid, full automatic screw feeding can be selected in the feeding device
Device solid charging system.
Ultrasonic controller, temperature controller, pH value display instrument, conductance controller, peristaltic pump are equipped in the master controller
Adjuster and auto feed controller, the ultrasonic probe and the ultrasonic controller are electrically connected, the temperature sensor with
The temperature controller is electrically connected, and the conductivity sensor is electrically connected with the conductance controller, the pH electrodes and institute
The electric connection of pH value display instrument is stated, and the pH value display instrument is electrically connected with the wriggling pump control mechanism, and the pH value is shown
Showing that the pH value information on instrument passes to the wriggling pump control mechanism, the peristaltic pump is electrically connected with the wriggling pump control mechanism,
The feeding device is electrically connected with the auto feed controller.
It is additionally provided with sample tap on the kettle cover, probe tube is equipped at the sample tap, is equipped on the probe tube
Sampling pump with negative pressure extracting function, the sampling pump and the master controller are electrically connected, and the master controller can be according to
The time interval of setting automatically controls the sampling pump extraction reaction product.
It is additionally provided with sampling controller in the master controller, the sampling pump and the sampling controller, for according to setting
Fixed time interval automatically controls the sampling pump extraction reaction product.
The probe tube includes the sampling inner tube being arranged in the autoclave body, and the sampling inner tube is telescopic tube, sampling
Shi Shenchang is shunk when not sampling.
Condensation nozzle is additionally provided on the kettle cover, the condenser pipe is detachably arranged in the condensation nozzle of the kettle cover
On, the liquid that reaction product distills out when the condensation and vacuum distillation of solvent when for heating reaction is collected.
The peristaltic pump include the first peristaltic pump and the second peristaltic pump, the inlet include the first inlet and second into
Liquid mouth, first peristaltic pump are equipped with acid solution tank, and second peristaltic pump is equipped with alkali liquid tank, the liquid in the acid solution tank
The reaction is entered by first inlet after first peristaltic pump pumping by the adjusting of the wriggling pump control mechanism
Kettle, liquid in the alkali liquid tank is by the adjusting of the wriggling pump control mechanism by described the after second peristaltic pump pumping
Two inlets enter the reaction kettle, and the pH value of reaction mass in the reaction kettle is adjusted with this.
The blender includes agitating paddle, drive shaft and driving motor, the top of the drive shaft and the driving motor
It is drivingly connected, its underpart is fixedly connected with the agitating paddle, and the agitating paddle is extend into the autoclave body, and the driving motor is set
It is fixed in the reaction kettle upper end and by an iron stand.
The autoclave body of the reaction kettle is that double layer hollow is jacket structured, and double layer hollow is jacket structured to be connected with or interior set constant temperature bath
Device, for controlling the temperature of reaction mass in the autoclave body.
The constant temperature bath device is water bath with thermostatic control or constant temperature oil bath.
The charge door, the first inlet, the second inlet, ultrasonic probe mouth, temperature sensor mouth, pH electrode ports, electricity
Derivative sensor mouth, air inlet, sample tap and condensation nozzle are arranged at using the central point of the kettle cover as on the circle in the center of circle；More than
Each interface uses hickey, screw tip to be equipped with containment member O-ring, can be operated under positive pressure and vacuum state,
Press filtration and suction filtration can be used；Containment member O-ring is made of elastic material, preferably Teflon, epoxy resin or polyurethane, peace
Mounted in interface；In addition, also visual reaction system pressure requirements only realize sealing in interface using containment member O-ring.
It is equipped with a dismountable filter structure in the bottom inside front, the direct filtering for product particles after reacting
Washing.
The filter structure includes strainer/filter membrane and pallet, and the pallet stablizes support to strainer/filter membrane, and equipment can be held
Fluid seepage phenomenon is not had when by certain reaction solution pressure filtration；It the aperture of strainer/filter membrane can be according to reaction solution and nanoparticle
The grain size of son is selected.
The inner wall surface roughness of the reaction kettle is less than or equal to 0.4a, to prevent inner wall absorption adhesion and aggregation, is convenient for
Cleaning.
The reaction kettle can carry out the ultrasonic cleaning of reaction kettle inner wall by ultrasonic probe.The reaction kettle is that stainless steel is anti-
Answer one kind in kettle, glass reaction kettle and PVC reaction kettles.
The lower end base of the bottom is additionally provided with discharge port, the lower end of the condenser pipe and discharge port respectively by hose with
One solvent recovery unit one end is connected, and the other end of the solvent recovery unit is connected by hose with the feeding device
It connects, is used for the secondary use of material.
The solvent recovery unit is by solvent recovery container and vacuum pump group at by vacuumizing the true of achievable reaction kettle
Sky filters, and solvent is kept in solvent recovery unit, can also suck the liquid in condenser pipe receiving flask in solvent recovery unit.
Hose on the outside of the air inlet, inlet, the charge pipe on the outside of the charge door, taking on the outside of the sample tap
Control valve is further respectively had on sample pipe, for preventing material adverse current.
The reaction kettle is externally provided with the protection blimp with visual window, on the protection blimp equipped with lighting device and
Camera, the camera can mobile phone wireless and Bluetooth controls.
The master controller is equipped with wireless control switch, can carry out wireless control to master controller.
Art solutions of the present invention have the following advantages that：
A. it is of the invention it is easy to operate, the degree of automation is higher, add stirring by using controllable ultrasound is carried out to mixture
The design mix, automatically control adjustment pH value, measuring conductivity in real time so that mixture enters that kettle mixing velocity is fast, dispersibility
Good, pH value control is accurate, and product grain good evenness, good sphericity improve the controllability of synthetizing micro-nano material.
B. the present invention on kettle cover by setting sample tap, and setting tool has the sampling pump of negative pressure extracting function on probe tube, simultaneously
Sampling pump is connected with the sampling controller on master controller, can automatically extract reaction product at set time intervals, take
Sample monitors particle size size in real time for process analysis procedure analysis.
C. the present invention by passing through hose and solvent recovery unit one end phase respectively in the lower end of condenser pipe and discharge port
Connection, the other end of solvent recovery unit are connected by hose with peristaltic pump, and the solvent after recycling is controlled by peristaltic pump
Hose is added in reaction kettle, realizes the recycling of material, and the waste of resource is reduced while reducing environmental pollution.
Description of the drawings
It, below will be to needed in specific implementation mode in order to illustrate more clearly of the specific embodiment of the invention
Attached drawing is briefly described, it should be apparent that, the accompanying drawings in the following description is some embodiments of the present invention, for this field
For those of ordinary skill, without creative efforts, other drawings may also be obtained based on these drawings.
Fig. 1 is micro Nano material preparation facilities structural schematic diagram of the present invention；
Fig. 2 is the overlooking structure diagram of kettle cover in Fig. 1；
Fig. 3 is the control principle schematic diagram of master controller in the present invention.
Reference sign：
1- reaction kettles
11- autoclave bodies
12- kettle covers
121- charge doors
122- inlets
The first inlets of 1221-, the second inlets of 1222-
123- installing ports, 124- ultrasonic probe mouths, 125- temperature sensor mouths
126-pH electrode ports, 127- conductivity sensor mouths
128- air inlets
1281- control valves
129- sample taps, 1210- condense nozzle
The bottoms 13-
131- discharge ports
2- blenders
21- agitating paddles, 22- drive shafts, 23- driving motors
3- condenser pipes
4- peristaltic pumps
The first peristaltic pumps of 41-
411- acid solution tanks
The second peristaltic pumps of 42-
421- alkali liquid tanks
5- master controllers
51- ultrasonic controllers, 52- temperature controllers, 53-pH value display instruments, 54- conductance controllers
55- wriggling pump control mechanisms, 56- auto feed controllers, 57- sampling controllers
6- ultrasonic probes；7- temperature sensors；8-pH electrodes；9- conductivity sensors；10- gas tanks；
20- iron stands；30- constant temperature bath devices；40- protects blimp；50- feeding devices；
60- probe tubes
601- samples inner tube；
70- sampling pumps；80- filter structures；90- solvent recovery units.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, ordinary skill people
The every other embodiment that member is obtained without making creative work, shall fall within the protection scope of the present invention.
As shown in Figure 1-Figure 3, a kind of micro Nano material preparation facilities, including reaction kettle 1, blender 2, charge door 121, band
Condenser pipe 3, peristaltic pump 4 and the master controller 5 of receiving flask, charge door 121 and condenser pipe 3 are arranged above reaction kettle 1, use respectively
It is collected in the liquid that the addition of reaction mass and product distill out, the agitating paddle 21 of blender 2 gos deep into reaction kettle 1, for anti-
The stirring of material, peristaltic pump 4 is answered to be electrically connected with master controller 5, peristaltic pump 4 is used by being connected inside hose and reaction kettle 1
In the pumping of acid & alkali liquid, to adjust the pH value of reaction mass in reaction kettle 1.
It is additionally provided with the ultrasonic probe 6 for being disperseed to reaction mass and being cleaned in reaction kettle 1, monitors reaction mass temperature
Temperature sensor 7, the pH electrodes 8 for monitoring reaction mass pH value and the conductivity sensor 9 for monitoring extent of reaction, ultrasonic probe 6, temperature
It spends sensor 7, pH electrodes 8 and conductivity sensor 9 to be electrically connected with master controller 5 respectively, master controller 5 is respectively to reaction kettle 1
Interior ultrasonic generation, temperature, pH value and conductivity is monitored and controls.The present invention is easy to operate, the degree of automation is higher, leads to
Cross using to mixture carry out controllable ultrasound add be stirred, automatically control adjustment pH value, in real time measure conductivity design,
So that mixture enters, kettle mixing velocity is fast, dispersibility is good, and pH value control is accurate, and product grain good evenness, good sphericity carry
The high controllability of synthetizing micro-nano material.
Specifically, reaction kettle 1 include autoclave body 11, kettle cover 12 and bottom 13, between autoclave body 11 and kettle cover 12, autoclave body 11 with
It is detachably fixed sealed connection between bottom 13, charge door 121 is respectively equipped on kettle cover 12, inlet 122, installing port 123, is surpassed
Sonic probe mouth 124, temperature sensor mouth 125, pH electrode ports 126, conductivity sensor mouth 127 and air inlet 128, wherein installing port
123 are arranged at the center of kettle cover 12, and inlet 122 is connected through hose with peristaltic pump 4, ultrasonic probe 6, temperature sensor 7,
PH electrodes 8 and conductivity sensor 9 be detachably arranged in respectively the ultrasonic probe mouth 124 of kettle cover 12, temperature sensor mouth 125,
In pH electrode ports 126 and conductivity sensor mouth 127, blender 2 is mounted at the installing port 123 of kettle cover 12, and air inlet 128 passes through
Hose is connected with the gas tank 10 being arranged outside reaction kettle 1.
It is corresponded in the upper surface of kettle cover 12 and is equipped with charge pipe at charge door 121, feeding device 50 is equipped on charge pipe,
Feeding device 50 and master controller 5 are electrically connected, master controller 5 to feeding device 50 to the auto feed of reaction kettle 1 act into
Row is monitored and controlled.When added material is liquid, the feeding device can be matched normal according to application and reaction kettle operating pressure
Press peristaltic pump, high-pressure piston pump, normal pressure/high pressure syringe pump, efficient liquid phase pump, large volume high-pressure pump, high pressure volatile liquid pump
In one kind, feeding device 50 can be one or more, it can be achieved that multichannel liquid feeding, and passing through master controller 5, to control multichannel different
Liquid rate liquid feeding by a certain percentage.When added material is solid, full automatic screw feeder can be selected in the feeding device
Solid charging system.
As shown, being equipped with ultrasonic controller 51, temperature controller 52, pH value display instrument 53, conductance control in master controller 5
Device 54, wriggling pump control mechanism 55 and auto feed controller 56 processed, ultrasonic probe 6 are electrically connected with ultrasonic controller 51, temperature
Sensor 7 is electrically connected with temperature controller 52, and conductivity sensor 9 is electrically connected with conductance controller 54, pH electrodes 8 and pH value
Display instrument 53 is electrically connected, and pH value display instrument 53 is electrically connected with wriggling pump control mechanism 55, by the pH on pH value display instrument 53
Value information passes to wriggling pump control mechanism 55, and peristaltic pump 4 is electrically connected with wriggling pump control mechanism 55, and feeding device 50 adds with automatic
Expect that controller 56 is electrically connected.
In addition, being additionally provided with sample tap 129 on kettle cover 12, probe tube 60 is equipped at sample tap 129, on probe tube 60
Equipped with the sampling pump 70 with negative pressure extracting function；Sampling controller 57 is additionally provided in master controller 5, sampling pump 70 is controlled with sampling
Device 57 processed is electrically connected, and reaction product is extracted for automatically controlling sampling pump 70 at set time intervals.Probe tube 60 wraps
Include the sampling inner tube 601 being arranged in autoclave body 11, sampling inner tube 601 is telescopic tube, and when sampling extends, and is shunk when not sampling.
Condensation nozzle 1210 is additionally provided on kettle cover 12, condenser pipe 3 is detachably arranged in the condensation nozzle of kettle cover 12
On 1210, the liquid that reaction product distills out when for being evaporated under reduced pressure is collected.
Further, as shown in Figure 1, peristaltic pump therein 4 includes the first peristaltic pump 41 and the second peristaltic pump 42, inlet
122 include the first inlet 1221 and the second inlet 1222, and the first peristaltic pump 41 is equipped with acid solution tank 411, the second peristaltic pump
42 are equipped with alkali liquid tank 421, and the liquid in acid solution tank 411 is by the adjusting of wriggling pump control mechanism 55 after the pumping of the first peristaltic pump
Reaction kettle 1 is entered by the first inlet 1221, the liquid in alkali liquid tank 421 is compacted through second by the adjusting of wriggling pump control mechanism 55
Reaction kettle 1 is entered by the second inlet 1222 after dynamic pump pumping, the pH value of reaction mass in reaction kettle 1 is adjusted with this.
Blender 2 includes agitating paddle 21, drive shaft 22 and driving motor 23, and top and the driving motor 23 of drive shaft 22 drive
Dynamic connection, its underpart are fixedly connected with agitating paddle 21, and agitating paddle 21 is extend into inside autoclave body 11, and driving motor 23 is placed in reaction kettle
1 upper end is simultaneously fixed by an iron stand 20.
The autoclave body 11 of reaction kettle 1 of the present invention is that double layer hollow is jacket structured, and interior be equipped with is used for keeping constant temperature
Constant temperature bath device 30 controls the temperature of reaction mass in autoclave body 11 with this.Medium in constant temperature bath device 30 can be selected water or
Oil is respectively formed as water bath with thermostatic control or constant temperature oil bath.
As shown in Fig. 2, charge door 121, the first inlet 1221, the second inlet 1222, ultrasonic probe mouth 124, temperature
Sensor port 125, pH electrode ports 126, conductivity sensor mouth 127, air inlet 128, sample tap 129 and condensation nozzle 1210 are all provided with
It sets on the circle using the central point of kettle cover 12 as the center of circle, and equidistantly distributed.Above each interface uses hickey, screw tip
It is equipped with containment member O-ring, can be operated under positive pressure and vacuum state, it is possible to use press filtration and suction filtration；Containment member O
Type circle is made of elastic material, preferably Teflon, epoxy resin or polyurethane, is mounted on interface；In addition, also visual reactant
It is that pressure requirements only realize sealing in interface using containment member O-ring.
In addition, being equipped with a dismountable filter structure 80 in 13 inside front of bottom, product particles is straight after being used to react
Take over filter washing.Filter structure includes strainer/filter membrane and pallet, and the aperture of strainer/filter membrane can be according to reaction solution and nano-particle
Grain size selected (more smaller than the grain size of reaction mass).The inner wall surface roughness of reaction kettle 1 is less than or equal to 0.4a, to prevent
Only inner wall absorption adhesion and aggregation, convenient for cleaning.The lower end base of bottom 13 is additionally provided with discharge port 131, for collecting described in warp
80 filtered filtrate of strainer；The lower end of condenser pipe 3 and discharge port 131 pass through 90 one end of hose and a solvent recovery unit respectively
It is connected, the other end of solvent recovery unit 90 is connected by hose with feeding device 50, and the solvent after recycling passes through master control
The feeding device 50 that device 5 processed controls is added in reaction kettle, is realized the recycling of material, is subtracted while reducing environmental pollution
The waste of few resource.Solvent recovery unit 90 is by solvent recovery container and vacuum pump group at by vacuumizing achievable reaction kettle
Vacuum filtration, solvent keeps in solvent recovery unit, and the liquid in condenser pipe receiving flask can also be sucked to solvent recovery dress
In setting.
Reaction kettle 1 can be one kind in stainless steel cauldron, glass reaction kettle and PVC reaction kettles.On the outside of air inlet
Hose on be additionally provided with control valve 1281, such as one-way control valve, for preventing back flow of gas.
It is externally provided with the protection blimp with visual window in reaction kettle, lighting device and camera shooting are housed on protection blimp
Head, camera can check experimental conditions by mobile phone wireless and Bluetooth control, available handsets in distal end and the non-experimental field in outside,
Also can record a video setting experiment reaction process, facilitate discovery and record reaction process.Wireless control can be also equipped on master controller
Switch can carry out wireless control to master controller.
Apparatus of the present invention can realize that the recycling of solvent specifically has to reduce the consumption of solvent by suction filtration etc.
Two ways：
(1) embodiment 1：
The vacuum pump for starting solvent recovery unit obtains nano material concentrated solution or powder using the mode of suction filtration, prepare and
Washing such as ethyl alcohol organic reagent used, which is directly stored in solvent recovery container, can directly be recycled as reaction reagent, pass through
Liquid feeding circulating pump is added to reaction system.Also liquid can be transferred to other containers from solvent recovery container, in case using.One
A little monodisperse silicas are prepared in experiment, can also optionally, and the solvent that solvent recovery unit is collected carries out pH value adjusting
Or other processing are carried out, it is recycled for using.
(2) embodiment 2：
Using vacuum distillation, reaction kettle, condenser pipe and solvent recovery unit.Reaction kettle is equipped with agitating device, heating dress
It sets, feed inlet, discharge port and pressure gauge, reaction kettle are connected by discharge port, condenser pipe and pipeline with solvent recovery unit, condensation
Pipe top is equipped with bleeding point, and solvent recovery unit lower end passes through feeding device circulating pump liquid feeding to reaction kettle by feeding tube.
It has the following advantages that：First, can be recycled by synthesizer recovered solvent, dirt of the organic solvent to environment is eliminated
Dye；Second is that synthesizer can prepare nano material powder with rapid batchization.
Such as in monodisperse silica prepares experiment, the first step carries out powder preparation in reaction kettle；Second step, it is cold
Solidifying pipe recycles the alcohol solvent in reaction kettle, and monodisperse silica powder or concentrate, condenser pipe recycling are obtained in reaction kettle
Solvent enter solvent recovery unit, recycling design enters reaction kettle by feeding tube and is used as the secondary use of raw material.
Specifically, ethyl alcohol, water, ammonium hydroxide are added by the feed inlet of reaction kettle, open motor and drive agitating device, by anti-
It answers the recirculated water in kettle chuck that temperature in the kettle is heated to specified value, ethyl orthosilicate and second is added by the feed inlet of reaction kettle
Alcohol, reaction start, opening conduits after the completion of reaction, open bleeding point, and the reading by observing pressure gauge judges the vacuum in kettle
Degree, after vacuum degree reaches specified value, condenser pipe starts to be condensed out the alcohol solvent in kettle, by controlling condensation time, condensate liquid
The quality of body adjusts the concentration of silica in kettle, and after a certain period of time, the solvent being condensed out enters solvent through pipeline and returns for condensation
Receiving apparatus, recovered solvent enter reaction kettle by feeding tube and reuse.
The concrete application of the present embodiment is introduced with reference to several experimental examples.
Experimental example 1：Monodisperse silica sphere particle shape preparation method of granules
Method 1：In a kettle, after concentrated ammonia liquor, ethyl alcohol, water stirring 30min are added from charge door 121, by positive silicic acid
Ethyl ester (TEOS) and alcohol mixeding liquid are added in reaction kettle, heated at constant temperature to certain temperature, and certain time, decompression is stirred by ultrasonic
Distillation filters removal solvent, and solvent is deposited to solvent recovery unit 90 in case recycles, with absolute ethyl alcohol ultrasonic cleaning 3 times,
Solvent is deposited to solvent recovery unit 90 in case recycling, then be cleaned by ultrasonic repeatedly with distilled water, with the measurement soda acid of pH electrodes 8
Property, it cleans to neutrality, also can set the automatic acid-base accommodation of pH value progress in master controller 5, obtain the list that grain size is certain grain size
Dispersed silicon dioxide spheric granules.Particle size can be changed by changing the amount of concentrated ammonia liquor, ethyl alcohol, water and TEOS.After recycling
Solvent by master controller 5 to feeding device 50 control be added in reaction kettle, can be controlled as desired by master controller 5
Peristaltic pump 4 adjusts pH value, realizes the recycling of material.
Method 2：Make seed with some particles prepared by method 1, a certain amount of concentrated ammonia liquor, ethyl alcohol, water stirring 30min be added,
Feeding device 50 (peristaltic pump) is controlled by master controller 5 a certain amount of with the flow velocity dropwise addition of 0.2mL/min-2mL/min
TEOS or TEOS and alcohol mixeding liquid are stirred by ultrasonic certain time with certain rotating speed, liquid obtained by the reaction are filtered or depressurized
Distillation centrifuges, and removes liquid, is cleaned by ultrasonic with absolute ethyl alcohol and distilled water, and organic solvent is deposited to solvent recovery unit 90
In case recycling, acid-base property is measured with pH electrodes 8, is cleaned to neutrality, also can set pH value progress automatic acid in master controller 5
Alkali is adjusted, and it is certain grain size monodisperse silica sphere particle shape particle to obtain grain size.Feeding device 50 is controlled by master controller 5
System, the monodisperse silica sphere particle shape particle of specified particle diameter can be prepared by controlling drop rate and sample-adding ratio.
Method 3：In a kettle, a certain amount of concentrated ammonia liquor, ethyl alcohol, water are added from charge door 121 and stirs 30min, centainly
Amount ethyl orthosilicate (TEOS) and alcohol mixeding liquid are added in reaction kettle, the control heated at constant temperature of master controller 5 to certain temperature,
Certain time is stirred by ultrasonic, obtains the monodisperse silica sphere particle shape particle that grain size is certain grain size.Added for 5 pairs by master controller
Expect that device 50 controls, a certain amount of TEOS or TEOS and alcohol mixeding liquid are added dropwise with certain flow rate, are stirred by ultrasonic with certain rotating speed
Liquid obtained by the reaction is filtered or is evaporated under reduced pressure by certain time, removes liquid, is cleaned by ultrasonic with absolute ethyl alcohol and distilled water,
Acid-base property, cleaning to neutrality are measured with pH electrodes 8.Also the automatic acid-base accommodation of pH value progress can be set in master controller 5.It is organic molten
Agent is deposited to solvent recovery unit 90 in case recycle, and certain grain size monodisperse silica sphere particle shape particle is obtained.Pass through master control
Device 5 processed controls drop rate and sample-adding ratio to feeding device 50 can prepare the monodisperse silica sphere particle shape of specified particle diameter
Grain.
Experimental example 2：Monodisperse polystyrene spheric granules preparation method
Method 1：In a kettle, after purging a period of time by 128 nitrogen of air inlet, continue to be passed through nitrogen protection, from
The a certain amount of ethyl alcohol of addition, polyvinylpyrrolidone at charge door 121, addition styrene monomer and azodiisobutyronitrile (or peroxide
Change benzoyl), control is stirred by ultrasonic at a certain temperature, after reacting a period of time, stops reaction and is cooled to room temperature, product filters
Or removal liquid is evaporated under reduced pressure or centrifuged in system, it is cleaned by ultrasonic with absolute ethyl alcohol and distilled water, obtains the list of certain grain size
Rnonodisperse polystyrene spheric granules.Change particle size by changing to match, conductivity value can be monitored by conductivity sensor 9 and sentenced
Disconnected response situation and whether the reaction was complete.
Method 2：In a kettle, after purging a period of time by 128 nitrogen of air inlet, continue to be passed through nitrogen protection, from
The a certain amount of ethyl alcohol of addition, polyvinylpyrrolidone at charge door 121, addition styrene monomer and azodiisobutyronitrile (or peroxide
Change benzoyl), control is stirred by ultrasonic at a certain temperature, after reacting a period of time, is controlled to feeding device 50 by master controller 5
System is added dropwise a certain amount of styrene monomer from certain interval of time from charge door 121 with certain flow rate, is stirred with certain rotating speed ultrasound
It mixes certain time, stops reaction and being cooled to room temperature, using filtering or vacuum distillation or one of centrifugation removal liquid in system
Body is cleaned by ultrasonic with absolute ethyl alcohol and distilled water, obtains the monodisperse polystyrene spheric granules of certain grain size.Matched by changing
Than changing particle size with drop rate, dripping quantity, conductivity value can be monitored by conductivity sensor 9 and judges response situation and is
It is no that the reaction was complete.
Experimental example 3：It is prepared by hollow silica ball
Method 1：Using in experimental example 2 method 1 or 2 synthetic polystyrene microballoon of method as template, surface is added and lives
Property agent hexadecyltrimethylammonium chloride self-assembles to template surface.Be added at one time from charge door 121 a certain amount of concentrated ammonia liquor,
Ethyl alcohol, water stir 30min, in a certain amount of ethyl orthosilicate (TEOS) and alcohol mixeding liquid to reaction kettle, add from charge door 121
Enter polystyrene microsphere template, master controller 5 controls heated at constant temperature to certain temperature, certain time is stirred by ultrasonic.By automatic
Sampling system timing sampling monitors shell thickness.Liquid obtained by the reaction is filtered or is evaporated under reduced pressure, liquid is removed, use is anhydrous
Ethyl alcohol and distilled water are cleaned by ultrasonic, and acid-base property, cleaning to neutrality are measured with pH electrodes 8.Also can in master controller 5 setting pH value into
The automatic acid-base accommodation of row.Also the automatic acid-base accommodation of pH value progress can be set in master controller 5.Organic solvent is deposited to solvent recovery and is filled
90 are set in case recycling.Finally obtained polymer microballoon is calcined, obtains regular hollow silica microsphere.
Method 2：Using in experimental example 2 method 1 or 2 synthetic polystyrene microballoon of method as template, surface is added and lives
Property agent hexadecyltrimethylammonium chloride self-assembles to template surface.Be added from charge door 121 a certain amount of concentrated ammonia liquor, ethyl alcohol,
Water stirs 30min, and polystyrene microsphere template is added from charge door 121, and master controller 5 controls feed system 50 with a constant speed
A certain amount of ethyl orthosilicate (TEOS) and alcohol mixeding liquid are added dropwise in reaction kettle by rate, heated at constant temperature to certain temperature, are surpassed
Sound stirs certain time.By automatic sampling system timing sampling, shell thickness is monitored.Liquid obtained by the reaction is filtered or subtracted
Pressure distillation, removes liquid, is cleaned by ultrasonic with absolute ethyl alcohol and distilled water, and acid-base property, cleaning to neutrality are measured with pH electrodes 8.?
The automatic acid-base accommodation of pH value progress can be set in master controller 5.Solvent is deposited to solvent recovery unit 90 in case recycling.Finally
Obtained polymer microballoon is calcined, regular hollow silica microsphere is obtained.
Experimental example 4：Nano-scale pucherite preparation method
Method 1：In a kettle, certain density salpeter solution, ammonium metavanadate and bismuth nitrate, ultrasonic agitation dissolving is added
Afterwards, alternative that a certain amount of P123 or PVP is added, different pH value are preset by master controller 5, continual ultrasonic stirring is wriggled
4 transmission liquid of pump reaches pH value, and peristaltic pump 4 is stopped.Presoma is placed in the reaction kettle of polytetrafluoroethyllining lining later, into
Row hydro-thermal reaction, it is dry later (also can be dry after dry after directly filtering or vacuum distillation without hydro-thermal reaction).Pass through control
It makes different pH value and prepares different-shape micro-or nano size pucherite.
Experimental example 5：Ceramic yellow color of bismuth vanadate clad by compound of silicate class preparation method
The preparation facilities of the present embodiment can also be used for ceramic yellow color of bismuth vanadate clad by compound of silicate class, including Huang
The preparation of color pigment BiVO4 and the preparation of heat safe yellow uitramarine BiVO4/SiO2, using compound of silicate class as silicon
Source, by coated with silica on the surface of pucherite, since the extremely strong inertia of silica makes BiVO4 can be resistant to 1000 DEG C of left sides
Right high temperature, can be used for the applications such as ceramic paint.It is specific as follows：
(1) hydro-thermal device using the present invention does not prepare BiVO4
In a kettle, the salpeter solution of 2mol/L is added, a certain amount of five water bismuth nitrate is added, after ultrasonic agitation dissolving
Ammonium metavanadate is added, after ultrasonic agitation dissolving, alternative is added a certain amount of P123 or PVP or is added without, and passes through master control
Device 5 processed presets different pH value, continual ultrasonic stirring, and peristaltic pump 4 transmits lye (such as ammonium hydroxide, sodium hydroxide or sodium bicarbonate solution)
Reach pH value, peristaltic pump 4 is automatically stopped work.Different pH value, heated at constant temperature a to constant temperature are adjusted to by master controller 5
It is dry after degree, ultrasonic agitation certain time, direct filtration drying or vacuum distillation, obtain the powder of micro-nano BiVO4.In 400-
Roasting obtains yellow uitramarine BiVO4 at 500 DEG C.
(2) device using the present invention prepares BiVO4 cooperation hydro-thermals
In a kettle, the salpeter solution of 2mol/L is added, a certain amount of five water bismuth nitrate is added, after ultrasonic agitation dissolving
Ammonium metavanadate is added, after ultrasonic agitation dissolving, alternative is added a certain amount of P123 or PVP or is added without, and passes through master control
Device 5 processed presets different pH value, continual ultrasonic stirring, and peristaltic pump transmits lye (such as ammonium hydroxide, sodium hydroxide or sodium bicarbonate solution)
Reach pH value, peristaltic pump is automatically stopped work.It is adjusted to different pH value by master controller, heated at constant temperature to certain temperature,
Certain time is stirred by ultrasonic, the precursor liquid prepared is opened into the discharge port below reaction kettle, it is anti-to transfer them to 100mL hydro-thermals
(it is 80% to keep filling rate) is answered in kettle, 6h is handled in 180 DEG C of constant temperature, after filtering, washing 3 times and absolute ethyl alcohol washs 3 times,
Gained yellow powder is in 60 DEG C of dry 12h, then is risen to from room temperature with the rate of 1 DEG C/min under air atmosphere in Muffle furnace
And 4h is kept at such a temperature, to obtain final product by 400 DEG C.
(3) method for using apparatus of the present invention to prepare coated with silica pucherite BiVO4/SiO2
In a kettle, certain density salpeter solution is added, a certain amount of ammonium metavanadate and bismuth nitrate is added, ultrasound is stirred
After mixing dissolving, alternative is added a certain amount of P123 or PVP or is added without, and presets different pH value, and continual ultrasonic stirring is compacted
Dynamic pump transmission liquid reaches pH value, and peristaltic pump is automatically stopped work.It is adjusted to certain different pH value, constant temperature by master controller
It is heated to certain temperature, certain time is stirred by ultrasonic, it is dry after dry after directly filtering or vacuum distillation, it obtains micro-nano
The powder of BiVO4.
Method 1：A certain amount of concentrated ammonia liquor, ethyl alcohol is added, 30min is stirred by ultrasonic together with the powder of BiVO4, makes BiVO4 for water
Powder evenly spread out in the solution, a certain amount of surfactant, a certain amount of ethyl orthosilicate (TEOS) and ethyl alcohol is added
Mixed liquor is added to be added in reaction kettle, heated at constant temperature to certain temperature, ultrasonic wave stirs certain time, a certain amount of positive silicic acid second
Ester (TEOS) and ethyl alcohol are added drop-wise to the speed of 0.2-3mL/min in reaction kettle by peristaltic pump, heated at constant temperature to certain temperature,
Ultrasonic wave stirring certain time obtains BiVO4/SiO2 by coated with silica on the surface of pucherite.Vacuum distillation removal liquid
Body or removal liquid are centrifuged, and are cleaned by ultrasonic with absolute ethyl alcohol and distilled water.BiVO4/SiO2 is obtained, heat safe Huang can be done
Color pigment BiVO4/SiO2.The roasting removal surfactant at 500 DEG C.By changing concentrated ammonia liquor, ethyl alcohol, water and TEOS
Amount changes the cladding thickness of particle size and SiO2.
It is added a certain amount of concentrated ammonia liquor, ethyl alcohol, water stirs 30min, and can will use this equipment preparation BiVO4 or through hydro-thermal legal system
It is added thereto by charge door after standby BiVO4 washings, is stirred by ultrasonic, so that the powder of BiVO4 is evenly spread out in the solution, add
Enter a certain amount of surfactant, a certain amount of ethyl orthosilicate (TEOS) and ethyl alcohol are added mixed liquor and are added to reaction kettle or a certain amount of
Ethyl orthosilicate (TEOS) and ethyl alcohol are added drop-wise to the speed of 0.2-3mL/min in reaction kettle by peristaltic pump, and heated at constant temperature arrives
Certain temperature, ultrasonic wave stirring certain time obtain BiVO4/SiO2 by coated with silica on the surface of pucherite.Filtering
Or vacuum distillation removal liquid or removal liquid are centrifuged, and are cleaned by ultrasonic with absolute ethyl alcohol and distilled water.Obtain BiVO4/
SiO2 can be heat safe yellow uitramarine BiVO4/SiO2.Amount by changing concentrated ammonia liquor, ethyl alcohol, water and TEOS changes grain
The cladding thickness of diameter size and SiO2.Electronic Speculum measurement, monitoring cladding thickness are carried out by automatic sampling system real time sample.
Experimental example 6：Using silica as the packet caryogram bismuth vanadium pigments preparation method of kernel
By after a series of monodisperse silica bead-ethanol-water solution ultrasonic disperse for synthesizing concentration, with concentrated nitric acid tune
Section is to neutrality, in a kettle, the salpeter solution of 2mol/L is added, and a certain amount of five water bismuth nitrate, ultrasonic agitation dissolving is added
After be added ammonium metavanadate, after ultrasonic agitation dissolving, alternative is added a certain amount of P123 or PVP or is added without, main control
Device 5 presets pH value, continual ultrasonic stirring, and peristaltic pump transmission lye (such as ammonium hydroxide, sodium hydroxide or sodium bicarbonate solution) reaches pH
Value, peristaltic pump are automatically stopped work.It is adjusted to different pH value by master controller 5, is dried through suction filtration, washing, 100 DEG C,
Calcining is able to the packet caryogram bismuth vanadium pigments that silica is kernel at 600 DEG C.
In addition, the preparation facilities of the present invention also can be used and prepare coloured polystyrene sphere, fluorescence polystyrene sphere, fluorescence
The materials such as silica.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
Variation is still in the protection scope of this invention.
Claims (10)
1. a kind of micro Nano material preparation facilities, which is characterized in that including reaction kettle (1), blender (2), charge door (121),
Condenser pipe (3), peristaltic pump (4) and master controller (5), the charge door (121) and condenser pipe (3) are arranged in the reaction kettle
(1) top, is respectively used to the addition of reaction mass and liquid that product distills out is collected, the agitating paddle of the blender (2)
(21) go deep into the reaction kettle (1), be used for the stirring of reaction mass, the peristaltic pump (4) is electrical with the master controller (5)
Connection, the peristaltic pump (4) are used for the pumping of acid & alkali liquid, to adjust by being connected inside hose and the reaction kettle (1)
State the pH value of reaction kettle (1) interior reaction mass；
The ultrasonic probe (6) for being disperseed to reaction mass and being cleaned, monitoring reactant material temperature are additionally provided in the reaction kettle (1)
The temperature sensor (7) of degree, the pH electrodes (8) for monitoring reaction mass pH value and the conductivity sensor (9) for monitoring extent of reaction, institute
It is electrical with the master controller (5) respectively to state ultrasonic probe (6), temperature sensor (7), pH electrodes (8) and conductivity sensor (9)
Connection, the master controller (5) are respectively monitored ultrasonic generation, temperature, pH value and the conductivity in the reaction kettle (1)
And control.
2. micro Nano material preparation facilities according to claim 1, which is characterized in that the reaction kettle (1) includes autoclave body
(11), kettle cover (12) and bottom (13), between the autoclave body (11) and kettle cover (12), removable between autoclave body (11) and bottom (13)
Fixed seal connection is unloaded, charge door (121), inlet (122), installing port (123), ultrasound are respectively equipped on the kettle cover (12)
Probe mouth (124), temperature sensor mouth (125), pH electrode ports (126), conductivity sensor mouth (127) and air inlet (128),
Described in installing port (123) be arranged at the center of the kettle cover (12), the inlet (122) is through hose and the peristaltic pump
(4) it is connected, the ultrasonic probe (6), temperature sensor (7), pH electrodes (8) and conductivity sensor (9) are dismountable respectively
It is sensed mounted on the ultrasonic probe mouth (124) of the kettle cover (12), temperature sensor mouth (125), pH electrode ports (126) and conductance
On device mouth (127), the blender (2) is mounted at the installing port (123) of the kettle cover (12), and the air inlet (128) is logical
Hose is crossed with setting to be connected in the gas tank (10) of the reaction kettle (1) outside.
It is corresponded in the upper surface of the kettle cover (12) and is equipped with charge pipe at the charge door (121), set on the charge pipe
There are feeding device (50), the feeding device (50) that one or more charging, the feeding device (50) and the master can be achieved
Controller (5) is electrically connected, auto feed of the master controller (5) to the feeding device (50) to the reaction kettle (1)
Action is monitored and controls.
3. micro Nano material preparation facilities according to claim 2, which is characterized in that be equipped in the master controller (5)
Ultrasonic controller (51), temperature controller (52), pH value display instrument (53), conductance controller (54), wriggling pump control mechanism (55)
With auto feed controller (56), the ultrasonic probe (6) is electrically connected with the ultrasonic controller (51), the temperature sensing
Device (7) is electrically connected with the temperature controller (52), and the conductivity sensor (9) electrically connects with the conductance controller (54)
It connects, the pH electrodes (8) are electrically connected with the pH value display instrument (53), and the pH value display instrument (53) and the peristaltic pump
Adjuster (55) is electrically connected, and the pH value information on the pH value display instrument (53) is passed to the wriggling pump control mechanism
(55), the peristaltic pump (4) is electrically connected with the wriggling pump control mechanism (55), and the feeding device (50) adds automatically with described
Expect that controller (56) is electrically connected.
4. micro Nano material preparation facilities according to claim 3, which is characterized in that be additionally provided on the kettle cover (12)
Sample tap (129) is equipped with probe tube (60) at the sample tap (129), and being equipped on the probe tube (60) has negative pressure
The sampling pump (70) of extract function, the sampling pump (70) are electrically connected with the master controller (5), the master controller (5)
The sampling pump (70) extraction reaction product can be automatically controlled at set time intervals；
Sampling controller (57), the sampling pump (70) and the sampling controller (57) are additionally provided in the master controller (5),
Reaction product is extracted for automatically controlling the sampling pump (70) at set time intervals；
Condensation nozzle (1210) is additionally provided on the kettle cover (12), the condenser pipe (3) is detachably arranged in the kettle cover
(12) on condensation nozzle (1210), the liquid that distills out of reaction product when the condensation and vacuum distillation of solvent when for heating reaction
Body is collected.
5. micro Nano material preparation facilities according to claim 4, which is characterized in that the probe tube (60) includes setting
Sampling inner tube (601) in the autoclave body (11), the sampling inner tube (601) are telescopic tube, and when sampling extends, and does not sample
When shrink.
6. micro Nano material preparation facilities according to claim 5, which is characterized in that the peristaltic pump (4) includes first
Peristaltic pump (41) and the second peristaltic pump (42), the inlet (122) include the first inlet (1221) and the second inlet
(1222), first peristaltic pump (41) is equipped with acid solution tank (411), and second peristaltic pump (42) is equipped with alkali liquid tank
(421), the liquid in the acid solution tank (411) by the adjusting of the wriggling pump control mechanism (55) through first peristaltic pump
The reaction kettle (1) is entered by first inlet (1221) after sending, the liquid in the alkali liquid tank (421) passes through described compacted
The adjusting of dynamic pump control mechanism (55) enters the reaction after second peristaltic pump pumping by second inlet (1222)
Kettle (1) adjusts the pH value of the reaction kettle (1) interior reaction mass with this.
The blender (2) includes agitating paddle (21), drive shaft (22) and driving motor (23), the top of the drive shaft (22)
It is drivingly connected with the driving motor (23), its underpart is fixedly connected with the agitating paddle (21), and the agitating paddle (21) is stretched into
In to the autoclave body (11), the driving motor (23) is placed in the reaction kettle (1) upper end and is fixed by an iron stand (20).
7. micro Nano material preparation facilities according to claim 6, which is characterized in that the autoclave body of the reaction kettle (1)
(11) be that double layer hollow is jacket structured, double layer hollow is jacket structured be connected with or it is interior set constant temperature bath device (30), for controlling
State the temperature of autoclave body (11) interior reaction mass.
8. micro Nano material preparation facilities according to claim 9, which is characterized in that the charge door (121), first into
Liquid mouth (1221), the second inlet (1222), ultrasonic probe mouth (124), temperature sensor mouth (125), pH electrode ports (126),
Conductivity sensor mouth (127), air inlet (128), sample tap (129) and condensation nozzle (1210) are arranged at the kettle cover
(12) central point is on the circle in the center of circle.
9. micro Nano material preparation facilities according to claim 8, which is characterized in that in the bottom (13) inside front
Equipped with a dismountable filter structure (80), the direct filtration washing for product particles after reacting；
The inner wall surface roughness of the reaction kettle (1) is less than or equal to 0.4a, to prevent inner wall absorption adhesion and aggregation, convenient for clear
It washes.
10. according to claim 1-9 any one of them micro Nano material preparation facilities, which is characterized in that the bottom (13)
Lower end base be additionally provided with discharge port (131) condenser pipe (3) lower end and discharge port (131) it is molten with one by hose respectively
Agent retracting device (90) one end is connected, and the other end of the solvent recovery unit (90) passes through hose and the feeding device
(50) it is connected, is used for the secondary use of material.
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