CN110559935A - Preparation method of one-dimensional nano magnetons with stable solution dispersibility - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 70
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 14
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 12
- 239000012279 sodium borohydride Substances 0.000 claims description 12
- 229920002521 macromolecule Polymers 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 229910017108 Fe—Fe Inorganic materials 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 3
- 230000005389 magnetism Effects 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 239000006249 magnetic particle Substances 0.000 description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 6
- 239000002122 magnetic nanoparticle Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 150000001450 anions Chemical group 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000011553 magnetic fluid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- 108010039918 Polylysine Proteins 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- -1 carbon nanotube compound Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000656 polylysine Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- GUCXXOFNASDXOJ-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate;styrene Chemical compound [Na+].C=CC1=CC=CC=C1.[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 GUCXXOFNASDXOJ-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/45—Magnetic mixers; Mixers with magnetically driven stirrers
- B01F33/452—Magnetic mixers; Mixers with magnetically driven stirrers using independent floating stirring elements
Abstract
The invention belongs to the technical field of magnetic stirring, and relates to a preparation method of one-dimensional nano magnetons with stable solution dispersibility3O4The nano particles are fixed on the surface of the water-soluble one-dimensional carbon nano tube which can be stably dispersed in water, so that the prepared one-dimensional nano magnetons have stable dispersibility in water, magnetic stirring can be realized under the micro-nano scale and in a confined micro space, and Fe is controlled3O4The size and distribution density of the nano particles on the surface of the water-soluble carbon nano tube control the magnetism of the one-dimensional nano magnetons.
Description
The technical field is as follows:
The invention belongs to the technical field of magnetic stirring, and relates to a preparation method of one-dimensional nano magnetons with stable solution dispersibility, which is used for preparing one-dimensional nano magnetons capable of realizing magnetic stirring under the micro-nano scale and in a confined micro space.
background art:
the magnetic stirring utilizes the principle that like poles repel and opposite poles attract of a magnetic field, and magnetic particles with magnetism placed in a container are pushed to move by the magnetic field, so that the purpose of stirring is achieved. The magnetic stirring can realize the non-mechanical contact type power transmission of the driving device and the stirring device, and has important application value in a closed system (such as a high-pressure container). In addition, the non-mechanical contact power transmission of magnetic stirring can realize the multi-magneton synergistic stirring function, and particularly, when the magneton reaches the nanoscale and can be stably dispersed in a solution, the stirring function of the nanomagnet under the micro-nano scale and in a confined micro-space can be realized through the action of a magnetic field. The preparation of nano-sized magnetons capable of being stably dispersed in an aqueous solution is the key of magnetic stirring in a micro-nano scale and a confined micro-space, but related researches are only rarely reported at present, and researchers have conducted more research reports on the preparation of magnetic nanoparticles in the fields of physical adsorption, medical carriers, magnetic resonance imaging and the like: chinese patent 201610476814.1 discloses a preparation method and application of a nano magnetic polylysine/(graphene oxide-carbon nanotube) biological adsorption material, wherein a chemical coprecipitation method is used for preparing Fe3O4depositing magnetic particles on the surface of the graphene and carbon nanotube compound, and modifying lysine on a magnetic hybrid body by a surface grafting technology to prepare a magnetic biological adsorption material; chinese patent 200510041150.8 discloses a method for preparing nano magnetic liquid, which is to prepare Fe by using a coprecipitation method3O4particles, then by the reaction of Fe3O4the particles are peptized under acidic condition to obtain Fe3O4A transparent colloidal solution; chinese patent 200910197295.5 discloses a method for preparing water-soluble amino-functionalized Fe nano magnetic particles by iron-based coordination reaction-high-temperature pyrolysis-deamination protection reaction3O4a nanoparticle; the preparation method of the nano-magnetic polymer composite microsphere disclosed in Chinese patent 200810227202.4 and the preparation method of the nano-magnetic polymer composite microsphere disclosed in Chinese patent 201019114005.6 are both that Fe subjected to hydrophobic treatment is added in the emulsion polymerization process3O4Particle preparation of nano-polymersa biomagnetic microsphere; chinese patent 201310576592.7 discloses a method for preparing magnetic liquid with polyaniline derivative coated nano magnetic particles, which prepares polyaniline derivative coated magnetic nano Fe through distribution interpenetration reaction3O4A magnetic liquid of particles; chinese patent 201410152393.8 discloses a method for preparing water-soluble ferroferric oxide nano-magnetic fluid, which is to prepare Fe with the diameter of 3-5 nm by carrying out sealed reflux on trivalent ferric salt, urea and tartaric acid polyalcohol-water solution at the temperature of 100-200 DEG C3O4A nanofluid; chinese patent 201811050455.9 discloses a method for preparing nano magnetic particles for sewage treatment, which is prepared by mixing Fe3O4Treating the nano magnetons with an alkali solution, then treating with tetramethylsiloxane and coupling with PEG polymerization to prepare magnetic nanoparticles with PEG; chinese patent 201910025790.1 discloses a method for preparing high-stability water-based nano magnetic fluid, which is characterized in that Fe with good water solubility is prepared by a coprecipitation method under the dispersion action of macromolecular surfactant3O4Magnetic nanoparticles; although the above reports all provide methods for the preparation of magnetic nanoparticles, it is by the use of Fe3O4The magnetic particles are obtained by modification, and are enriched and purified under the magnetic field condition, so that the magnetic particles have low dispersion stability under the action of a magnetic field and are difficult to satisfy magnetic stirring under the micro-nano scale and in a limited space. Therefore, the method for preparing the one-dimensional nano magnetons with stable solution dispersibility has high social significance and practical value.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and develops and designs a preparation method of one-dimensional nano magnetons with stable solution dispersibility, which can prepare one-dimensional nano magnetons for realizing magnetic stirring under nano-micro scale and in a confined micro space.
In order to realize the aim, the one-dimensional nano magneton with stable solution dispersibility is prepared by generating magnetic Fe on the surface of a water-soluble carbon nano tube carrier through electrostatic adsorption-in-situ reduction3O4The specific process of the nano-particles comprises the preparation of water-solubleThe method comprises the following two steps of preparing a nano magneton by using a carbon nano tube carrier:
(1) Preparing a water-soluble carbon nano tube carrier by a concentrated acid oxidation method or a water-soluble macromolecule coating method;
The process for preparing the water-soluble carbon nano tube carrier by the concentrated acid oxidation method comprises the following steps: dispersing carbon nanotubes with set mass in concentrated acid formed by mixing nitric acid and sulfuric acid with a volume ratio of 1:3 under the magnetic stirring condition of 70-90 ℃ and a rotating speed of 100-500rpm, standing for 8-12h to form oxidized carbon nanotube slurry, dispersing the oxidized carbon nanotube slurry in deionized water, cleaning the slurry to be neutral through a filter membrane, collecting a substrate, drying the substrate in a vacuum drying box at a temperature of 50-80 ℃ for 24h to obtain oxidized carbon nanotube powder, and dissolving the oxidized carbon nanotube powder in water to obtain a water-soluble carbon nanotube carrier with a mass percentage concentration of 0.1-1%;
The process for preparing the water-soluble carbon nano tube carrier by the water-soluble macromolecule coating method comprises the following steps: preparing water-soluble macromolecular aqueous solution with set mass percentage concentration, dispersing carbon nano tubes with set mass in the water-soluble macromolecular aqueous solution under the stirring condition of the rotating speed of 200-500rpm, wherein the mass ratio of the carbon nano tubes to the water-soluble macromolecules is 1:20-2:1, ultrasonically dispersing for 3-5h under the condition of the power of 50-300W, filtering and collecting the carbon nano tubes coated with the water-soluble macromolecules, drying for 24h in a vacuum drying box at the temperature of 55 ℃ to obtain macromolecular coated carbon nano tube powder, and dissolving in water to obtain a water-soluble carbon nano tube carrier with the mass percentage concentration of 0.1-1%;
(2) Preparing nano magnetons: FeCl is dripped into the water-soluble carbon nano tube carrier prepared in the step (1) at the speed of 1-5 drops/10 s under the stirring condition that the rotating speed is 100-500rpm3Aqueous solution of Fe3+The mass ratio of the Fe-Fe3+Adsorbed to the surface of the carbon nano tube under the electrostatic adsorption effect with the anionic groups on the surface of the carbon nano tube, and then dropwise adding sodium borohydride aqueous solution, sodium borohydride aqueous solution and Fe at the speed of 1-5 drops/10 s3+The molar concentration ratio of the aqueous solution is 2:1-6:1, and stirring is carried out for 1-2h at a constant speed after dropwise adding to ensure that Fe3+Fe is separated out under the reduction of sodium borohydride3O4Nano particles are immobilized on the surface of the carbon nano tube carrier to obtain Fe immobilized on the surface3O4one-dimensional nanomagnets of particles.
The mass fractions of the nitric acid and the sulfuric acid related to the step (1) of the invention are respectively 98% and 68%, the mass ratio of the carbon nano tube to the concentrated acid is 1:10-1:50, and the mass percentage concentration of the water-soluble macromolecular aqueous solution is 0.1-10 g/L.
Compared with the prior art, the invention adopts a concentrated acid oxidation method or a water-soluble macromolecule coating method to prepare the water-soluble carbon nanotube carrier, and Fe is subjected to electrostatic adsorption-in-situ reduction growth3O4The nano particles are fixed on the surface of the water-soluble one-dimensional carbon nano tube which can be stably dispersed in water, so that the prepared one-dimensional nano magnetons have stable dispersibility in water, and Fe is controlled3O4The size and distribution density of the nano particles on the surface of the water-soluble carbon nano tube control the magnetism of the one-dimensional nano magnetons.
Description of the drawings:
Fig. 1 is a process flow diagram of a one-dimensional nanomagnet preparation method according to embodiment 1 of the present invention.
Fig. 2 is a transmission electron micrograph of the one-dimensional nanomagnet according to embodiment 1 of the present invention.
the specific implementation mode is as follows:
the invention is further illustrated by the following examples in conjunction with the accompanying drawings.
Example 1:
The preparation method of the one-dimensional nano magnetons with stable solution dispersibility comprises the following two steps of preparing a water-soluble carbon nano tube carrier by a concentrated acid oxidation method and preparing nano magnetons:
(1) Preparing a water-soluble carbon nano tube carrier by a concentrated acid oxidation method: dispersing 5g of carbon nano tube in 200g of concentrated acid formed by mixing nitric acid and sulfuric acid with the volume ratio of 1:3 under the magnetic stirring condition that the temperature is 70 ℃ and the rotating speed is 300rpm, standing for 8-12h to form oxidized carbon nano tube slurry, dispersing the oxidized carbon nano tube slurry in deionized water, cleaning the slurry to be neutral through a filter membrane, collecting a substrate, drying the substrate in a vacuum drying box at the temperature of 50-80 ℃ for 24h to obtain oxidized carbon nano tube powder, and dissolving the oxidized carbon nano tube powder in water to obtain a water-soluble carbon nano tube carrier with the mass percentage concentration of 0.1%;
(2) Preparing nano magnetons: FeCl is dripped into the water-soluble carbon nano tube carrier prepared in the step (1) at the speed of 3 drops/10 s under the stirring condition that the rotating speed is 300rpm3Aqueous solution of Fe3+the mass ratio of the Fe-3+Is adsorbed on the surface of the carbon nano tube under the electrostatic adsorption effect with the anion group on the surface of the carbon nano tube, and then sodium borohydride aqueous solution, the sodium borohydride aqueous solution and Fe are dripped at the speed of 3 drops/10 s3+The molar concentration ratio of the aqueous solution is 2:1, stirring at 300rpm for 2h after dropwise addition to allow Fe3+Fe is separated out under the reduction of sodium borohydride3O4Nano particles are immobilized on the surface of the carbon nano tube carrier to obtain Fe immobilized on the surface3O4One-dimensional nanomagnets of particles.
Example 2:
The preparation method of the one-dimensional nano magnetons with stable solution dispersibility comprises two steps of preparing a water-soluble carbon nano tube carrier by a macromolecule coating method and preparing nano magnetons:
(1) preparing a water-soluble carbon nanotube carrier by a macromolecular coating method: dispersing 0.1g of carbon nano tube in 100g of poly (styrene-sodium p-styrene sulfonate) aqueous solution with the concentration of 2g/L under the magnetic stirring condition with the rotating speed of 300rpm, carrying out ultrasonic treatment for 30min, carrying out suction filtration and washing for three times, collecting a substrate, carrying out vacuum drying for 24h at 55 ℃, obtaining macromolecular coated carbon nano tube powder, and dissolving the macromolecular coated carbon nano tube powder in water to obtain a water-soluble carbon nano tube carrier with the mass percentage concentration of 0.1%;
(2) Preparing nano magnetons: FeCl is dripped into the water-soluble carbon nano tube carrier prepared in the step (1) at the speed of 3 drops/10 s under the stirring condition that the rotating speed is 300rpm3Aqueous solution of Fe3+The mass ratio of the Fe-3+Under the electrostatic adsorption effect with the anion groups on the surface of the carbon nano tubeAdsorbed on the surface of the carbon nano tube, and then dropwise adding sodium borohydride aqueous solution, sodium borohydride aqueous solution and Fe at the speed of 3 drops/10 s3+The molar concentration ratio of the aqueous solution is 2:1, stirring at 300rpm for 2h after dropwise addition to allow Fe3+Fe is separated out under the reduction of sodium borohydride3O4nano particles are immobilized on the surface of the carbon nano tube carrier to obtain Fe immobilized on the surface3O4One-dimensional nanomagnets of particles.
Claims (5)
1. a preparation method of one-dimensional nano magnetons with stable solution dispersibility is characterized in that magnetic Fe is generated on the surface of a water-soluble carbon nano tube carrier through electrostatic adsorption-in-situ reduction3O4the specific process of the nano-particle comprises two steps of preparing a water-soluble carbon nano-tube carrier and preparing a nano magneton:
(1) Preparing a water-soluble carbon nano tube carrier by a concentrated acid oxidation method or a water-soluble macromolecule coating method;
(2) Preparing nano magnetons: FeCl is dripped into the water-soluble carbon nano tube carrier prepared in the step (1) at the speed of 1-5 drops/10 s under the stirring condition that the rotating speed is 100-500rpm3Aqueous solution of Fe3+The mass ratio of the Fe-Fe3+Adsorbed to the surface of the carbon nano tube under the electrostatic adsorption effect with the anionic groups on the surface of the carbon nano tube, and then dropwise adding sodium borohydride aqueous solution, sodium borohydride aqueous solution and Fe at the speed of 1-5 drops/10 s3+The molar concentration ratio of the aqueous solution is 2:1-6:1, and stirring is carried out for 1-2h at a constant speed after dropwise adding to ensure that Fe3+Fe is separated out under the reduction of sodium borohydride3O4Nano particles are immobilized on the surface of the carbon nano tube carrier to obtain Fe immobilized on the surface3O4One-dimensional nanomagnets of particles.
2. the method for preparing one-dimensional nano magnetons with stable solution dispersibility according to claim 1, wherein the concentrated acid oxidation method is used for preparing the water-soluble carbon nano tube carrier by the following steps: dispersing carbon nano tubes with set mass in concentrated acid formed by mixing nitric acid and sulfuric acid with a volume ratio of 1:3 under the magnetic stirring condition that the temperature is 70-90 ℃ and the rotating speed is 100-500rpm, standing for 8-12h to form oxidized carbon nano tube slurry, dispersing the oxidized carbon nano tube slurry in deionized water, cleaning the slurry to be neutral through a filter membrane, collecting a substrate, drying the substrate in a vacuum drying box at the temperature of 50-80 ℃ for 24h to obtain oxidized carbon nano tube powder, and dissolving the oxidized carbon nano tube powder in water to obtain a water-soluble carbon nano tube carrier with the mass percentage concentration of 0.1-1%.
3. The method for preparing one-dimensional nano magnetons with stable solution dispersibility according to claim 2, wherein the water-soluble carbon nanotube carrier is prepared by a water-soluble macromolecule coating method, which comprises the following steps: preparing water-soluble macromolecular aqueous solution with set mass percentage concentration, dispersing carbon nano tubes with set mass in the water-soluble macromolecular aqueous solution under the stirring condition of the rotating speed of 200-500rpm, wherein the mass ratio of the carbon nano tubes to the water-soluble macromolecules is 1:20-2:1, ultrasonically dispersing for 3-5h under the condition of the power of 50-300W, filtering and collecting the carbon nano tubes coated with the water-soluble macromolecules, drying for 24h in a vacuum drying box at the temperature of 55 ℃ to obtain macromolecular coated carbon nano tube powder, and dissolving in water to obtain the water-soluble carbon nano tube carrier with the mass percentage concentration of 0.1-1%.
4. The method according to claim 2, wherein the mass fractions of nitric acid and sulfuric acid are 98% and 68%, respectively, and the mass ratio of the carbon nanotubes to the concentrated acid is 1:10 to 1: 50.
5. The method according to claim 3, wherein the water-soluble macromolecule aqueous solution has a mass percentage concentration of 0.1-10 g/L.
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| CN114129724A (en) * | 2020-09-03 | 2022-03-04 | 天津大学 | Microwave-excited targeted sterilization nano particle, preparation method and application thereof |
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