CN109433129A - A kind of integrated apparatus and preparation method preparing nano zero valence iron for laboratory - Google Patents
A kind of integrated apparatus and preparation method preparing nano zero valence iron for laboratory Download PDFInfo
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- CN109433129A CN109433129A CN201811313309.0A CN201811313309A CN109433129A CN 109433129 A CN109433129 A CN 109433129A CN 201811313309 A CN201811313309 A CN 201811313309A CN 109433129 A CN109433129 A CN 109433129A
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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
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/08—Apparatus therefor
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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
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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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
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses a kind of integrated apparatus and preparation method that nano zero valence iron is prepared for laboratory, integrated apparatus includes reaction preparation facilities, attachment device, separation cleaning device, heating, drying device, fixed support device, separation cleaning device is fixed on fixed support device bottom, reaction preparation facilities is connected to the top of separation cleaning device by attachment device, for carrying out sample preparation and separation cleaning process；Attachment device is connect with fixed support device by turnover mechanism, for separation cleaning device to be overturn 180 degree, heating, drying device is installed at outside the separation cleaning device of overturning 180 degree, for carrying out heating, drying process, negative pressure collecting device is connected in separation cleaning device, for carrying out material transfer flow.In short, the present invention will react, and clean, dry and collect integration operation, there is no the transfer processes of exposure for whole process, reduce material oxidation risk.
Description
Technical field
The invention belongs to material for water treatment preparation technical fields, and in particular to one kind prepares nano zero valence iron for laboratory
Integrated apparatus and preparation method.
Background technique
In recent years, nanometer recovery technique is greatly improved in environmental science.Nanometer part iron particle size
1-100nm, as particle diameter reduces, the surface area of nanoparticle and surface can be increased rapidly, and also be easier to be oxidized.Study table
Bright, zeroth order iron material especially nanoscale zero-valent iron material is due to that can repair a variety of environmental contaminants with high reactivity
The features such as, become a very active research field in current environmental pollution recovery technique.Extraction and nanometer iron metal can effectively drop
Such as many organic matters of halogenated hydrocarbons, alkenyl halide, halogenated aromatic, organo-chlorine pesticide are solved, can also be removed with nano zero valence iron
The inorganic environment pollutant of heavy metal Cr (VI) etc. in nitrate nitrogen and surface water body in water body.
By to laboratory prepare the materials such as nano zero valence iron preparation, separation, cleaning process the study found that due to material
Special nature (oxidizable), lead to entirely to prepare filtering, separation, drying course will ensure the environment in anaerobic, so that whole
A preparation, separation, drying process are inconvenient to operate, and traditional method is that preparation solution is transferred to the operation of anaerobism glove box, use
Separation, cleaning be filter paper-funnel and centrifugation method " filter paper-funnel " process is inconvenient for operation, single fractional dose is limited, point
From the disadvantages of time-consuming, loss is big, " centrifugation " method is on the one hand oxidizable, loss is big, is on the other hand only applicable to quality weight
Material, therefore go to greatly improve nano zero valence iron and load prepared by laboratory we have invented a whole set of experimental method and equipment
The working efficiency of material etc..
Summary of the invention
For the technical problem present on, the present invention provides a kind of integration that nano zero valence iron is prepared for laboratory
Device.
Technology contents of the invention are as follows: a kind of integrated apparatus that nano zero valence iron is prepared for laboratory, including reaction
Preparation facilities, attachment device, separation cleaning device, heating, drying device, fixed support device；
The reaction preparation facilities includes tank body one, stirring rod, stirring motor, separatory funnel, the top of the tank body one
Equipped with inlet one, bottom centre position is equipped with liquid outlet one, and the lower sidewall of tank body one is equipped with air inlet one, the air inlet
One is equipped with air intake valve one, and the stirring motor is arranged in one top center of tank body, and the stirring rod is located at tank body one
Inside, and stirring rod upper end is connected with the output shaft of stirring motor, the separatory funnel is arranged in one top side of tank body, liquid separation
The lower end of funnel extends to inside tank body one；
The attachment device includes that siphunculus, main valve and connection are moved close to somebody's ear, and the upper end of the siphunculus and the liquid outlet one are logical
Threaded connection is crossed, the main valve is arranged on siphunculus, and leans on one end of liquid in-out mouth one, and the connection is moved close to somebody's ear two totally, point
It is not symmetrically welded at the left and right sides of siphunculus；
The separation cleaning device includes tank body two and filter membrane retainer plate, and the tank body two divides for cleaning part and separation unit,
The top of the cleaning part is equipped with inlet two, is equipped with air inlet two at the upper side wall of cleaning part, the air inlet two is equipped with
Air intake valve two, the inlet two are connected through a screw thread with siphunculus lower end, and the bottom of the separation unit is equipped with liquid outlet two, institute
The upper port that filter membrane retainer plate level is connected to separation unit is stated, nano-filtration membrane, the cleaning part are fixed in filter membrane retainer plate
Pass through flanged joint between separation unit；
The heating, drying device includes heating jacket and gas heater, and the heating jacket is detachably arranged at separation
The outside of cleaning device, and heating jacket is fitted closely with separation cleaning device lateral wall, the gas heater setting into
The outer end of port two, the heating jacket and gas heater with external power supply by being connected；
The fixed support device includes support base, support frame and turnover mechanism, and it is clear that the support base is located at separation
The lower section of cleaning device, is respectively fixedly connected in the upper end two sides of support base, the upper end of support frame is set totally by support frame as described above two
Have a mounting hole, the mounting hole and the connection of attachment device position of moving close to somebody's ear are concordant, the overturning structure be connected to connection move close to somebody's ear with
Between mounting hole, for spinning upside down separation cleaning device.
Further, the heating jacket is the chimeric splicing structure in left and right, by the heat-conducting layer of inside, middle part heating layer and
The insulating layer in outside is constituted, and the heat-conducting layer is the grapheme foam to match with separation cleaning device contour structures, described to add
Thermosphere is heat tape, and the insulating layer is vacuum heat-insulation plate.The chimeric splicing structure in left and right conveniently adds assembly and disassembly, utilizes heating
Collet carries out drying heating to the sample in separation cleaning device in situ, can avoid entering sky during shifting baking oven
Gas causes to aoxidize, to influence the quality of sample.
Further, the turnover mechanism includes connecting plate one, connecting plate two and lock, the inner end of the connecting plate one
It is connect with one and moves close to somebody's ear to be bolted to connection, the outer end of connecting plate one is collateral through the mounting hole and one by rotation axis
Support is flexibly connected, and the lock is arranged on the outer end of rotation axis, for limiting the activity of turnover mechanism, the connecting plate
Two inner end is connect with another to be moved close to somebody's ear to be bolted to connection, and the outer end of connecting plate two passes through crank rocker penetrating mounting holes
It is flexibly connected with another side stand component.Separation cleaning device is spun upside down using turnover mechanism, can be made during drying
Dry sample is obtained by gravity fall, convenient for collecting.
Further, the lock includes turntable and retainer ring, and the center of the turntable is equipped with and the rotation
The adaptation threaded hole of axle thread connection, the retainer ring are positioned close to one end of the turntable of mounting hole.It can prevent turnover mechanism from sending out
Raw movement guarantees the stability of entire drying and transfer flow.
Further, auxiliary-valve is additionally provided in the siphunculus, the auxiliary-valve is close to inlet two.Close auxiliary-valve be for
Preventing the dry sample from falling into narrow eyes into a slit has in the siphunculus of heating and heat preservation, influences the drying effect of sample, and main valve is close to receiving
Ji Kou, closing are to be mixed into air during sample transfer in order to prevent.
Further, the tank body one and tank body two are transparent glass material, it may be convenient to observe experimental conditions.
The present invention also provides the methods for preparing nano zero valence iron using above-mentioned integrated apparatus, comprising the following steps:
Sample preparation process: closing the main valve and auxiliary-valve, opens the air intake valve one and the inlet
Valve on one imports green vitriol solution from inlet one, is passed through nitrogen aeration 5min from the air inlet one, beats
The stirring motor is opened, drives the stirring rod that solution is sufficiently stirred, reducing agent is added by the separatory funnel, and
The rate of addition for controlling reducing agent is 3 drops/s, until reducing agent is added dropwise, reaction is prepared into sample, closes stirring motor, is opened
Main valve and auxiliary-valve flow into solution with sample in the separation cleaning device by the siphunculus；
Separation cleaning process: first closing the valve on inlet one, and open the liquid outlet two, will from air inlet one into
The nitrogen flow entered promotes 1 times, connects positive-pressure filter unit in two bottom of liquid outlet, carries out positive pressure to solution in tank body two
Filtering obtains concentrate, closes liquid outlet two, then opens inlet one and ultrapure water is added, and the volume of ultrapure water is the concentration
5 times of liquid close air intake valve one, again positive press filtration, and use alternately cleaning 3 times of ultrapure water and dehydrated alcohol repeatedly, finally
One time is washes of absolute alcohol, and positive press filtration obtains the residue in the nanofiltration membrane on filter membrane retainer plate, close out liquid to doing
Mouth two；
Heating, drying process: main valve and auxiliary-valve are closed, turntable is rotated to retainer ring to the installation for exiting support frame as described above
Hole rotates the crank rocker, connecting plate one, connecting plate two drive under, by separation cleaning device overturn 180 degree, then will
Turntable rotation playback is locked, and is installed heating jacket additional outside separation cleaning device, is heated to tank body two, and in air inlet
Install gas heater on mouth two additional, regulation heating temperature preheating opens the liquid outlet two at air intake valve two and top, from air inlet
The nitrogen that mouth two is passed through enter in tank body two after gas heater heats, then flow out from liquid outlet two, return in the nitrogen of heating
Under stream protection atmosphere, the residue in nanofiltration membrane is dried, after drying, obtains solids；Closing heating jacket,
Gas heater is passed through nitrogen at room and flows back in tank body two, cooled down, and closes air intake valve two and liquid outlet two；
Material transfer flow: negative pressure collecting device is connected in the lower end of siphunculus, main valve and auxiliary-valve are opened, after cooling
Material be collected it is spare.
Further, the negative pressure collecting device includes negative pressure bottle body, the screw thread bottleneck that negative pressure bottle body upper end is arranged in, with
And the switch valve one on the screw thread bottleneck is set, after screw thread bottleneck is connected with liquid outlet two, valve one is turned on the switch, is collected
After, turn off the switch valve one, it is ensured that air will not be mixed into negative pressure bottle body, prevent specimen material from aoxidizing.
Further, the inside of the negative pressure bottle body is additionally provided with interception filter membrane, and negative pressure bottle side wall bottom is equipped with connector,
The connector is equipped with switch valve two, and connector is connected with negative pressure generator by exhaust tube.The capacity of negative pressure bottle body is limited,
It is smaller to will cause negative pressure during collecting specimen material using negative pressure, the problems such as low there are collection efficiency is easy, in negative pressure
The additional negative pressure generator of bottle body can form biggish negative pressure, can effectively solve the above problems.
It should be noted that integrated apparatus of the invention can also be used to prepare other oxidizable materials, such as nanometer
Zinc powder, charcoal load nano zero valence iron, loaded on mineral material nano zero valence iron etc..
Compared with prior art, beneficial effects of the present invention:
1. integrated design for disassembly is convenient for operation, cleaning；
2. organic transparent glass material facilitates look at whole experiment process；
3. entire preparation, separation, cleaning, drying course are all completed under nitrogen protection, centre does not have transfer process, reduces
The material oxidation risk of whole process；
It, can be by adjusting nitrogen flow tune while material has obtained protection 4. cleaning process is filtered using positive pressure of nitrogen
Control entire cleaning process.Greatly reinforce the efficiency of entire cleaning, increased 18-90 times of efficiency.Furthermore it entirely separates, cleaned
The proportion of goods damageds are well below traditional separation, cleaning way afterwards；
5. cleaning, drying, collecting process, there is no the transfer processes of exposure, material oxidation risk is reduced.
Detailed description of the invention
Fig. 1 is the structure chart of sample preparation and separation cleaning process of the invention；
Fig. 2 is heating, drying and the structure chart of material transfer flow in the embodiment of the present invention 1；
Fig. 3 is heating, drying and the structure chart of material transfer flow in the embodiment of the present invention 2.
Wherein, 1- react preparation facilities, 10- tank body one, 11- stirring rod, 12- stirring motor, 13- separatory funnel, 14- into
Liquid mouth one, 15- liquid outlet one, 16- air inlet one, 17- air intake valve one, 2- attachment device, 20- siphunculus, 21- main valve, 22-
Connection move close to somebody's ear, 23- auxiliary-valve, 3- separation cleaning device, 30- tank body two, 31- filter membrane retainer plate, 32- inlet two, 33- air inlet
Mouth two, 34- air intake valve two, 35- liquid outlet two, 36- flange, 4- heating, drying device, 40- heating jacket, the heating of 41- gas
Device, 5- fixed support device, 50- support base, 51- support frame, 510- mounting hole, 52- turnover mechanism, 520- connecting plate one,
521- connecting plate two, 522- lock, 523- rotation axis, 524- crank rocker, 525- turntable, 526- retainer ring, 6- negative pressure are collected
Device, 60- negative pressure bottle body, 61- screw thread bottleneck, 62- switch valve one, 63- connector, 64- switch valve two, 65- intercept filter membrane,
66- negative pressure generator.
Specific embodiment
Explanation is further explained to the present invention with attached drawing 1-3 combined with specific embodiments below.
Embodiment 1
As shown in Figure 1, a kind of integrated apparatus that nano zero valence iron is prepared for laboratory, including reaction preparation facilities 1,
Attachment device 2, separation cleaning device 3, heating, drying device 4, fixed support device 5；Reacting preparation facilities 1 includes tank body one
10, the top of stirring rod 11, stirring motor 12, separatory funnel 13, tank body 1 is equipped with inlet 1, and bottom centre position is set
There is liquid outlet 1, the lower sidewall of tank body 1 is equipped with air inlet 1, and air inlet 1 is equipped with air intake valve 1, stirs
Mix motor 12 be arranged in one 10 top center of tank body, stirring rod 11 is located inside tank body 1, and 11 upper end of stirring rod and
The output shaft of stirring motor 12 is connected, and the separatory funnel 13 is arranged in one 10 top side of tank body, the lower end of separatory funnel 13
It extends to inside tank body 1；
As shown in Figure 1, attachment device 2 includes that siphunculus 20, main valve 21 and connection move close to somebody's ear 22, the upper end of siphunculus 20 and liquid out
Mouthfuls 1 are connected through a screw thread, and main valve 21 is arranged on siphunculus 20, and lean on one end of liquid in-out mouth 1, and connection is moved close to somebody's ear 22 total
Two, respectively symmetrically it is welded on the left and right sides of siphunculus 20；As shown in Figure 1-3, being additionally provided with auxiliary-valve 23, auxiliary-valve in siphunculus 20
23 close to inlet 2 32.Closing auxiliary-valve 23 is the siphunculus 20 that sample dry in order to prevent falls into that narrow eyes into a slit has heating and heat preservation
It is interior, influence the drying effect of sample, and main valve 21 is close to collection port, closing is mixed during sample transfer in order to prevent
Enter air.
As shown in Figure 1, separation cleaning device 3 includes tank body 2 30 and filter membrane retainer plate 31,2 30 points of tank body are cleaning part
And separation unit, the top of cleaning part are equipped with inlet 2 32, are equipped with air inlet 2 33, air inlet 2 33 at the upper side wall of cleaning part
It is equipped with air intake valve 2 34, inlet 2 32 is connected through a screw thread with 20 lower end of siphunculus, and the bottom of separation unit is equipped with liquid outlet
2 35,31 level of filter membrane retainer plate is connected to the upper port of separation unit, is fixed with nano-filtration membrane in filter membrane retainer plate 31, cleaning
It is connected between portion and separation unit by flange 36；Wherein, the tank body 1 and tank body 2 30 are transparent glass material, can be with
Easily observe experimental conditions.
As shown in Figures 2 and 3, heating, drying device 4 includes heating jacket 40 and gas heater 41, and heating jacket 40 is removable
The outside that separation cleaning device 3 is set is unloaded, and heating jacket 40 is fitted closely with 3 lateral wall of separation cleaning device, gas adds
The outer end of air inlet 2 33 is arranged in hot device 41, and heating jacket 40 and gas heater 41 with external power supply by being connected；Wherein,
Heating jacket 40 is the chimeric splicing structure in left and right, is made of, leads the insulating layer of the heat-conducting layer of inside, the heating layer at middle part and outside
Thermosphere is the grapheme foam to match with 3 contour structures of separation cleaning device, and heating layer is heat tape, and insulating layer is vacuum
Insulation board.The chimeric splicing structure in left and right conveniently adds assembly and disassembly, using heating jacket 40 in situ in separation cleaning device 3
Sample carries out drying heating, can avoid entering air during shifting baking oven, causes to aoxidize, to influence the matter of sample
Amount.
As shown in Figure 1, fixed support device 5 includes support base 50, support frame 51 and turnover mechanism 52, support base 50
Positioned at the lower section of separation cleaning device 3, support frame 51 totally two, it is respectively fixedly connected in the upper end two sides of support base 50, branch
The upper end of support 51 is equipped with mounting hole 510, and mounting hole 510 and the connection of attachment device 2 22 positions of moving close to somebody's ear are concordant, overturning structure 52
It is connected to connection to move close to somebody's ear between 22 and mounting hole 510, for spinning upside down separation cleaning device 3.Turnover mechanism 52 includes connection
Plate 1, connecting plate 2 521 and lock 522, the inner end of connecting plate 1 is connect with one to be moved close to somebody's ear 22 to be bolted
The outer end of connection, connecting plate 1 is flexibly connected by 523 penetrating mounting holes 510 of rotation axis with a side stand component 51, lock
522 are arranged on the outer end of rotation axis 523, for limiting the activity of turnover mechanism 52, the inner end of connecting plate 2 521 and another
Connection is moved close to somebody's ear 22 to be bolted to connection, the outer end of connecting plate 2 521 by 524 penetrating mounting holes 510 of crank rocker with it is another
One side stand component 51 is flexibly connected.Separation cleaning device 3 is spun upside down using turnover mechanism 52, can during drying,
So that dry sample by gravity fall, is convenient for collecting.As shown in Figure 1, lock 522 includes turntable 525 and retainer ring 526,
The center of turntable 525, which is equipped with, is adapted to threaded hole with what rotation axis 523 was threadedly coupled, and retainer ring 526 is positioned close to mounting hole
One end of 510 turntable 525.It can prevent turnover mechanism 52 from moving, guarantee the stability of entire drying and transfer flow.
The method for preparing nano zero valence iron using above-mentioned integrated apparatus, comprising the following steps:
1 sample preparation process: closing main valve 21 and auxiliary-valve 23, opens on air intake valve 1 and inlet 1
Valve, import green vitriol solution from inlet 1, be passed through nitrogen aeration 5min from air inlet 1, opening stirs
Motor 12 is mixed, solution is sufficiently stirred in driving stirring rod 11, reducing agent is added by separatory funnel 13, and control reducing agent
Rate of addition be 3 drops/s, until reducing agent is added dropwise, reaction is prepared into sample, closes stirring motor 12, opens main valve 21
Solution with sample is flowed into separation cleaning device 3 by siphunculus 20 with auxiliary-valve 23；
2 separation cleaning processes: first closing the valve on inlet 1, and open liquid outlet 2 35, will be from air inlet one
16 nitrogen flows entered promote 1 times, connect positive-pressure filter unit in 2 35 bottom of liquid outlet, carry out to solution in tank body 2 30
Positive press filtration obtains concentrate, closes liquid outlet 2 35, then opens inlet 1 and ultrapure water is added, and the volume of ultrapure water is
5 times of concentrate close air intake valve 1, again positive press filtration, and repeatedly with the alternately cleaning 3 of ultrapure water and dehydrated alcohol
Time, last time is washes of absolute alcohol, and positive press filtration obtains the residual in the nanofiltration membrane on filter membrane retainer plate 31 to doing
Object closes liquid outlet 2 35；
3 heating, drying processes: closing main valve 21 and auxiliary-valve 23, and support frame is exited in the rotation of turntable 525 to retainer ring 526
51 mounting hole 510, rotating crank rocking bar 524, connecting plate 1, connecting plate 2 521 drive under, separation cleaning is filled
3 overturning 180 degrees are set, then the rotation playback of turntable 525 is locked, install heating jacket 40 additional outside separation cleaning device 3, it is right
Tank body 2 30 is heated, and installs gas heater 41 additional on air inlet 2 33, and intake valve is opened in regulation heating temperature preheating
Door 2 34 and the liquid outlet 2 35 at top, the nitrogen being passed through from air inlet 2 33 enter tank body after the heating of gas heater 41
In 2 30, then from the outflow of liquid outlet 2 35, in the case where the nitrogen reflux of heating protects atmosphere, to the residue progress in nanofiltration membrane
Drying, after drying, obtains solids；Heating jacket 40, gas heater 41 are closed, is passed through nitrogen at room in tank body 2 30
Interior reflux, is cooled down, and air intake valve 2 34 and liquid outlet 2 35 are closed；
4 material transfer flows: connecting negative pressure collecting device 6 in the lower end of siphunculus 20, open main valve 21 and auxiliary-valve 23,
Material after cooling is collected spare.As shown in Fig. 2, negative pressure collecting device 6 includes negative pressure bottle body 60, is arranged in negative pressure bottle
The screw thread bottleneck 61 of 60 upper end of body, and the switch valve 1 being arranged on screw thread bottleneck 61, by screw thread bottleneck 61 and liquid outlet
After 2 35 are connected, valve 1 is turned on the switch, after collection, turns off the switch valve 1, it is ensured that will not mix in negative pressure bottle body 60
Enter air, prevents specimen material from aoxidizing.
Further, the inside of negative pressure bottle body 60, which is additionally provided with, intercepts filter membrane 65, and 60 sidewall bottom of negative pressure bottle body is equipped with connection
Mouth 63, connector 63 are equipped with switch valve 2 64, and connector 63 is connected with negative pressure generator 66 by exhaust tube.Negative pressure bottle body 60
Capacity it is limited, it is smaller during collecting specimen material using negative pressure to will cause negative pressure, is easy low etc. there are collection efficiency
Problem, outside negative pressure bottle body 60 plus negative pressure generator 66 can form biggish negative pressure, can effectively solve the above problems.
Embodiment 2
The present invention is substantially the same manner as Example 1, the difference is that:
The method for preparing nano zero valence iron using above-mentioned integrated apparatus, comprising the following steps:
1 sample preparation process: closing main valve 21 and auxiliary-valve 23, opens on air intake valve 1 and inlet 1
Valve, import green vitriol solution from inlet 1, be passed through nitrogen aeration 5min from air inlet 1, opening stirs
Motor 12 is mixed, solution is sufficiently stirred in driving stirring rod 11, reducing agent is added by separatory funnel 13, and control reducing agent
Rate of addition be 3 drops/s, until reducing agent is added dropwise, reaction is prepared into sample, closes stirring motor 12, opens main valve 21
Solution with sample is flowed into separation cleaning device 3 by siphunculus 20 with auxiliary-valve 23；
2 separation cleaning processes: first closing the valve on inlet 1, and open liquid outlet 2 35, will be from air inlet one
16 nitrogen flows entered promote 1 times, connect positive-pressure filter unit in 2 35 bottom of liquid outlet, carry out to solution in tank body 2 30
Positive press filtration obtains concentrate, closes liquid outlet 2 35, then opens inlet 1 and ultrapure water is added, and the volume of ultrapure water is
5 times of concentrate close air intake valve 1, again positive press filtration, and repeatedly with the alternately cleaning 3 of ultrapure water and dehydrated alcohol
Time, last time is washes of absolute alcohol, and positive press filtration obtains the residual in the nanofiltration membrane on filter membrane retainer plate 31 to doing
Object closes liquid outlet 2 35；
3 heating, drying processes: closing main valve 21 and auxiliary-valve 23, and support frame is exited in the rotation of turntable 525 to retainer ring 526
51 mounting hole 510, rotating crank rocking bar 524, connecting plate 1, connecting plate 2 521 drive under, separation cleaning is filled
3 overturning 180 degrees are set, then the rotation playback of turntable 525 is locked, install heating jacket 40 additional outside separation cleaning device 3, it is right
Tank body 2 30 is heated, and installs gas heater 41 additional on air inlet 2 33, and intake valve is opened in regulation heating temperature preheating
Door 2 34 and the liquid outlet 2 35 at top, the nitrogen being passed through from air inlet 2 33 enter tank body after the heating of gas heater 41
In 2 30, then from the outflow of liquid outlet 2 35, in the case where the nitrogen reflux of heating protects atmosphere, to the residue progress in nanofiltration membrane
Drying, after drying, obtains solids；Heating jacket 40, gas heater 41 are closed, is passed through nitrogen at room in tank body 2 30
Interior reflux, is cooled down, and air intake valve 2 34 and liquid outlet 2 35 are closed；
4 material transfer flows: connecting negative pressure collecting device 6 in the lower end of siphunculus 20, open main valve 21 and auxiliary-valve 23,
Material after cooling is collected spare.As shown in Fig. 2, negative pressure collecting device 6 includes negative pressure bottle body 60, is arranged in negative pressure bottle
It oh blocks the inside of the screw thread bottleneck 61 of 60 upper end of body, the switch valve 1 and negative pressure bottle body 60 that are arranged on screw thread bottleneck 61
Cut-off filter film 65, the connector 63 of 60 sidewall bottom of negative pressure bottle body, connector 63 are equipped with switch valve 2 64, and connector 63 passes through pumping
Tracheae is connected with negative pressure generator 66.After screw thread bottleneck 61 is connected with liquid outlet 2 35, by negative pressure generator 66 to negative pressure
Bottle body 60 carries out negative-pressure ward, the drying sample material in tank body 2 30 is collected into negative pressure bottle body 60, and turn off the switch valve
One 62 and switch valve 2 64.Since the capacity of negative pressure bottle body 60 is limited, can be made during collecting specimen material using negative pressure
It is smaller at negative pressure, it is easy the problems such as low there are collection efficiency, adds negative pressure generator 66 that can be formed outside negative pressure bottle body 60 biggish
Negative pressure can effectively solve the above problems.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment or equivalent replacement of some of the technical features；And
These are modified or replaceed, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (9)
1. a kind of integrated apparatus for preparing nano zero valence iron for laboratory, which is characterized in that including reacting preparation facilities
(1), attachment device (2), separation cleaning device (3), heating, drying device (4), fixed support device (5)；
The reaction preparation facilities (1) includes tank body one (10), stirring rod (11), stirring motor (12), separatory funnel (13), institute
The top for stating tank body one (10) is equipped with inlet one (14), and bottom centre position is equipped with liquid outlet one (15), tank body one (10)
Lower sidewall is equipped with air inlet one (16), and the air inlet one (16) is equipped with air intake valve one (17), the stirring motor
(12) it is arranged in tank body one (10) top center, the stirring rod (11) is located at tank body one (10) inside, and stirring rod
(11) upper end is connected with the output shaft of stirring motor (12), and the separatory funnel (13) is arranged in tank body one (10) top side,
It is internal that the lower end of separatory funnel (13) extends to tank body one (10)；
The attachment device (2) includes that (22) are moved close to somebody's ear in siphunculus (20), main valve (21) and connection, the upper end of the siphunculus (20) with
The liquid outlet one (15) is connected through a screw thread, and the main valve (21) is arranged on siphunculus (20), and leans on liquid in-out mouth one
(15) one end, the connection are moved close to somebody's ear (22) totally two, to be respectively symmetrically welded on the left and right sides of siphunculus (20)；
The separation cleaning device (3) includes tank body two (30) and filter membrane retainer plate (31), and the tank body two (30) is divided into cleaning
Portion and separation unit, the top of the cleaning part are equipped with inlet two (32), are equipped with air inlet two (33) at the upper side wall of cleaning part,
The air inlet two (33) is equipped with air intake valve two (34), the inlet two (32) and siphunculus (20) lower end and is connected by screw thread
It connects, the bottom of the separation unit is equipped with liquid outlet two (35), the horizontal upper end for being connected to separation unit of the filter membrane retainer plate (31)
Mouthful, it is fixed with nano-filtration membrane in filter membrane retainer plate (31), is connected between the cleaning part and separation unit by flange (36)；
The heating, drying device (4) includes heating jacket (40) and gas heater (41), and the heating jacket (40) is removable
It unloads and is arranged in the outside of separation cleaning device (3), and heating jacket (40) is fitted closely with separation cleaning device (3) lateral wall,
In the outer end of air inlet two (33), the heating jacket (40) and gas heater (41) are logical for gas heater (41) setting
It crosses and is connected with external power supply；
The fixed support device (5) includes support base (50), support frame (51) and turnover mechanism (52), the support base
(50) it is located at the lower section of separation cleaning device (3), support frame as described above (51) totally two, is respectively fixedly connected in support base (50)
Upper end two sides, the upper end of support frame (51) is equipped with mounting hole (510), the connection of the mounting hole (510) and attachment device (2)
Moving close to somebody's ear, (22) position is concordant, and the overturning structure (52) is connected to connection and moves close to somebody's ear between (22) and mounting hole (510), for up and down
It overturns separation cleaning device (3).
2. a kind of integrated apparatus for preparing nano zero valence iron for laboratory according to claim 1, which is characterized in that
The heating jacket (40) is the chimeric splicing structure in left and right, by the insulating layer of the heat-conducting layer of inside, the heating layer at middle part and outside
It constitutes, the heat-conducting layer is the grapheme foam to match with separation cleaning device (3) contour structures, and the heating layer is that electricity adds
The torrid zone, the insulating layer are vacuum heat-insulation plate.
3. a kind of integrated apparatus for preparing nano zero valence iron for laboratory according to claim 1, which is characterized in that
The turnover mechanism (52) includes connecting plate one (520), connecting plate two (521) and lock (522), the connecting plate one
(520) inner end connect with one move close to somebody's ear (22) be bolted to connection, the outer end of connecting plate one (520) passes through rotation axis
(523) it is flexibly connected through the mounting hole (510) with a side stand component (51), the lock (522) is arranged in rotation axis
(523) on outer end, for limiting the activity of turnover mechanism (52), the inner end of the connecting plate two (521) is connect with another
Move close to somebody's ear (22) be bolted to connection, the outer end of connecting plate two (521) passes through crank rocker (524) penetrating mounting holes (510)
It is flexibly connected with another side stand component (51).
4. a kind of integrated apparatus for preparing nano zero valence iron for laboratory according to claim 3, which is characterized in that
The lock (522) includes turntable (525) and retainer ring (526), and the center of the turntable (525) is equipped with and the rotation
The adaptation threaded hole that axis (523) is threadedly coupled, the retainer ring (526) are positioned close to the one of the turntable (525) of mounting hole (510)
End.
5. a kind of integrated apparatus for preparing nano zero valence iron for laboratory according to claim 1, which is characterized in that
It is additionally provided with auxiliary-valve (23) in the siphunculus (20), the auxiliary-valve (23) is close to inlet two (32).
6. a kind of integrated apparatus for preparing nano zero valence iron for laboratory according to claim 1, which is characterized in that
It is additionally provided with auxiliary-valve (23) in the siphunculus (20), the auxiliary-valve (23) is close to inlet two (32).
7. a kind of integrated apparatus for preparing nano zero valence iron for laboratory according to claim 1, which is characterized in that
The tank body one (10) and tank body two (30) are transparent glass material.
8. the method for preparing nano zero valence iron using above-mentioned integrated apparatus, which comprises the following steps:
(1) sample preparation process: closing the main valve (21) and auxiliary-valve (23), open the air intake valve one (17) and
Valve on the inlet one (14) imports green vitriol solution from inlet one (14), from the air inlet one
(16) it is passed through nitrogen aeration 5min, the stirring motor (12) is opened, the stirring rod (11) is driven sufficiently to stir solution
It mixes, the rate of addition that reducing agent is added by the separatory funnel (13), and controls reducing agent is 3 drops/s, until reducing agent is added dropwise
It finishes, reaction is prepared into sample, closes stirring motor (12), opens main valve (21) and auxiliary-valve (23) for solution with sample
It is flowed into the separation cleaning device (3) by the siphunculus (20)；
(2) separation cleaning process: first closing the valve on inlet one (14), and open the liquid outlet two (35), will from into
The nitrogen flow that port one (16) enters promotes 1 times, positive-pressure filter unit is connected in liquid outlet two (35) bottom, to tank body
The interior solution in two (30) carries out positive press filtration, obtains concentrate, closes liquid outlet two (35), then opens inlet one (14) and be added and surpass
Pure water, the volume of ultrapure water are 5 times of the concentrate, are closed air intake valve one (17), again positive press filtration, and repeatedly with super
Pure water and dehydrated alcohol alternately cleaning 3 times, last time are washes of absolute alcohol, and positive press filtration obtains filter membrane retainer plate to doing
(31) residue in nanofiltration membrane on is closed liquid outlet two (35)；
(3) heating, drying process: closing main valve (21) and auxiliary-valve (23), and turntable (525) rotation to retainer ring (526) is exited
The mounting hole (510) of support frame as described above (51), rotates the crank rocker (524), in connecting plate one (520), connecting plate two
(521) under drive, separation cleaning device (3) are overturn into 180 degree, then turntable (525) rotation playback is locked, separated
Heating jacket (40) are installed additional outside cleaning device (3), tank body two (30) are heated, and install gas additional on air inlet two (33)
Body heater (41), regulation heating temperature preheating, opens the liquid outlet two (35) at air intake valve two (34) and top, from air inlet
The nitrogen that two (33) of mouth are passed through enters in tank body two (30) after gas heater (41) heating, then flows from liquid outlet two (35)
Out, in the case where the nitrogen reflux of heating protects atmosphere, the residue in nanofiltration membrane is dried, after drying, consolidate
Body object；Heating jacket (40), gas heater (41) are closed, nitrogen at room reflux in tank body two (30) is passed through, is cooled down,
Close air intake valve two (34) and liquid outlet two (35)；
(4) material transfer flow: negative pressure collecting device (6) are connected in the lower end of siphunculus (20), open main valve (21) and secondary valve
Door (23), material after cooling is collected spare.
9. a kind of integrated apparatus for preparing nano zero valence iron for laboratory according to claim 7, which is characterized in that
The negative pressure collecting device (6) include negative pressure bottle body (60), setting negative pressure bottle body (60) upper end screw thread bottleneck (61), and
Switch valve one (62) on the screw thread bottleneck (61) is set, and the screw thread bottleneck (61) is connected with liquid outlet two (35).
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| CN201811313309.0A CN109433129B (en) | 2018-11-06 | 2018-11-06 | Integrated device for preparing nano zero-valent iron in laboratory and preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111230137A (en) * | 2020-01-15 | 2020-06-05 | 上海海事大学 | Integrated reaction device for preventing nano zero-valent iron from being oxidized and use method thereof |
| CN112007566A (en) * | 2020-08-27 | 2020-12-01 | 张玉梅 | Single-drive type double-cavity mutual dissolving and uniform beating device |
| CN113637866A (en) * | 2021-08-09 | 2021-11-12 | 江西蓝微电子科技有限公司 | Graphene bonded silver wire and preparation method thereof |
| CN114345122A (en) * | 2022-01-06 | 2022-04-15 | 江苏理文造纸有限公司 | Waste gas purification system and purification device thereof |
| CN115430382A (en) * | 2022-09-04 | 2022-12-06 | 美亚药业海安有限公司 | Reaction kettle for cytidine triphosphate preparation and preparation method thereof |
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| CN1054424A (en) * | 1989-12-22 | 1991-09-11 | 埃尔夫·阿奎坦国营公司 | In a unique multi-function rotating reactor, implement the method and the spendable agitator of magnetic drive, particularly spendable agitator of magnetic drive in this reactor of the solid ingredient of synthetic Ziegler-type catalytic solid or this class catalytic solid |
| CN207856903U (en) * | 2018-07-16 | 2018-09-14 | 江西顺泉生物科技有限公司 | A kind of automation equipment for pesticide producing |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1054424A (en) * | 1989-12-22 | 1991-09-11 | 埃尔夫·阿奎坦国营公司 | In a unique multi-function rotating reactor, implement the method and the spendable agitator of magnetic drive, particularly spendable agitator of magnetic drive in this reactor of the solid ingredient of synthetic Ziegler-type catalytic solid or this class catalytic solid |
| CN207856903U (en) * | 2018-07-16 | 2018-09-14 | 江西顺泉生物科技有限公司 | A kind of automation equipment for pesticide producing |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111230137A (en) * | 2020-01-15 | 2020-06-05 | 上海海事大学 | Integrated reaction device for preventing nano zero-valent iron from being oxidized and use method thereof |
| CN112007566A (en) * | 2020-08-27 | 2020-12-01 | 张玉梅 | Single-drive type double-cavity mutual dissolving and uniform beating device |
| CN113637866A (en) * | 2021-08-09 | 2021-11-12 | 江西蓝微电子科技有限公司 | Graphene bonded silver wire and preparation method thereof |
| CN113637866B (en) * | 2021-08-09 | 2022-03-04 | 江西蓝微电子科技有限公司 | Graphene bonded silver wire and preparation method thereof |
| CN114345122A (en) * | 2022-01-06 | 2022-04-15 | 江苏理文造纸有限公司 | Waste gas purification system and purification device thereof |
| CN115430382A (en) * | 2022-09-04 | 2022-12-06 | 美亚药业海安有限公司 | Reaction kettle for cytidine triphosphate preparation and preparation method thereof |
| CN115430382B (en) * | 2022-09-04 | 2023-10-03 | 美亚药业海安有限公司 | Reaction kettle for preparing cytidine triphosphate and preparation method thereof |
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| CN109433129B (en) | 2019-12-31 |
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