CN115064640A - Tubular micromotor made of MOF (Metal-organic framework) annealing material and preparation method thereof - Google Patents
Tubular micromotor made of MOF (Metal-organic framework) annealing material and preparation method thereof Download PDFInfo
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- 238000000137 annealing Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000012621 metal-organic framework Substances 0.000 title description 19
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 39
- 239000004417 polycarbonate Substances 0.000 claims abstract description 39
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 238000002207 thermal evaporation Methods 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 230000005389 magnetism Effects 0.000 abstract description 3
- 238000003828 vacuum filtration Methods 0.000 description 7
- 239000003814 drug Substances 0.000 description 5
- 229940079593 drug Drugs 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000033001 locomotion Effects 0.000 description 3
- 238000007726 management method Methods 0.000 description 3
- 238000005067 remediation Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000026058 directional locomotion Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002901 radioactive waste Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- -1 structures Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N35/00—Magnetostrictive devices
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H10N35/00—Magnetostrictive devices
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Abstract
The invention relates to a tubular micromotor made of MOF annealing materials and a preparation method thereof, wherein the preparation method comprises the following steps: preparing ZIF-67; respectively cleaning and drying a porous polycarbonate template A1 and a porous polycarbonate template A2, and then evaporating a layer of metal on one side of a porous polycarbonate template A1 by using a thermal evaporation instrument to serve as a substrate; dissolving ZIF-67 in deionized water to obtain a ZIF-67 dispersion liquid, sequentially passing the ZIF-67 dispersion liquid through a stacked porous polycarbonate template A2 and a porous polycarbonate template A1, and taking out the porous polycarbonate template A1 as a tubular micro-nano motor precursor; and (3) carrying out post-treatment on the tubular micro-nano motor precursor by using dichloromethane, dissolving the porous polycarbonate template, and then centrifuging and washing to obtain the tubular micro motor of the MOF annealing material. Compared with the prior art, the preparation method is simple, and the obtained micro-nano motor not only has strong magnetism, but also has better adsorption capacity based on the inherent porous structure and porosity.
Description
Technical Field
The invention relates to the field of micro-nano motors, in particular to a tubular micro-motor made of an MOF (metal-organic framework) annealing material and a preparation method thereof.
Background
Since the emergence of 2002, micro-motors have become one of the research areas in which nanotechnology is attracting much attention. The self-driven micro-nano motor is concerned about due to the intelligentization trend. To date, micro-motors have found widespread use in drug delivery, biosensing, imaging, environmental remediation, and bacterial isolation.
In order to realize the bubble-driven micro motor, it is necessary to dope expensive, toxic, unstable catalysts, or to add expensive metals or high concentrations of toxic chemical fuels, which severely limits their practical applications.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a tubular micromotor made of MOF annealing materials and a preparation method thereof, the preparation method is simple, and the obtained micro-micromotor not only has strong magnetism, but also has good adsorption capacity based on the inherent porous structure and porosity.
In the conception process, the applicant considers that in order to break through the limitations, the integration of the highly ordered porous material with large surface area into the colloidal motor is a promising strategy for improving the self-propulsion speed and adsorption, which is beneficial to many applications, so the technical scheme selects the ZIF-67 as an MOF material as a precursor of a micro-motor, and the magnetic Co nanocomposite material can be obtained by annealing the ZIF-67.
While individual annealed MOF particles have been chemically drivable in prior studies, they are not sufficiently widely feasible, practical, and serve as a carrier payload. Therefore, the technical scheme adopts the annealing particles to prepare the tubular micro-nano motor, is convenient to uniformly control and apply, can be massively produced and stable, has biocompatibility, and can change the tubular template to carry out directional self-driven directional movement or transportation. Due to the presence of magnetic Co, their motion can be controlled in magnetic fields and thus can be applied in environmental remediation, recovery under magnetic control, and stable recycling capability and high selectivity. The self-propelled magnetic recyclable micro-nano motor can play a role in the management and the repair of radioactive wastes in the future, and provides great inspiration and opportunity for improving the efficiency and the accurate release of the medicines in a medicine conveying system.
The purpose of the invention can be realized by the following technical scheme:
a first object of the invention is to provide a method for the preparation of a tubular micromotor of MOF annealed material, comprising the following steps:
s1: preparing ZIF-67, and grinding into ZIF-67 powder particles;
s2: respectively cleaning and drying a porous polycarbonate template A1 and a porous polycarbonate template A2, and then evaporating a layer of metal on one side of the porous polycarbonate template A1 by using a thermal evaporation instrument to serve as a substrate;
s3: dissolving the ZIF-67 obtained in the step S1 in deionized water to obtain a ZIF-67 dispersion liquid, sequentially passing the ZIF-67 dispersion liquid through a stacked porous polycarbonate template A2 and a porous polycarbonate template A1, and taking out the porous polycarbonate template A1 as a tubular micro-nano motor precursor;
s4: and (3) carrying out post-treatment on the tubular micro-nano motor precursor obtained in the S3 by using dichloromethane, dissolving the porous polycarbonate template, and then centrifuging and washing to obtain the tubular micro motor of the MOF annealing material.
Further, in S1, ZIF-67 was synthesized from 2-methylimidazole, cobalt sulfate heptahydrate, and polyvinylpyrrolidone as raw materials.
Further, in S1, the composition of the raw material required for ZIF-67 included 0.05mol/L of CoSO 4 ·7H 2 O, 0.004mol/L polyvinylpyrrolidone and 0.8 mol/L2-methylimidazole.
Further, in S1, the preparation process of ZIF-67 includes:
preparing 2-methylimidazole, cobalt sulfate heptahydrate and polyvinylpyrrolidone into a solution, standing at room temperature for 24 hours, separating supernatant, reserving a lower product, and performing aftertreatment to obtain ZIF-67.
Further, the post-processing process comprises: the remaining lower product was washed 5 times with ethanol and deionized water successively at 6000 rpm for 10 minutes each, and then vacuum-dried to obtain ZIF-67.
Further, the prepared ZIF-67 was annealed at a temperature of 800 ℃, and then ground into powder particles;
wherein the parameters set in the annealing treatment process are as follows:
initial temperature: 30 ℃;
heating time: 154 min;
final temperature: 800 ℃;
retention time: 180 min;
heating rate: 5 ℃/min.
Further, in S2, one side of the porous polycarbonate template a1 was evaporated with a layer of metal Au as a substrate using a thermal evaporation apparatus.
Further, in S3, when the porous polycarbonate template a2 and the porous polycarbonate template a1 are stacked, the Au-plated side of the porous polycarbonate template a1 is placed at the bottommost part;
the solution after suction filtration is recycled and passes through the porous polycarbonate template A2 and the porous polycarbonate template A1 which are stacked in sequence in the suction filtration process.
Further, the tubular micro-nano motor precursor is dissolved and treated by dichloromethane, then the dissolved solution is placed in a centrifuge, and is continuously centrifuged for 3 minutes by alcohol and water at the rotating speed of 6000 rpm, and each solution is sequentially cleaned for 3 times.
A second object of the invention is to provide a tubular micromotor of MOF annealed material obtained as described above.
Compared with the prior art, the invention has the following technical advantages:
1) the preparation method is simple, and the obtained micro-nano motor not only has strong magnetism, but also has an inherent porous structure and porosity, has good adsorption capacity, and can be applied to the efficient management of the environment and the functions of carrying, transmitting and releasing medicines in the future medical field.
2) According to the technical scheme, the tubular micro-nano motor is prepared by adopting the annealing particles, so that unified control and application are facilitated, mass production and stability can be realized, biocompatibility is realized, and the tubular template can be changed to perform directional self-driving directional movement or transportation. Due to the presence of magnetic Co, their motion can be controlled in magnetic fields and thus can be applied in environmental remediation, recovery under magnetic control, and stable recycling capability and high selectivity. The self-propelled magnetic recyclable micro-nano motor can play a role in the management and the repair of radioactive wastes in the future, and provides great inspiration and opportunity for improving the efficiency and the accurate release of the medicines in a medicine conveying system.
Drawings
Fig. 1 is a scanning electron microscope (scale is 1 μm) of the MOF-annealed tubular micro-nano motor in the technical scheme;
FIG. 2 is a schematic view of a tube annealing furnace used in the examples;
FIG. 3 is a diagram of a vacuum filtration apparatus used in the examples;
fig. 4 is XRD data of the tubular micro-nano motor for annealing MOF in the present technical scheme.
Detailed Description
The present invention is described in detail below with reference to the accompanying drawings and specific examples, and features of preparation means, materials, structures, or composition ratios which are not explicitly described in the technical scheme are all regarded as common technical features disclosed in the prior art.
The tubular micro-nano motor for annealing the MOF in the embodiment is of a tubular structure, the length of the tubular micro-nano motor is 10-12um, the pore diameter of the tubular micro-nano motor is 5um, and the tubular micro-nano motor is prepared by the following steps:
the method comprises the following steps: first 0.05mol of cobalt sulfate heptahydrate (CoSO) 4 ·7H 2 O) and 0.004mol of polyvinylpyrrolidone (PVP) are mixed and put into 1L of deionized water, and then 0.8mol of 2-methylimidazole (2-MeIM) is added for chemistryReacting, stirring vigorously for thirty minutes, standing at room temperature for 24 hours to achieve the purpose of full reaction, and synthesizing the raw material ZIF-67 as shown in the following table.
The composition of the ZIF-67 bath is shown in the following table:
the synthesized ZIF-67 product is kept standing at room temperature for 24 hours, then the supernatant is separated, and the lower product is reserved
Step two: the separated lower product in the beaker was washed three times with deionized water at 6000 revolutions for 10 minutes each using a centrifuge for the purpose of reducing impurities in the sample, and then dried in a vacuum oven for 24 hours, and ground into powder particles.
Step three: putting the powdery particles obtained in the second step into a tube annealing furnace, performing annealing treatment at 800 ℃ as shown in fig. 2 (the tube annealing furnace adopted in the embodiment of fig. 2), vacuum-drying the annealed material for 24 hours, and grinding the material into powdery particles as a raw material for later use, wherein the setting parameters of the tube furnace in the annealing treatment process are as follows:
initial temperature: 30 ℃;
heating time: 154 min;
final temperature: 800 ℃;
retention time: 180 min;
heating rate: 5 ℃/min.
Step four: pretreating two porous polycarbonate templates A1 and A2, and evaporating a layer of gold on one side of the porous polycarbonate template A1 by using a thermal evaporation instrument to serve as a substrate;
step five: dissolving the ZIF-67 annealed in the third step into deionized water, performing vacuum filtration on a vacuum filtration device for three minutes as shown in fig. 3 (fig. 3 is a vacuum filtration device adopted in the embodiment), so that a space A1 and a2 are placed at the upper part of the vacuum filtration device to form a low-pressure state, allowing the solution to pass through two pretreated porous polycarbonate templates A1 and A2 to perform stacking and precipitation to prepare a tubular micro-nano motor as shown in fig. 1 (fig. 1 is a scanning electron microscope sample of the tubular micro-nano motor for annealing the MOF in the technical scheme), and performing the vacuum filtration process to circularly utilize the solution subjected to the vacuum filtration to sequentially pass through a plurality of stacked porous polycarbonate templates A2 and a porous polycarbonate template A1 to reach a particle tight stacking tube.
Step six: and finally, respectively cleaning the template A2 subjected to deposition in the fifth step with dichloromethane for three times under the condition of 6000 revolutions for 3 minutes each time by using a centrifugal machine, and removing the porous polycarbonate template, so as to obtain the multifunctional self-driven annealing MOF tubular micro-nano motor, wherein the speed of the micro motor under the concentration of 3% hydrogen peroxide is about 150 mu m/s, and the micro motor has a faster movement speed compared with a single particle.
Step seven: as in the above-mentioned procedures, it was found that different ratios were used in the preparation process (the ratio was changed such that the composition of the raw materials required for ZIF-67 included 0.1mol/L CoSO 4 ·7H 2 O, 0.008mol/L polyvinylpyrrolidone, 0.8 mol/L2-methylimidazole), the prepared product has a certain degree of adverse effect on the size of the particles and the carbonization degree of the tubular micro-nano motor of the annealed MOF, as shown in fig. 4 (fig. 4 is XRD data of the tubular micro-nano motor of the annealed MOF in the technical scheme), two peaks appear between 2 theta and 40 degrees and 55 degrees, the comparison shows that the change of the proportion results in the increase of the crystallinity, the size of the Co nano particles is increased, so the moving speed of the tubular micro-nano motor is reduced, and the application of the tubular micro-nano motor of the annealed MOF is adversely affected.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a tubular micromotor of MOF annealing material is characterized by comprising the following steps:
s1: preparing ZIF-67, and grinding into ZIF-67 powder particles;
s2: respectively cleaning and drying a porous polycarbonate template A1 and a porous polycarbonate template A2, and then evaporating a layer of metal on one side of the porous polycarbonate template A1 by using a thermal evaporation instrument to serve as a substrate;
s3: dissolving the ZIF-67 obtained in the step S1 in deionized water to obtain a ZIF-67 dispersion liquid, sequentially passing the ZIF-67 dispersion liquid through a stacked porous polycarbonate template A2 and a porous polycarbonate template A1, and taking out the porous polycarbonate template A1 as a tubular micro-nano motor precursor;
s4: and (3) carrying out post-treatment on the tubular micro-nano motor precursor obtained in the step S3 by using dichloromethane, dissolving the porous polycarbonate template, and then centrifuging and washing to obtain the tubular micro-motor of the MOF annealing material.
2. The method for preparing the tubular micromotor of the MOF annealing material, according to the claim 1, wherein in S1, the ZIF-67 is synthesized by taking 2-methylimidazole, cobalt sulfate heptahydrate and polyvinylpyrrolidone as raw materials.
3. The method of claim 2, wherein the raw material composition for ZIF-67 in S1 comprises 0.05mol/L CoSO 4 ·7H 2 O, 0.004mol/L polyvinylpyrrolidone and 0.8 mol/L2-methylimidazole.
4. The method for preparing the tubular micromotor of the MOF annealing material, according to the claim 1, wherein in S1, the ZIF-67 preparation process comprises the following steps:
preparing 2-methylimidazole, cobalt sulfate heptahydrate and polyvinylpyrrolidone into a solution, standing at room temperature for 24 hours, separating supernatant, reserving a lower product, and performing aftertreatment to obtain ZIF-67.
5. The method of manufacturing a tubular micromotor of MOF annealed material according to claim 4, wherein the post-treatment process comprises: the remaining lower product was washed 5 times with alcohol and deionized water at 6000 rpm for 10 minutes each, followed by vacuum drying to obtain ZIF-67.
6. The method for preparing the tubular micromotor of the MOF annealed material according to claim 1, characterized in that the prepared ZIF-67 is annealed at a temperature of 800 ℃ and then ground into powdery particles;
wherein the parameters set in the annealing treatment process are as follows:
initial temperature: 30 ℃;
heating time: 154 min;
final temperature: 800 ℃;
retention time: 180 min;
heating rate: 5 ℃/min.
7. The method of claim 1, wherein in step S2, a layer of metal Au is evaporated from one side of the porous polycarbonate template a1 by a thermal evaporation apparatus to form a substrate.
8. The method of claim 7, wherein in step S3, when the porous polycarbonate template a2 and the porous polycarbonate template a1 are stacked, the Au-plated side of the porous polycarbonate template a1 is placed at the bottom;
the solution after suction filtration is recycled and passes through the porous polycarbonate template A2 and the porous polycarbonate template A1 which are stacked in sequence in the suction filtration process.
9. The method for preparing the tubular micromotor of the MOF annealing material, according to claim 1, is characterized in that dichloromethane is used for dissolving and treating the tubular micromotor precursor, then the dissolved solution is placed in a centrifuge, alcohol and water are respectively used for continuous centrifugation for 3 minutes at the rotating speed of 6000 revolutions per minute, and each solution is sequentially washed for 3 times.
10. A tubular micromotor of MOF annealed material obtained by the method of any one of claims 1 to 9.
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| CN116587318A (en) * | 2023-04-27 | 2023-08-15 | 东华大学 | Metal organic framework reinforced micro-nano fiber film-based actuator and preparation and application thereof |
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| CN116587318A (en) * | 2023-04-27 | 2023-08-15 | 东华大学 | Metal organic framework reinforced micro-nano fiber film-based actuator and preparation and application thereof |
| CN116587318B (en) * | 2023-04-27 | 2024-05-14 | 东华大学 | Metal organic framework reinforced micro-nano fiber film-based actuator and preparation and application thereof |
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