CN110156090B - For preparing Fe3O4Fluid synthesis preparation device of magnetic nanoparticles and control method thereof - Google Patents
For preparing Fe3O4Fluid synthesis preparation device of magnetic nanoparticles and control method thereof Download PDFInfo
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- CN110156090B CN110156090B CN201910573580.6A CN201910573580A CN110156090B CN 110156090 B CN110156090 B CN 110156090B CN 201910573580 A CN201910573580 A CN 201910573580A CN 110156090 B CN110156090 B CN 110156090B
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- 239000002122 magnetic nanoparticle Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 119
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 43
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 19
- 239000012530 fluid Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 230000002572 peristaltic effect Effects 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000010425 asbestos Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 229910052895 riebeckite Inorganic materials 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 10
- 239000002699 waste material Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 5
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 4
- 229940038773 trisodium citrate Drugs 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001311 chemical methods and process Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 238000003759 clinical diagnosis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 229940032296 ferric chloride Drugs 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
Hair brushRelates to a method for preparing Fe3O4Compared with the prior art, the fluid synthesis preparation device of the magnetic nano-particles and the control method thereof solve the problem that Fe can not be prepared3O4Defects in magnetic nanoparticle devices. The invention comprises a first micro-reaction cavity component and a second micro-reaction cavity component, wherein the first micro-reaction cavity component comprises a first micro-reaction cavity, the upper end of the first micro-reaction cavity is connected with an ethylene glycol supply pipe, the bottom of the first micro-reaction cavity is funnel-shaped, the first micro-reaction cavity is placed on a magnetic stirrer, a sieve plate is arranged in the first micro-reaction cavity, magnetons are placed on the sieve plate, the head end of a silicone tube is connected to the bottom of the first micro-reaction cavity, and the tail end of the silicone tube is connected to the upper end of the second micro-reaction cavity component. The invention provides a method for synthesizing Fe3O4The preparation device of the magnetic nano particles can realize Fe by matching with a fluid control method based on a pump valve3O4Automated preparation of magnetic nanoparticles.
Description
Technical Field
The invention relates to the technical field of chemical preparation devices, in particular to a device for preparing Fe3O4A fluid synthesis preparation device of magnetic nanoparticles and a control method thereof.
Background
Fe3O4The magnetic nano-particles are common superparamagnetic nano-materials, have the characteristics of magnetic guidance and nano-materials, and have the advantages of simple preparation, low toxicity, good biocompatibility and the like, so the magnetic nano-particles are widely applied to the fields of clinical diagnosis, contrast imaging, targeted drugs, biomarkers, separation and the like.
To obtain monodisperse, uniform-sized Fe3O4Nanoparticles, generally hydrothermal, i.e.: adding reagent such as trisodium citrate and anhydrous sodium acetate into ferric chloride dissolved in ethylene glycol in sequence, and stirring for half an hour to fully dissolve; and transferring the mixture into a reaction kettle, placing the reaction kettle in an oven to react for 10 hours at the temperature of 200 ℃, and cooling the reaction kettle to room temperature to obtain a black product. Manually placing the magnet at the bottom of a beaker, collecting the product, sequentially washing with deionized water and ethanol, and finally placing the product in a vacuum drying oven at 60 ℃ for drying for 6 hours to obtain the product.
Therefore, the traditional artificial chemical method has the defects of complicated preparation and cleaning process, large reagent consumption amount, long period, and inconvenience in batch synthesis and use due to the fact that the synthesis of the nano particles with uniform sizes depends on the experience of operators.
At the same time, it would be obvious to one skilled in the chemical arts to develop a set of methods for producing Fe3O4The hardware of the magnetic nano-particle synthesizing device can provide a control method based on a chemical process flow on the basis of the hardware so as to realize Fe3O4Automated non-artificial synthesis preparation processing of magnetic nanoparticles.
Therefore, how to incorporate Fe3O4The magnetic nano-particle chemical synthesis technology is realized in automatic processing equipment, and a set of Fe is developed3O4The preparation device of magnetic nanoparticles has become a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the problem that Fe can not be prepared in the prior art3O4A magnetic nanoparticle device, a method for making the samePreparation of Fe3O4The fluid synthesis preparation device of magnetic nanoparticles and the control method thereof solve the problems.
In order to achieve the purpose, the technical scheme of the invention is as follows:
for preparing Fe3O4The fluid synthesis preparation device of the magnetic nanoparticles comprises a first micro-reaction cavity component and a second micro-reaction cavity component, wherein the first micro-reaction cavity component comprises a first micro-reaction cavity, the upper end of the first micro-reaction cavity is connected with an ethylene glycol supply pipe, the bottom of the first micro-reaction cavity is funnel-shaped, the first micro-reaction cavity is placed on a magnetic stirrer, a sieve plate is arranged in the first micro-reaction cavity, magnetons are placed on the sieve plate, the head end of a silica gel tube is connected to the bottom of the first micro-reaction cavity, and the tail end of the silica gel tube is connected to the upper end of the second micro-reaction cavity component;
the second micro-reaction cavity assembly comprises a second micro-reaction cavity and a magnet rotating assembly, the bottom of the second micro-reaction cavity is positioned above the radius of a magnet rotating track of the magnet rotating assembly, the bottom of the second micro-reaction cavity is funnel-shaped, a resistance heating wire is wound on the outer wall of the second micro-reaction cavity, a heat insulation asbestos sleeve is wrapped outside the second micro-reaction cavity, and a thermocouple is inserted into the heat insulation asbestos sleeve and is sleeved on the resistance heating wire;
the tail end of the silicone tube is also connected with a deionized water delivery pipe and an ethanol delivery pipe, the tail end of the silicone tube passes through a heat-insulating asbestos sleeve of the second micro-reaction cavity component to be inserted at the upper end of the second micro-reaction cavity, and Fe3O4The head end of the magnetic nano particle conveying pipe penetrates through a heat insulation asbestos sleeve of the second micro reaction cavity assembly to be connected to the bottom of the second micro reaction cavity.
The ethylene glycol supply pipe is provided with a first peristaltic pump and a first pinch valve, the silicone tube is provided with a second pinch valve, the deionized water conveying pipe is provided with a second peristaltic pump, the ethanol conveying pipe is provided with a third peristaltic pump, and the Fe conveying pipe is provided with a third peristaltic pump3O4A third pinch valve is arranged on the magnetic nano particle conveying pipe, and Fe3O4The magnetic nano particle conveying pipe is positioned between the third pinch valve and the second micro-reaction cavityIs connected with a self-control drain pipe.
Magnet rotating assembly include automatically controlled rotary rod, fixed mounting has anchor clamps on the automatically controlled rotary rod, accompanies magnet on the anchor clamps, the rotation orbit radius top that the bottom of second micro-reaction cavity is located magnet.
The temperature controller is characterized by further comprising a temperature controller, wherein one end of the temperature controller is connected to the thermocouple, and the other end of the temperature controller is connected to the resistance heating wire.
The device comprises a main control chip, and control signal input ends of a first peristaltic pump, a first pinch valve, a magnetic stirrer, a second pinch valve, a second peristaltic pump, a third peristaltic pump, a temperature controller, an electric control rotating rod, a third pinch valve and an automatic control drain pipe are respectively connected with a control signal output end of the main control chip.
For preparing Fe3O4The control method of the fluid synthesis preparation device of the magnetic nanoparticles comprises the following steps:
after three powder samples of ferric chloride hexahydrate, trisodium citrate and anhydrous sodium acetate are placed into the cavity of the first micro-reaction cavity, the main control chip starts the first peristaltic pump and opens the first pinch valve, and ethylene glycol is injected into the cavity of the first micro-reaction cavity through the ethylene glycol supply pipe;
the main control chip starts a magnetic stirrer, and magnetons in the first micro-reaction cavity are used for stirring the reaction solution;
after the main control chip controls the magnetic stirrer to work for half an hour continuously, the main control chip closes the magnetic stirrer;
the main control chip opens the second pinch valve and sends the liquid which is completely reacted in the silica gel tube into the second micro-reaction cavity;
the main control chip controls the temperature controller to heat the resistance heating wire, so that the resistance heating wire is heated to 200 ℃ and lasts for 10 hours;
the main control chip controls the temperature controller to close the resistance heating wire, and the natural cooling is completed after waiting for two hours;
the main control chip controls an electric control rotating rod of the magnet rotating assembly, and the magnet is rotatably placed below the second micro-reaction cavity;
the main control chip closes the third pinch valve, opens the automatic control drain pipe, and discharges the waste liquid in the second micro-reaction cavity through the automatic control drain pipe;
the main control chip closes the self-control water discharge pipe, controls the electric control rotary rod to drive the magnet to reset, and moves out of the lower part of the second micro-reaction cavity;
and (3) deionized water cleaning: the main control chip opens a second peristaltic pump and leads in deionized water through a deionized water conveying pipe; then the magnet is driven by the electric control rotating rod to move to the lower part of the second micro-reaction cavity, the main control chip opens the automatic control drain pipe, and the deionized water waste liquid is discharged; carrying out multiple deionized water cleaning steps;
ethanol cleaning: the main control chip controls the electric control rotating rod to drive the magnet to reset, moves out of the lower part of the second micro-reaction cavity, controls to start a third peristaltic pump, and leads in ethanol through an ethanol conveying pipe; then the magnet is driven by the electric control rotating rod to move to the lower part of the second micro-reaction cavity, the main control chip opens the automatic control drain pipe, and the ethanol waste liquid is discharged; carrying out ethanol cleaning for multiple times; ,
finally, the main control chip controls to open a third pinch valve to enable Fe3O4And discharging the magnetic nanoparticles.
Advantageous effects
The invention relates to a method for preparing Fe3O4Compared with the prior art, the fluid synthesis preparation device of the magnetic nano particles and the control method thereof provide the device capable of synthesizing Fe3O4The preparation device of the magnetic nano-particles can realize Fe by matching with the traditional control method based on the chemical process3O4The automatic preparation of the magnetic nanoparticles reduces the manual participation process, avoids the disturbance of manual operation, and has the characteristics of simple and convenient operation, simple structure, low cost and batch synthesis.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of the circuit connection of the main control chip according to the present invention;
wherein, 1-the first micro-reaction chamber, 2-ethylene glycol supply pipe, 3-magnetic stirrer, 4-sieve plate, 5-magneton, 6-A silicone tube, 7-a second micro-reaction cavity, 8-a resistance heating wire, 9-a heat insulation asbestos jacket, 10-a magnet rotating component, 11-a thermocouple, 12-a deionized water conveying pipe, 13-an ethanol conveying pipe, 14-a first peristaltic pump, 15-a first pinch valve, 16-a second pinch valve, 17-a second peristaltic pump, 18-a third peristaltic pump, 19-a third pinch valve, 20-an electric control rotating rod, 21-a clamp, 22-a magnet, 23-a temperature controller and 24-Fe3O4Magnetic nano-particle delivery pipe, 25-main control chip.
Detailed Description
So that the manner in which the above recited features of the present invention can be understood and readily understood, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings, wherein:
to cooperate with Fe3O4As shown in FIG. 1, the chemical preparation method (control method) of magnetic nanoparticles comprises a first micro-reaction chamber assembly and a second micro-reaction chamber assembly, wherein the first micro-reaction chamber assembly comprises a first micro-reaction chamber 1, and the first micro-reaction chamber 1 is used for simulating Fe3O4Adding a reagent in the preparation process of the magnetic nano-particles and magnetically stirring and dissolving.
The upper end of the first micro-reaction chamber 1 is connected with a glycol supply pipe 2, and a first peristaltic pump 14 and a first pinch valve 15 can be additionally arranged on the glycol supply pipe 2 according to the traditional technology so as to provide glycol. The bottom of the first micro reaction chamber 1 is funnel-shaped to facilitate the collection of the put powder sample. The first micro-reaction chamber 1 is placed on a magnetic stirrer 3 to achieve a magnetic stirring effect. A sieve plate 4 is arranged in the first micro-reaction chamber 1, and a magneton 5 is placed on the sieve plate 4 to be matched with magnetic stirring for use. The head end of the silicone tube 6 is connected to the bottom of the first micro-reaction cavity 1, and the tail end of the silicone tube 6 is connected to the upper end of the second micro-reaction cavity component, so that the first micro-reaction cavity 1 is transmitted to the second micro-reaction cavity 7.
The second micro-reaction cavity component is used for simulating and realizing processing links such as heating of the polytetrafluoroethylene reaction kettle, and comprises a second micro-reaction cavity 7 and a magnet rotating component 10.
The magnet rotating assembly 10 is used to implement an external magnet function to facilitate product collection. Magnet rotating assembly 10 includes automatically controlled rotary rod 20, and fixed mounting has anchor clamps 21 on the automatically controlled rotary rod 20, and anchor clamps 21 can rotate under the drive of automatically controlled rotary rod 20, accompany magnet 22 on the anchor clamps 21 to make magnet 22 rotate according to the rotation of automatically controlled rotary rod 20. The bottom of the second micro-reaction cavity 7 is located above the radius of the rotating track of the magnet 22, the magnet rotating assembly 10 is installed on the related equipment platform in a traditional way, and when the product collection is needed by means of magnetism, the magnet 22 can rotate to the bottom of the second micro-reaction cavity 7 under the control of the electric control rotating rod 20 to realize the function of magnetic collection.
Also, the bottom of the second micro-reaction chamber 7 is funnel-shaped to facilitate the collection of the product. A resistance heating wire 8 is wound on the outer wall of the second micro-reaction cavity 7, a heat insulation asbestos sleeve 9 is wrapped outside the second micro-reaction cavity 7, and a thermocouple 11 is inserted into the heat insulation asbestos sleeve 9 and connected onto the resistance heating wire 8, so that the polytetrafluoroethylene reaction kettle is loaded into a kettle sleeve and placed in a drying oven at 200 ℃. The temperature is controlled by a conventional temperature controller 23, which is connected to the thermocouple 11 at one end and to the resistance heating wire 8 at the other end. The tail end of the silicone tube 6 is also connected with a deionized water delivery pipe 12 and an ethanol delivery pipe 13, and similarly, the silicone tube 6 is provided with a second pinch valve 16, the second pinch valve 16 is used for controlling the delivery of the compound in the silicone tube 6, the deionized water delivery pipe 12 is provided with a second peristaltic pump 17, and the ethanol delivery pipe 13 is provided with a third peristaltic pump 18 which is respectively used for controlling the delivery of the deionized water and the delivery of the ethanol.
The tail end (output end) of the silicone tube 6 passes through a heat-insulating asbestos sleeve 9 of the second micro-reaction cavity component and is inserted at the upper end of the second micro-reaction cavity 7, and Fe3O4The head end of the magnetic nano particle conveying pipe 24 passes through a heat insulation asbestos sleeve 9 of the second micro reaction cavity assembly to be connected to the bottom of the second micro reaction cavity 7 at Fe3O4A self-control drain pipe is connected between the third pinch valve 19 and the second micro-reaction cavity 7 on the magnetic nano-particle conveying pipe 24, the self-control drain pipe is a traditional drain pipe additionally provided with a self-control valve and used for discharging waste liquid in the treatment process, and the self-control drain pipe is provided with a drain pipeAn electric control valve is used for controlling the drainage switch. Fe3O4The magnetic nanoparticle delivery pipe 24 is used for synthetically preparing Fe3O4And (4) outputting the magnetic nanoparticles.
To realize Fe3O4The fluid synthesis preparation device of the magnetic nanoparticles can be controlled automatically and can be controlled in a unified way through the main control chip 25. As shown in fig. 2, control signal input ends of the first peristaltic pump 14, the first pinch valve 15, the magnetic stirrer 3, the second pinch valve 16, the second peristaltic pump 17, the third peristaltic pump 18, the temperature controller 23, the electrically controlled rotary rod 20, the third pinch valve 19 and the self-controlled drain pipe are respectively connected with a control signal output end of a main control chip 25, and the valves, the pumps and the like are comprehensively controlled through the main control chip 25.
Here, provision is also made for Fe3O4An automated method for controlling a fluid synthesis production facility for magnetic nanoparticles, comprising the steps of:
firstly, three powder samples of ferric chloride hexahydrate, trisodium citrate and anhydrous sodium acetate are manually weighed and placed into a cavity of a first micro-reaction cavity 1, a main control chip 25 opens a first peristaltic pump 14 and a first pinch valve 15, and ethylene glycol is injected into the cavity of the first micro-reaction cavity 1 through an ethylene glycol supply pipe 2.
In the second step, the main control chip 25 starts the magnetic stirrer 3, and the magnetons 5 in the first micro-reaction chamber 1 are used for stirring the reaction solution.
And thirdly, after the operation lasts for half an hour, the main control chip 25 controls the magnetic stirrer 3 to be closed.
Fourthly, the main control chip 25 opens the second pinch valve 16, and the liquid which is completely reacted in the silicone tube 6 is introduced into the second micro-reaction cavity assembly and is sent into the second micro-reaction cavity 7.
And fifthly, the main control chip 25 controls the temperature controller 23 to turn on the resistance heating wire 8 to heat to 200 ℃ for 10 hours.
And sixthly, the main control chip 25 controls the temperature controller 23 to close the heating wire 1, and the natural cooling is completed after waiting for two hours.
Seventh, the main control chip 25 controls the magnetThe electrically controlled rotary rod 20 of the rotary component 10 drives the magnet 22 to be placed under the second micro-reaction chamber 7, and the product Fe is obtained by the action of the magnet 223O4The magnetic nanoparticles are collected and deposited at the bottom of the second micro-reaction chamber 7.
And step eight, the main control chip 25 closes the third pinch valve 19, opens the self-control drain pipe, and discharges the waste liquid in the second micro-reaction cavity 7 through the self-control drain pipe.
And step nine, the main control chip 25 closes the self-control water drainage pipe, and controls the electric control rotating rod 20 to drive the magnet 22 to reset.
Step ten, deionized water cleaning: the main control chip 25 closes the automatic control drain pipe, the magnet rotating assembly 10 drives the magnet 22 to reset, the magnet moves out of the lower portion of the second micro-reaction cavity 7, the main control chip 25 opens the second peristaltic pump 17, deionized water is introduced through the deionized water conveying pipe 12, the magnet rotating assembly 10 drives the magnet 22 to move into the lower portion of the second micro-reaction cavity 7, the automatic control drain pipe is opened, and deionized water waste liquid is discharged. And multiple deionized water cleaning steps are carried out.
Step ten, ethanol cleaning: the main control chip 25 controls the magnet 22 to reset, starts the third peristaltic pump 18, and introduces ethanol through the ethanol delivery pipe 13, and in the same way as the previous step, the displacement of the magnet 22 is repeated, and the automatic control drain pipe is matched to start and discharge ethanol waste liquid; and ethanol washing is performed for a plurality of times.
The twelfth step, finally, the main control chip 25 opens the third pinch valve 19 to let Fe3O4And (4) outputting the magnetic nanoparticles.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (2)
1. For preparing Fe3O4The fluid synthesis preparation device of magnetic nanoparticles is characterized in that: the device comprises a first micro-reaction cavity assembly and a second micro-reaction cavity assembly, wherein the first micro-reaction cavity assembly comprises a first micro-reaction cavity (1), the upper end of the first micro-reaction cavity (1) is connected with an ethylene glycol supply pipe (2), the bottom of the first micro-reaction cavity (1) is funnel-shaped, the first micro-reaction cavity (1) is placed on a magnetic stirrer (3), a sieve plate (4) is arranged in the first micro-reaction cavity (1), a magneton (5) is placed on the sieve plate (4), the head end of a silicone tube (6) is connected to the bottom of the first micro-reaction cavity (1), and the tail end of the silicone tube (6) is connected to the upper end of the second micro-reaction cavity assembly;
the second micro-reaction cavity assembly comprises a second micro-reaction cavity (7) and a magnet rotating assembly (10), the bottom of the second micro-reaction cavity (7) is located above the radius of a magnet rotating track of the magnet rotating assembly (10), the bottom of the second micro-reaction cavity (7) is funnel-shaped, a resistance heating wire (8) is wound on the outer wall of the second micro-reaction cavity (7), a heat insulation asbestos sleeve (9) is wrapped outside the second micro-reaction cavity (7), and a thermocouple (11) is inserted into the heat insulation asbestos sleeve (9) and connected onto the resistance heating wire (8);
the tail end of the silicone tube (6) is also connected with a deionized water conveying pipe (12) and an ethanol conveying pipe (13), the tail end of the silicone tube (6) penetrates through a heat-insulating asbestos sleeve (9) of the second micro-reaction cavity component to be inserted at the upper end of the second micro-reaction cavity (7), and Fe3O4The head end of the magnetic nano particle conveying pipe (24) penetrates through a heat insulation asbestos sleeve (9) of the second micro reaction cavity assembly to be connected to the bottom of the second micro reaction cavity (7);
ethylene glycol supply pipe (2) on install first peristaltic pump (14), first pinch valve (15), silicone tube (6) on install second pinch valve (16), deionized water conveyer pipe (12) on install second peristaltic pump (17), ethanol conveyer pipe (13) on install third peristaltic pump (18), Fe3O4A third pinch valve (19) is arranged on the magnetic nano-particle delivery pipe (24), and Fe3O4A self-control drain pipe is connected between the third pinch valve (19) and the second micro-reaction cavity (7) on the magnetic nano-particle conveying pipe (24);
the magnet rotating assembly (10) comprises an electric control rotating rod (20), a clamp (21) is fixedly mounted on the electric control rotating rod (20), a magnet (22) is clamped on the clamp (21), and the bottom of the second micro-reaction cavity (7) is positioned above the radius of a rotating track of the magnet (22); the device also comprises a temperature controller (23), wherein one end of the temperature controller (23) is connected to the thermocouple (11), and the other end of the temperature controller is connected to the resistance heating wire (8);
the automatic control device is characterized by further comprising a main control chip (25), wherein control signal input ends of the first peristaltic pump (14), the first pinch valve (15), the magnetic stirrer (3), the second pinch valve (16), the second peristaltic pump (17), the third peristaltic pump (18), the temperature controller (23), the electric control rotating rod (20), the third pinch valve (19) and the automatic control drain pipe are respectively connected with a control signal output end of the main control chip (25).
2. A process for the preparation of Fe according to claim 13O4The control method of the fluid synthesis preparation device of the magnetic nanoparticles is characterized by comprising the following steps:
21) after three powder samples of ferric chloride hexahydrate, trisodium citrate and anhydrous sodium acetate are placed into the cavity of the first micro-reaction cavity (1), the main control chip (25) starts the first peristaltic pump (14) and opens the first pinch valve (15), and ethylene glycol is injected into the cavity of the first micro-reaction cavity (1) through the ethylene glycol supply pipe (2);
22) the main control chip (25) starts the magnetic stirrer (3) and utilizes the magnetons (5) in the first micro-reaction cavity (1) to stir the reaction solution;
23) after the main control chip (25) controls the magnetic stirrer (3) to work continuously for half an hour, the main control chip (25) closes the magnetic stirrer (3);
24) the main control chip (25) opens the second pinch valve (16) and sends the liquid which is completely reacted in the silicone tube (6) into the second micro-reaction cavity (7);
25) the main control chip (25) controls the temperature controller (23) to heat the resistance heating wire (8), so that the resistance heating wire (8) is heated to 200 ℃ and lasts for 10 hours;
26) the main control chip (25) controls the temperature controller (23) to close the resistance heating wire (8), and the natural cooling is completed after two hours;
27) the main control chip (25) controls an electric control rotating rod (20) of the magnet rotating assembly (10) to rotatably place the magnet (22) below the second micro-reaction cavity (7);
28) the main control chip (25) closes the third pinch valve (19), opens the automatic control drain pipe, and discharges the waste liquid in the second micro-reaction cavity (7) through the automatic control drain pipe;
29) the main control chip (25) closes the self-control water drainage pipe, controls the electric control rotating rod (20) to drive the magnet (22) to reset, and moves out of the lower part of the second micro-reaction cavity (7);
210) and (3) deionized water cleaning: the main control chip (25) opens the second peristaltic pump (17) and leads in deionized water through the deionized water conveying pipe (12); then, the magnet (22) is driven by the electrically controlled rotating rod (20) to move to the lower part of the second micro-reaction cavity (7), and the main control chip (25) opens the self-controlled drain pipe to discharge the deionized water waste liquid; carrying out multiple deionized water cleaning steps;
211) ethanol cleaning: the main control chip (25) controls the electric control rotating rod (20) to drive the magnet (22) to reset, moves out of the lower part of the second micro-reaction cavity (7), controls the opening of the third peristaltic pump (18), and leads in ethanol through the ethanol conveying pipe (13); then, the magnet (22) is driven by the electrically controlled rotating rod (20) to move to the lower part of the second micro-reaction cavity (7), and the main control chip (25) opens the self-controlled drain pipe to discharge the ethanol waste liquid; carrying out ethanol cleaning for multiple times;
212) finally, the main control chip (25) controls to open the third pinch valve (19) to enable Fe3O4And discharging the magnetic nanoparticles.
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