CN109433129B - Integrated device for preparing nano zero-valent iron in laboratory and preparation method - Google Patents
Integrated device for preparing nano zero-valent iron in laboratory and preparation method Download PDFInfo
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- CN109433129B CN109433129B CN201811313309.0A CN201811313309A CN109433129B CN 109433129 B CN109433129 B CN 109433129B CN 201811313309 A CN201811313309 A CN 201811313309A CN 109433129 B CN109433129 B CN 109433129B
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- 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
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- 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
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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
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Abstract
The invention discloses an integrated device and a preparation method for preparing nano zero-valent iron in a laboratory, wherein the integrated device comprises a reaction preparation device, a connecting device, a separation cleaning device, a heating and drying device and a fixed supporting device, the separation cleaning device is fixed at the bottom of the fixed supporting device, and the reaction preparation device is connected above the separation cleaning device through the connecting device and is used for carrying out sample preparation and separation cleaning processes; the connecting device is connected with the fixed supporting device through the turnover mechanism and used for turning over the separation cleaning device for 180 degrees, the heating and drying device is additionally arranged outside the separation cleaning device turning over for 180 degrees and used for carrying out a heating and drying process, and the separation cleaning device is connected with the negative pressure collecting device and used for carrying out a material transfer process. In a word, the invention integrates the operations of reaction, cleaning, drying and collection, and the whole process has no exposed transfer process, thereby reducing the risk of material oxidation.
Description
Technical Field
The invention belongs to the technical field of water treatment material preparation, and particularly relates to an integrated device and a preparation method for preparing nano zero-valent iron in a laboratory.
Background
In recent years, nano-scale remediation techniques have made great progress in the field of environmental science. The size of the iron particle of the nanometer part is 1-100nm, and the surface area and the surface energy of the nanometer particle are rapidly increased along with the reduction of the particle diameter, so that the nanometer particle is easier to be oxidized. Research shows that zero-valent iron material, especially nanometer level zero-valent iron material, has high reaction activity, can repair several kinds of environmental pollutant and other features, and is one active research field in environment pollution repairing technology. The nanoscale zero-valent iron can effectively degrade a plurality of organic matters such as halogenated hydrocarbon, halogenated olefin, halogenated aromatic hydrocarbon, organochlorine pesticide and the like, and can also be used for removing nitrate nitrogen in water and inorganic environmental pollutants such as heavy metal Cr (VI) in surface water.
According to the research on the preparation, separation and cleaning processes of materials such as nano zero-valent iron prepared in a laboratory, the research discovers that due to the special properties (easy oxidation) of the materials, the whole preparation, filtration, separation and drying processes need to be ensured to be in an oxygen-free environment, so that the whole preparation, separation and drying processes are inconvenient to operate.
Disclosure of Invention
Aiming at the technical problems, the invention provides an integrated device for preparing nano zero-valent iron in a laboratory.
The technical content of the invention is as follows: an integrated device for preparing nano zero-valent iron in a laboratory comprises a reaction preparation device, a connecting device, a separation cleaning device, a heating and drying device and a fixed supporting device;
the reaction preparation device comprises a tank body I, a stirring rod, a stirring motor and a separating funnel, wherein a liquid inlet I is arranged at the top of the tank body I, a liquid outlet I is arranged at the center position of the bottom of the tank body I, a gas inlet I is arranged at the lower part of the side wall of the tank body I, a gas inlet valve I is arranged on the gas inlet I, the stirring motor is arranged at the center position of the top of the tank body I, the stirring rod is positioned in the tank body I, the upper end of the stirring rod is connected with an output shaft of the stirring motor, the separating funnel is arranged on one side of the top of the tank body I;
the connecting device comprises a through pipe, a main valve and two connecting lugs, the upper end of the through pipe is in threaded connection with the first liquid outlet, the main valve is arranged on the through pipe and is close to one end of the first liquid inlet and outlet, and the two connecting lugs are symmetrically welded on the left side and the right side of the through pipe respectively;
the separation cleaning device comprises a tank body II and a filter membrane fixing ring, the tank body is divided into a cleaning part and a separating part, a liquid inlet II is arranged at the top end of the cleaning part, a gas inlet II is arranged on the upper side wall of the cleaning part, a gas inlet valve II is arranged on the gas inlet II, the liquid inlet II is in threaded connection with the lower end of a through pipe, a liquid outlet II is arranged at the bottom of the separating part, the filter membrane fixing ring is horizontally clamped at the upper end port of the separating part, a nano filter membrane is fixed in the filter membrane fixing ring, and the cleaning part is connected with the separating part through a flange;
the heating and drying device comprises a heating jacket and a gas heater, the heating jacket is detachably arranged on the outer side of the separation and cleaning device, the heating jacket is tightly attached to the outer side wall of the separation and cleaning device, the gas heater is arranged at the outer end of the gas inlet II, and the heating jacket and the gas heater are connected with an external power supply;
the fixed support device comprises a support base, a support frame and a turnover mechanism, the support base is located below the separation cleaning device, the number of the support frames is two, the support frames are fixedly connected to two sides of the upper end of the support base respectively, a mounting hole is formed in the upper end of the support frame, the mounting hole is parallel and level to the position of an attached lug connected with the connecting device, and the turnover structure is connected between the attached lug and the mounting hole and used for turning over the separation cleaning device up and down.
Further, the heating jacket is a left-right embedded assembly structure and is composed of an inner heat conduction layer, a middle heating layer and an outer heat preservation layer, the heat conduction layer is graphene foam matched with the appearance structure of the separation cleaning device, the heating layer is an electric heating belt, and the heat preservation layer is a vacuum heat preservation plate. The left and right embedded assembling structure is convenient to install and disassemble, samples in the separation and cleaning device are dried and heated in situ by the heating jacket, and the phenomenon that the air enters the transfer oven to cause oxidation and the quality of the samples is affected can be avoided.
Furthermore, the turnover mechanism comprises a first connecting plate, a second connecting plate and a locker, wherein the inner end of the first connecting plate is fixedly connected with one connecting lug through a bolt, the outer end of the first connecting plate penetrates through the mounting hole through a rotating shaft and is movably connected with the support frame on one side, the locker is arranged at the outer end of the rotating shaft and is used for limiting the movement of the turnover mechanism, the inner end of the second connecting plate is fixedly connected with the other connecting lug through a bolt, and the outer end of the second connecting plate penetrates through the mounting hole through a crank rocker and is movably connected with the support frame on the other side. The separation and cleaning device is turned over up and down by the turnover mechanism, so that the dried sample falls down by gravity in the drying process, and the collection is facilitated.
Furthermore, the locking device comprises a rotary disc and a clamping ring, wherein an adaptive threaded hole in threaded connection with the rotating shaft is formed in the center of the rotary disc, and the clamping ring is arranged at one end, close to the mounting hole, of the rotary disc. The turnover mechanism can be prevented from moving, and the stability of the whole drying and transferring process is ensured.
Furthermore, an auxiliary valve is further arranged in the through pipe and is close to the liquid inlet II. The secondary valve is closed to prevent dried sample from falling into glance sideways heated and insulated pipe to affect sample drying effect, and the primary valve is close to the collection port to prevent air from mixing in sample transfer process.
Furthermore, the first tank body and the second tank body are made of transparent glass materials, so that experimental conditions can be observed conveniently.
The invention also provides a method for preparing the nano zero-valent iron by using the integrated device, which comprises the following steps:
the sample preparation process comprises the following steps: closing the main valve and the auxiliary valve, opening the first air inlet valve and the valves on the first liquid inlet, introducing a ferrous sulfate heptahydrate solution from the first liquid inlet, introducing nitrogen gas from the first air inlet for aeration for 5min, opening the stirring motor, driving the stirring rod to fully stir the solution, adding a reducing agent through the separating funnel, controlling the dropping speed of the reducing agent to be 3 drops/s, reacting to prepare a sample after the dropping of the reducing agent is finished, closing the stirring motor, and opening the main valve and the auxiliary valve to flow the solution containing the sample into the separation cleaning device through the through pipe;
separation and cleaning process: firstly closing a valve on a liquid inlet I, opening a liquid outlet II, increasing the flow of nitrogen entering from a gas inlet I by 1 time, connecting a positive pressure filtering device at the bottom of the liquid outlet II, carrying out positive pressure filtering on the solution in a tank body II to obtain a concentrated solution, closing the liquid outlet II, opening the liquid inlet I, adding ultrapure water, wherein the volume of the ultrapure water is 5 times that of the concentrated solution, closing the gas inlet valve I, carrying out positive pressure filtering again, repeatedly cleaning with ultrapure water and absolute ethyl alcohol for 3 times alternately, cleaning with absolute ethyl alcohol for the last time, filtering to be dry by positive pressure to obtain residues on a nano filter membrane on a filter membrane fixing ring, and closing the liquid outlet II;
a heating and drying process: closing the main valve and the auxiliary valve, rotating the rotary table until the clamping ring exits from the mounting hole of the support frame, rotating the crank rocker, turning the separation cleaning device for 180 degrees under the driving of the first connecting plate and the second connecting plate, then rotationally returning the rotary table to be locked, additionally arranging a heating jacket outside the separation cleaning device, heating the second tank body, additionally arranging a gas heater on the second gas inlet, regulating and controlling the heating temperature for preheating, opening the second gas inlet valve and the second liquid outlet at the top, heating nitrogen introduced from the second gas inlet by the gas heater, then entering the second tank body, then flowing out of the second liquid outlet, drying residues on the nano filter membrane under the protection atmosphere of heated nitrogen backflow, and obtaining a solid after drying; closing the heating jacket and the gas heater, introducing normal-temperature nitrogen to flow back in the second tank body, cooling, and closing the second air inlet valve and the second liquid outlet;
material transfer process: and the lower end of the through pipe is connected with a negative pressure collecting device, and the main valve and the auxiliary valve are opened to collect the cooled materials for later use.
Furthermore, the negative pressure collecting device comprises a negative pressure bottle body, a threaded bottle opening arranged at the upper end of the negative pressure bottle body, and a first switch valve arranged on the threaded bottle opening, wherein after the threaded bottle opening is connected with a second liquid outlet, the first switch valve is opened, and after the collection is finished, the first switch valve is closed, so that air cannot be mixed in the negative pressure bottle body, and the sample material is prevented from being oxidized.
Furthermore, the inside of the negative pressure bottle body is also provided with an intercepting filter membrane, the bottom of the side wall of the negative pressure bottle body is provided with a connector, the connector is provided with a second switch valve, and the connector is connected with a negative pressure generator through an exhaust pipe. The capacity of the negative pressure bottle body is limited, the negative pressure is small in the process of collecting sample materials by utilizing the negative pressure, the problems of low collecting efficiency and the like easily exist, the negative pressure generator can form large negative pressure outside the negative pressure bottle body, and the problems can be effectively solved.
It should be noted that the integrated device of the present invention can also be used for preparing other easily oxidized materials, such as nano zinc powder, bio-carbon loaded nano zero-valent iron, mineral loaded nano zero-valent iron, and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. the integrated detachable design is convenient for operation and cleaning;
2. the organic transparent glass material is beneficial to observing the whole experimental process;
3. the whole preparation, separation, cleaning and drying processes are finished under the protection of nitrogen, and no transfer process is arranged in the middle, so that the risk of material oxidation in the whole process is reduced;
4. the cleaning process uses nitrogen positive pressure filtration, and the whole cleaning process can be regulated and controlled by adjusting the nitrogen flow while the material is protected. The efficiency of the whole cleaning is greatly enhanced by 18-90 times. The loss rate after the whole separation and cleaning is far lower than that of the traditional separation and cleaning mode;
5. the processes of cleaning, drying and collecting do not have an exposed transfer process, so that the risk of material oxidation is reduced.
Drawings
FIG. 1 is a block diagram of a sample preparation and separation cleaning process of the present invention;
FIG. 2 is a structural diagram of a heating, drying and material transfer process in example 1 of the present invention;
fig. 3 is a structural diagram of a heating drying and material transfer process in embodiment 2 of the present invention.
Wherein, 1-reaction preparation device, 10-tank body I, 11-stirring rod, 12-stirring motor, 13-separating funnel, 14-liquid inlet I, 15-liquid outlet I, 16-gas inlet I, 17-gas inlet valve I, 2-connecting device, 20-communicating pipe, 21-main valve, 22-connecting lug, 23-auxiliary valve, 3-separation cleaning device, 30-tank body II, 31-filter membrane fixing ring, 32-liquid inlet II, 33-gas inlet II, 34-gas inlet valve II, 35-liquid outlet II, 36-flange, 4-heating drying device, 40-heating jacket, 41-gas heater, 5-fixing supporting device, 50-supporting base, 51-supporting frame, and, 510-mounting hole, 52-turnover mechanism, 520-connecting plate I, 521-connecting plate II, 522-locking device, 523-rotating shaft, 524-crank rocker, 525-rotating disc, 526-clamping ring, 6-negative pressure collecting device, 60-negative pressure bottle body, 61-threaded bottle mouth, 62-switching valve I, 63-connecting port, 64-switching valve II, 65-intercepting filter membrane and 66-negative pressure generator.
Detailed Description
The invention will be further explained below with reference to specific embodiments and the accompanying figures 1-3.
Example 1
As shown in fig. 1, an integrated device for preparing nano zero-valent iron in a laboratory comprises a reaction preparation device 1, a connecting device 2, a separation cleaning device 3, a heating and drying device 4 and a fixed support device 5; the reaction preparation device 1 comprises a tank body I10, a stirring rod 11, a stirring motor 12 and a separating funnel 13, wherein a liquid inlet I14 is arranged at the top of the tank body I10, a liquid outlet I15 is arranged at the center position of the bottom of the tank body I10, a gas inlet I16 is arranged at the lower part of the side wall of the tank body I10, a gas inlet valve I17 is arranged on the gas inlet I16, the stirring motor 12 is arranged at the center position of the top of the tank body I10, the stirring rod 11 is positioned in the tank body I10, the upper end of the stirring rod 11 is connected with an output shaft of the stirring motor 12, the separating funnel 13 is arranged on one side of the top of;
as shown in fig. 1, the connecting device 2 includes a through pipe 20, a main valve 21 and two connecting lugs 22, the upper end of the through pipe 20 is connected with the first liquid outlet 15 through threads, the main valve 21 is arranged on the through pipe 20 and close to one end of the first liquid inlet/outlet 15, and the two connecting lugs 22 are respectively and symmetrically welded on the left side and the right side of the through pipe 20; as shown in fig. 1-3, an auxiliary valve 23 is further disposed in the through pipe 20, and the auxiliary valve 23 is close to the second liquid inlet 32. The secondary valve 23 is closed to prevent the dried sample from falling glance sideways into the heated and insulated tube 20, which affects the drying effect of the sample, while the primary valve 21 is closed to prevent air from being mixed in during the sample transfer process.
As shown in fig. 1, the separation cleaning device 3 comprises a tank body two 30 and a filter membrane fixing ring 31, the tank body two 30 is divided into a cleaning part and a separating part, a liquid inlet two 32 is arranged at the top end of the cleaning part, an air inlet two 33 is arranged on the upper side wall of the cleaning part, an air inlet valve two 34 is arranged on the air inlet two 33, the liquid inlet two 32 is in threaded connection with the lower end of the through pipe 20, a liquid outlet two 35 is arranged at the bottom of the separating part, the filter membrane fixing ring 31 is horizontally clamped at the upper end opening of the separating part, a nano filter membrane is fixed in the filter membrane fixing ring 31, and the cleaning part and the; the first tank body 10 and the second tank body 30 are made of transparent glass materials, so that experimental conditions can be observed conveniently.
As shown in fig. 2 and 3, the heating and drying device 4 comprises a heating jacket 40 and a gas heater 41, the heating jacket 40 is detachably arranged outside the separation and cleaning device 3, the heating jacket 40 is tightly attached to the outer side wall of the separation and cleaning device 3, the gas heater 41 is arranged at the outer end of the gas inlet two 33, and the heating jacket 40 and the gas heater 41 are connected with an external power supply; wherein, heating jacket 40 is for controlling the gomphosis structure of assembling, comprises the heat-conducting layer of inboard, the zone of heating at middle part and the heat preservation in the outside, and the heat-conducting layer is the graphite alkene foam that is identical with separation belt cleaning device 3 appearance structure, and the zone of heating is the electrical heating area, and the heat preservation is vacuum insulation board. The left and right embedded assembling structure is convenient to install and disassemble, samples in the separation and cleaning device 3 are dried and heated in situ by the heating jacket 40, and the phenomenon that the air enters the transfer oven to cause oxidation and influence the quality of the samples can be avoided.
As shown in fig. 1, the fixed supporting device 5 includes a supporting base 50, two supporting frames 51 and a turning mechanism 52, the supporting base 50 is located below the separation cleaning device 3, the two supporting frames 51 are respectively and fixedly connected to two sides of the upper end of the supporting base 50, the upper end of the supporting frame 51 is provided with a mounting hole 510, the mounting hole 510 is flush with the connecting attachment lug 22 of the connecting device 2, and the turning mechanism 52 is connected between the connecting attachment lug 22 and the mounting hole 510 and is used for turning the separation cleaning device 3 up and down. The turnover mechanism 52 comprises a first connecting plate 520, a second connecting plate 521 and a locking device 522, the inner end of the first connecting plate 520 is fixedly connected with one connecting lug 22 through a bolt, the outer end of the first connecting plate 520 penetrates through the mounting hole 510 through a rotating shaft 523 and is movably connected with the supporting frame 51 on one side, the locking device 522 is arranged at the outer end of the rotating shaft 523 and is used for limiting the movement of the turnover mechanism 52, the inner end of the second connecting plate 521 is fixedly connected with the other connecting lug 22 through a bolt, and the outer end of the second connecting plate 521 penetrates through the mounting hole 510 through a crank rocker 524 and is movably connected with the supporting frame 51. The separation and cleaning device 3 is turned upside down by the turning mechanism 52, so that the dried sample falls down by gravity in the drying process, and is convenient to collect. As shown in fig. 1, the locking device 522 includes a rotary plate 525 and a collar 526, the rotary plate 525 is provided with a screw hole at a center thereof to be screwed with the rotary shaft 523, and the collar 526 is provided at an end of the rotary plate 525 adjacent to the mounting hole 510. The turnover mechanism 52 can be prevented from moving, and the stability of the whole drying and transferring process is ensured.
The method for preparing the nano zero-valent iron by utilizing the integrated device comprises the following steps:
1 sample preparation procedure: closing the main valve 21 and the auxiliary valve 23, opening the air inlet valve 17 and the valves on the liquid inlet 14, introducing a ferrous sulfate heptahydrate solution from the liquid inlet 14, introducing nitrogen gas from the air inlet 16 for aeration for 5min, opening the stirring motor 12, driving the stirring rod 11 to fully stir the solution, adding a reducing agent through the separating funnel 13, controlling the dropping speed of the reducing agent to be 3 drops/s, reacting to prepare a sample after the dropping of the reducing agent is finished, closing the stirring motor 12, opening the main valve 21 and the auxiliary valve 23, and allowing the solution containing the sample to flow into the separation cleaning device 3 through the through pipe 20;
2, separation and cleaning process: firstly closing a valve on a first liquid inlet 14, opening a second liquid outlet 35, increasing the flow of nitrogen entering from a first air inlet 16 by 1 time, connecting a positive pressure filtering device at the bottom of the second liquid outlet 35, carrying out positive pressure filtering on the solution in a second tank body 30 to obtain a concentrated solution, closing the second liquid outlet 35, opening the first liquid inlet 14 again, adding ultrapure water, wherein the volume of the ultrapure water is 5 times that of the concentrated solution, closing a first air inlet valve 17, carrying out positive pressure filtering again, repeatedly cleaning with the ultrapure water and absolute ethyl alcohol for 3 times alternately, cleaning with the absolute ethyl alcohol for the last time, filtering at positive pressure till the liquid is dry to obtain residues on a nanofiltration membrane on a filter membrane fixing ring 31, and closing the second liquid outlet 35;
3, heating and drying process: closing the main valve 21 and the auxiliary valve 23, rotating the rotary disc 525 until the clamping ring 526 exits from the mounting hole 510 of the support frame 51, rotating the crank rocker 524, turning the separation cleaning device 3 for 180 degrees under the drive of the first connecting plate 520 and the second connecting plate 521, then rotationally returning the rotary disc 525 to the original position for locking, additionally installing a heating jacket 40 outside the separation cleaning device 3 to heat the second tank body 30, additionally installing a gas heater 41 on the second gas inlet 33, regulating and controlling the heating temperature for preheating, opening the second gas inlet valve 34 and the second liquid outlet 35 at the top, introducing nitrogen from the second gas inlet 33, heating by the gas heater 41, entering the second tank body 30, then flowing out of the second liquid outlet 35, drying residues on the nanofiltration membrane under the protection atmosphere of heated nitrogen backflow, and obtaining solids after drying; closing the heating jacket 40 and the gas heater 41, introducing normal-temperature nitrogen to flow back in the second tank body 30 for cooling, and closing the second inlet valve 34 and the second liquid outlet 35;
4, material transfer process: the lower end of the through pipe 20 is connected to a negative pressure collecting device 6, and the main valve 21 and the sub-valve 23 are opened to collect the cooled material for standby. As shown in fig. 2, the negative pressure collecting device 6 includes a negative pressure bottle body 60, a screw thread opening 61 disposed at the upper end of the negative pressure bottle body 60, and a first switch valve 62 disposed on the screw thread opening 61, wherein after the screw thread opening 61 is connected to the second liquid outlet 35, the first switch valve 62 is opened, and after the collection is completed, the first switch valve 62 is closed, so as to ensure that air is not mixed into the negative pressure bottle body 60, and prevent the sample material from being oxidized.
Furthermore, the interior of the negative pressure bottle 60 is also provided with an interception filter membrane 65, the bottom of the side wall of the negative pressure bottle 60 is provided with a connecting port 63, the connecting port 63 is provided with a second switch valve 64, and the connecting port 63 is connected with a negative pressure generator 66 through an exhaust pipe. The negative pressure bottle 60 has a limited capacity, so that the problems of low negative pressure, low collection efficiency and the like are easily caused in the process of collecting sample materials by using negative pressure, and the problem can be effectively solved by adding the negative pressure generator 66 outside the negative pressure bottle 60 to form larger negative pressure.
Example 2
The invention is essentially the same as example 1, except that:
the method for preparing the nano zero-valent iron by utilizing the integrated device comprises the following steps:
1 sample preparation procedure: closing the main valve 21 and the auxiliary valve 23, opening the air inlet valve 17 and the valves on the liquid inlet 14, introducing a ferrous sulfate heptahydrate solution from the liquid inlet 14, introducing nitrogen gas from the air inlet 16 for aeration for 5min, opening the stirring motor 12, driving the stirring rod 11 to fully stir the solution, adding a reducing agent through the separating funnel 13, controlling the dropping speed of the reducing agent to be 3 drops/s, reacting to prepare a sample after the dropping of the reducing agent is finished, closing the stirring motor 12, opening the main valve 21 and the auxiliary valve 23, and allowing the solution containing the sample to flow into the separation cleaning device 3 through the through pipe 20;
2, separation and cleaning process: firstly closing a valve on a first liquid inlet 14, opening a second liquid outlet 35, increasing the flow of nitrogen entering from a first air inlet 16 by 1 time, connecting a positive pressure filtering device at the bottom of the second liquid outlet 35, carrying out positive pressure filtering on the solution in a second tank body 30 to obtain a concentrated solution, closing the second liquid outlet 35, opening the first liquid inlet 14 again, adding ultrapure water, wherein the volume of the ultrapure water is 5 times that of the concentrated solution, closing a first air inlet valve 17, carrying out positive pressure filtering again, repeatedly cleaning with the ultrapure water and absolute ethyl alcohol for 3 times alternately, cleaning with the absolute ethyl alcohol for the last time, filtering at positive pressure till the liquid is dry to obtain residues on a nanofiltration membrane on a filter membrane fixing ring 31, and closing the second liquid outlet 35;
3, heating and drying process: closing the main valve 21 and the auxiliary valve 23, rotating the rotary disc 525 until the clamping ring 526 exits from the mounting hole 510 of the support frame 51, rotating the crank rocker 524, turning the separation cleaning device 3 for 180 degrees under the drive of the first connecting plate 520 and the second connecting plate 521, then rotationally returning the rotary disc 525 to the original position for locking, additionally installing a heating jacket 40 outside the separation cleaning device 3 to heat the second tank body 30, additionally installing a gas heater 41 on the second gas inlet 33, regulating and controlling the heating temperature for preheating, opening the second gas inlet valve 34 and the second liquid outlet 35 at the top, introducing nitrogen from the second gas inlet 33, heating by the gas heater 41, entering the second tank body 30, then flowing out of the second liquid outlet 35, drying residues on the nanofiltration membrane under the protection atmosphere of heated nitrogen backflow, and obtaining solids after drying; closing the heating jacket 40 and the gas heater 41, introducing normal-temperature nitrogen to flow back in the second tank body 30 for cooling, and closing the second inlet valve 34 and the second liquid outlet 35;
4, material transfer process: the lower end of the through pipe 20 is connected to a negative pressure collecting device 6, and the main valve 21 and the sub-valve 23 are opened to collect the cooled material for standby. As shown in fig. 2, the negative pressure collecting device 6 includes a negative pressure bottle body 60, a screw bottle mouth 61 disposed at the upper end of the negative pressure bottle body 60, a first switch valve 62 disposed on the screw bottle mouth 61, an internal hiccup intercepting filter membrane 65 of the negative pressure bottle body 60, a connection port 63 at the bottom of the side wall of the negative pressure bottle body 60, a second switch valve 64 disposed on the connection port 63, and a negative pressure generator 66 connected to the connection port 63 through an air suction pipe. And after the threaded bottle mouth 61 is connected with the second liquid outlet 35, the negative pressure generator 66 is used for performing negative pressure suction on the negative pressure bottle body 60, collecting the dried sample material in the second tank body 30 into the negative pressure bottle body 60, and closing the first switch valve 62 and the second switch valve 64. Because the capacity of the negative pressure bottle body 60 is limited, the negative pressure is small in the process of collecting the sample material by using the negative pressure, the problem of low collecting efficiency is easy to exist, and the negative pressure generator 66 additionally arranged on the negative pressure bottle body 60 can form larger negative pressure, so that the problems can be effectively solved.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. An integrated device for preparing nano zero-valent iron in a laboratory is characterized by comprising a reaction preparation device (1), a connecting device (2), a separation cleaning device (3), a heating and drying device (4) and a fixed supporting device (5);
the reaction preparation device (1) comprises a tank body I (10), a stirring rod (11), a stirring motor (12) and a separating funnel (13), wherein a liquid inlet I (14) is arranged at the top of the tank body I (10), a liquid outlet I (15) is arranged at the center of the bottom of the tank body I (10), a gas inlet I (16) is arranged at the lower part of the side wall of the tank body I (10), a gas inlet valve I (17) is arranged on the gas inlet I (16), the stirring motor (12) is arranged at the center of the top of the tank body I (10), the stirring rod (11) is positioned inside the tank body I (10), the upper end of the stirring rod (11) is connected with an output shaft of the stirring motor (12), the separating funnel (13) is arranged on one side of the top of the tank body I (10), and the lower end of the;
the connecting device (2) comprises a through pipe (20), a main valve (21) and connecting attachment lugs (22), the upper end of the through pipe (20) is connected with the first liquid outlet (15) through threads, the main valve (21) is arranged on the through pipe (20) and close to one end of the first liquid inlet and outlet (15), and the connecting attachment lugs (22) are two in number and are symmetrically welded on the left side and the right side of the through pipe (20) respectively;
the separation cleaning device (3) comprises a tank body II (30) and a filter membrane fixing ring (31), the tank body II (30) is divided into a cleaning part and a separation part, a liquid inlet II (32) is arranged at the top end of the cleaning part, a gas inlet II (33) is arranged on the upper side wall of the cleaning part, a gas inlet valve II (34) is arranged on the gas inlet II (33), the liquid inlet II (32) is in threaded connection with the lower end of the through pipe (20), a liquid outlet II (35) is arranged at the bottom of the separation part, the filter membrane fixing ring (31) is horizontally clamped at the upper port of the separation part, a nano filter membrane is fixed in the filter membrane fixing ring (31), and the cleaning part is connected with the separation part through a flange (36);
the heating and drying device (4) comprises a heating jacket (40) and a gas heater (41), the heating jacket (40) is detachably arranged on the outer side of the separation and cleaning device (3), the heating jacket (40) is tightly attached to the outer side wall of the separation and cleaning device (3), the gas heater (41) is arranged at the outer end of the gas inlet II (33), and the heating jacket (40) and the gas heater (41) are connected with an external power supply; the heating jacket (40) is of a left-right embedded assembly structure and comprises an inner heat conduction layer, a middle heating layer and an outer heat insulation layer, the heat conduction layer is made of graphene foam matched with the appearance structure of the separation cleaning device (3), the heating layer is an electric heating belt, and the heat insulation layer is a vacuum heat insulation plate;
the fixed supporting device (5) comprises supporting bases (50), supporting frames (51) and a turnover mechanism (52), the supporting bases (50) are located below the separation cleaning devices (3), the number of the supporting frames (51) is two, the two supporting frames are respectively and fixedly connected to two sides of the upper end of the supporting bases (50), mounting holes (510) are formed in the upper ends of the supporting frames (51), the mounting holes (510) are flush with the connecting lugs (22) of the connecting device (2), and the turnover structure (52) is connected between the connecting lugs (22) and the mounting holes (510) and used for turning the separation cleaning devices (3) up and down;
the turnover mechanism (52) comprises a first connecting plate (520), a second connecting plate (521) and a locking device (522), wherein the inner end of the first connecting plate (520) is fixedly connected with one connecting lug (22) through a bolt, the outer end of the first connecting plate (520) penetrates through the mounting hole (510) through a rotating shaft (523) and is movably connected with the supporting frame (51) on one side, the locking device (522) is arranged on the outer end of the rotating shaft (523) and is used for limiting the movement of the turnover mechanism (52), the inner end of the second connecting plate (521) is fixedly connected with the other connecting lug (22) through a bolt, and the outer end of the second connecting plate (521) penetrates through the mounting hole (510) through a crank rocker (524) and is movably connected with the supporting frame (51) on the other side.
2. The integrated device for preparing nano zero-valent iron in a laboratory according to claim 1, wherein the locker (522) comprises a rotary disc (525) and a clamping ring (526), the rotary disc (525) is provided with a matching threaded hole in a central position for being in threaded connection with the rotating shaft (523), and the clamping ring (526) is arranged at one end of the rotary disc (525) close to the mounting hole (510).
3. The integrated device for preparing nano zero-valent iron in a laboratory according to claim 1, wherein an auxiliary valve (23) is further arranged in the through pipe (20), and the auxiliary valve (23) is close to the liquid inlet II (32).
4. The integrated device for preparing nano zero-valent iron in a laboratory according to claim 1, wherein the first tank body (10) and the second tank body (30) are both made of transparent glass.
5. The method for preparing nano zero-valent iron by using the integrated device of any one of claims 1 to 4, which is characterized by comprising the following steps:
the sample preparation process comprises the following steps: closing the main valve (21) and the auxiliary valve (23), opening the air inlet valve I (17) and valves on the liquid inlet I (14), introducing a ferrous sulfate heptahydrate solution from the liquid inlet I (14), introducing nitrogen from the air inlet I (16) for aeration for 5min, opening the stirring motor (12), driving the stirring rod (11) to fully stir the solution, adding a reducing agent through the separating funnel (13), controlling the dropping speed of the reducing agent to be 3 drops/s, reacting to prepare a sample, closing the stirring motor (12), opening the main valve (21) and the auxiliary valve (23), and allowing the solution containing the sample to flow into the separation cleaning device (3) through the through pipe (20);
separation and cleaning process: firstly closing a valve on a liquid inlet I (14), opening a liquid outlet II (35), increasing the flow of nitrogen entering from a gas inlet I (16) by 1 time, connecting a positive pressure filtering device at the bottom of the liquid outlet II (35), carrying out positive pressure filtering on the solution in a tank body II (30) to obtain a concentrated solution, closing the liquid outlet II (35), opening the liquid inlet I (14) again, adding ultrapure water, wherein the volume of the ultrapure water is 5 times that of the concentrated solution, closing a gas inlet valve I (17), carrying out positive pressure filtering again, repeatedly washing with the ultrapure water and absolute ethyl alcohol for 3 times alternately, washing with the absolute ethyl alcohol for the last time, filtering to be dry by positive pressure to obtain residues on a nanofiltration membrane on a filtration membrane fixing ring (31), and closing the liquid outlet II (35);
a heating and drying process: closing the main valve (21) and the auxiliary valve (23), rotating the rotary disc (525) to the collar (526) to exit from the mounting hole (510) of the support frame (51), rotating the crank rocker (524), turning the separation cleaning device (3) for 180 degrees under the drive of the connecting plate I (520) and the connecting plate II (521), then rotating and returning the rotary disc (525) to the original position for locking, adding a heating jacket (40) outside the separation cleaning device (3) to heat the tank body II (30), adding a gas heater (41) on the gas inlet II (33), regulating and controlling the heating temperature for preheating, opening the gas inlet valve II (34) and the liquid outlet II (35) at the top, heating nitrogen introduced from the gas inlet II (33) by the gas heater (41) and then entering the tank body II (30), then flowing out from the liquid outlet II (35), and under the protection atmosphere of heated nitrogen backflow, drying the residues on the nanofiltration membrane to obtain solid substances after drying; closing the heating jacket (40) and the gas heater (41), introducing normal-temperature nitrogen to flow back in the second tank body (30), cooling, and closing the second air inlet valve (34) and the second liquid outlet (35);
material transfer process: the lower end of the through pipe (20) is connected with a negative pressure collecting device (6), a main valve (21) and an auxiliary valve (23) are opened, and cooled materials are collected for standby;
the negative pressure collecting device (6) comprises a negative pressure bottle body (60), a thread bottle opening (61) arranged at the upper end of the negative pressure bottle body (60), and a first switch valve (62) arranged on the thread bottle opening (61), wherein the thread bottle opening (61) is connected with a second liquid outlet (35).
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| CN112007566A (en) * | 2020-08-27 | 2020-12-01 | 张玉梅 | Single-drive type double-cavity mutual dissolving and uniform beating device |
| 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 |
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| 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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