CN109455769A - A kind of preparation method of magnetism Nano carbon balls - Google Patents
A kind of preparation method of magnetism Nano carbon balls Download PDFInfo
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- CN109455769A CN109455769A CN201910014768.7A CN201910014768A CN109455769A CN 109455769 A CN109455769 A CN 109455769A CN 201910014768 A CN201910014768 A CN 201910014768A CN 109455769 A CN109455769 A CN 109455769A
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- 241000143432 Daldinia concentrica Species 0.000 title claims abstract description 50
- 229910021392 nanocarbon Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 230000005389 magnetism Effects 0.000 title claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 229920000428 triblock copolymer Polymers 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 12
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 19
- 230000035484 reaction time Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000012450 pharmaceutical intermediate Substances 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 241000209094 Oryza Species 0.000 description 7
- 235000007164 Oryza sativa Nutrition 0.000 description 7
- 235000009566 rice Nutrition 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000002122 magnetic nanoparticle Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002077 nanosphere Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XHQSLVIGPHXVAK-UHFFFAOYSA-K iron(3+);octadecanoate Chemical compound [Fe+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XHQSLVIGPHXVAK-UHFFFAOYSA-K 0.000 description 1
- 230000002101 lytic effect Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
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)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- 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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of magnetic Nano carbon balls, it is with naphthalene or 1,5- dihydroxy naphthlene is carbon source, triblock copolymer PF127 is surfactant, in the presence of source of iron ferrocene, solvent thermal reaction is carried out in the anhydrous ethanol solvent system containing hydrogen peroxide, one-step method prepares magnetic Nano carbon balls.The method of the present invention is low in cost, and reaction temperature is lower, and the reaction time is short, and the magnetic Nano carbon balls purity is high of preparation, chemical stability is good, can be applied to the technical fields such as adsorbent material, catalyst carrier, pharmaceutical intermediate, and practicability is wide.
Description
Technical field
The present invention relates to a kind of preparation method of Nano carbon balls, especially a kind of preparation method of magnetic Nano carbon balls.This
Invention prepares the magnetic Nano carbon balls using solvent-thermal method.
Background technique
Fe3O4It is a kind of excellent magnetic nano-particle, under the action of an external magnetic field, can be realized easily positioning, separation
Deng.However, the partial size due to magnetic nano-particle is small, specific surface energy is big and particle between existing dipolar magnetic interaction,
It is very easy to occur to reunite and settle, largely limit its application.To solve the above-mentioned problems, other can usually be passed through
Material carrys out coated magnetic nanoparticle.
Compared with other materials, carbon nanomaterial shows higher chemical stability, thermodynamic stability and biofacies
Capacitive etc..Nano carbon balls are widely used as electricity by advantages such as its low-density, stable physicochemical properties and excellent electric conductivity
Pole material, hydrogen storage material, adsorbent material etc..By Nano carbon balls and Fe3O4The magnetic microsphere of compound preparation is in wastewater treatment, oil product
The fields such as desulfurization significant effect.
The method for preparing magnetic Nano carbon balls at present mainly includes arc discharge method, chemical vapour deposition technique, pyrolysismethod, molten
Agent thermal method etc..But these methods are typically necessary higher temperature, complicated preparation route and longer reaction time, because
This energy consumption is larger, limits its application to a certain extent.
Johnson etc. [Chem Commun, 2004,2442-2443] is using ferric stearate as raw material, under an argon atmosphere
900 DEG C of one step pyrolysis generates the Fe of carbon-encapsulated iron3C nano particle.This method is easy to operate, but required temperature is higher, and product is living
Property is lower.
107032324 A of CN uses hydro-thermal method synthesizing ordered mesoporous carbon nanosphere first, then ferric nitrate and mesoporous carbon are received
The magnetic order mesoporous Nano carbon balls of rice ball ultrasonic mixing preparation.This method complex process needs the operation of two steps that can just prepare magnetic
Property Nano carbon balls.
Qi etc. [J Physi Chem C, 2009,113:15854-15861] prepares Fe using hydro-thermal method first3O4Magnetic
Property nanoparticle, then be scattered in glucose solution, hydro-thermal reaction prepares carbon coating Fe3O4Composite magnetic microballoon, is also deposited
In cumbersome problem.
Wang etc. [J Phys Chem C, 2011,115:11427-11434] be using ferrocene as carbon source and source of iron,
Acetone is solvent, and in the presence of hydrogen peroxide, 210 DEG C of hydro-thermal reaction 48h prepare magnetic Nano carbon balls.Although this method operation letter
Just, a step can be prepared by magnetic Nano carbon balls, but solvent acetone is unfavorable for environmental-friendly, and the reaction time is longer.
Therefore, the magnetic carbon easy to operate, that reaction temperature is lower, the reaction time is shorter, lytic activity is high of one kind is developed to receive
Rice ball preparation method, has important theory and realistic meaning.
Summary of the invention
That present invention aim to address magnetic Nano carbon balls preparation manipulations is cumbersome, the reaction time is long, surface activity is low
The problem of, provide it is a kind of it is easy to operate, reaction temperature is lower, the reaction time is shorter, there is the active magnetic carbon of certain surface to receive
The preparation method of rice ball.
The preparation method of magnetism Nano carbon balls of the present invention is with naphthalene or 1, and 5- dihydroxy naphthlene is carbon source, triblock copolymer
Object PF127 is that surfactant carries out molten in the presence of source of iron ferrocene in the anhydrous ethanol solvent system of Yu Hanyou hydrogen peroxide
Agent thermal response, to prepare the magnetic Nano carbon balls.
Wherein, the effect of the source of iron ferrocene is to confer to the certain magnetism of Nano carbon balls, and dosage is the 2 of carbon source quality
~3 times.
In turn, used surfactant PF127 is a kind of structure directing agent, and effect is to promote product balling-up.Institute
The dosage for stating PF127 is 3~5 times of carbon source quality.
The present invention adds hydrogen peroxide as oxidant, to promote the shape of graphite carbon-coating also in anhydrous ethanol solvent system
At.The additional amount of the hydrogen peroxide meets H2O2Molar ratio with ferrocene is (4~6): 1.
Further, present invention preferably uses the hydrogen peroxide of mass fraction 30%.
Specifically, solvent thermal reaction of the present invention is that airtight heating reaction carries out at 210~220 DEG C.
More specifically, the time of solvent thermal reaction of the present invention is preferably 6~30h.
It is black powder that magnetic Nano carbon balls of the surface rich in hydroxyl, carboxyl functional group, which are prepared, through the above method of the present invention
Body particle coats Fe by carbon-coating3O4Nano particle is constituted, Fe3O4Nano particle diameter is about 10~25nm, magnetic Nano carbon balls
Partial size is about 285~305nm.
Using field emission scanning electron microscope, transmission electron microscope and X-ray diffractometer to magnetic prepared by the present invention
Property Nano carbon balls carry out pattern and structural analysis, it was demonstrated that uniform particle diameter, the sphericity of prepared product are preferable, and have carbon coating
Fe3O4Amorphous carbon structure, there is apparent Fe3O4Diffraction maximum, product have magnetism.
FTIR spectrum analyzer surface functional group analysis is the results show that the magnetic Nano carbon balls surface prepared
With hydroxyl abundant, carboxyl etc., there is certain surface-active.Product thermal stability analysis is the results show that product is arrived at 100 DEG C
Total weight loss rate between 900 DEG C is 37%, better heat stability.
For the present invention with the naphthalene of small molecule or 1,5- dihydroxy naphthlene is carbon source, surfactant PF127, source of iron ferrocene and
Under the collective effect of oxidant hydrogen peroxide, magnetic Nano carbon balls have been prepared in solvent-thermal method.Preparation method of the present invention is at low cost
Honest and clean, reaction temperature is lower, and the reaction time is short, and the magnetic Nano carbon balls purity is high of preparation, chemical stability is good, can be applied to adsorb
The technical fields such as material, catalyst carrier, pharmaceutical intermediate, practicability are wide.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope shape appearance figure of magnetic Nano carbon balls.
Fig. 2 is the transmission electron microscope shape appearance figure of magnetic Nano carbon balls.
Fig. 3 is the X-ray diffraction intensity figure of magnetic Nano carbon balls.
Fig. 4 is the infrared spectrogram of magnetic Nano carbon balls.
Fig. 5 is the thermogravimetric curve figure of magnetic Nano carbon balls.
Specific embodiment
Following embodiments are only the preferred technical solution of the present invention, are not used to carry out any restrictions to the present invention.For
For those skilled in the art, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made
Any modification, equivalent substitution, improvement and etc., should all be included in the protection scope of the present invention.
Embodiment 1.
1,5- dihydroxy naphthlene 0.1g, PF127 0.5g, ferrocene 0.3g are weighed, is added in polytetrafluoroethylcontainer container, then plus
Enter the hydrogen peroxide 1mL of dehydrated alcohol 20mL, mass fraction 30%, is uniformly mixed and obtains mixed solution.
The polytetrafluoroethylcontainer container for filling mixed solution is put into reaction kettle, reaction kettle is sealed, is placed in heating furnace, is risen
Temperature to 220 DEG C of heating are reacted for 24 hours.
After reaction, it is cooled to room temperature, the mixed solution after taking out reaction, 6min is centrifuged with 8000r/min, it is heavy to collect
Starch.
Dehydrated alcohol 30mL is added in sediment, 10min, 8000r/min centrifugation are washed with frequency 20KHz ultrasonic disperse
6min collects sediment.The above washing process is repeated 3 times.
Deionized water 30mL is added into sediment, 10min, 8000r/min centrifugation are washed with frequency 20KHz ultrasonic disperse
6min collects sediment.Above-mentioned washing process is repeated, until centrifuged supernatant is colourless.
It puts the precipitate in vacuum oven, the lower 55 DEG C of dryings of vacuum degree 2Pa for 24 hours, obtain magnetic Nano carbon balls.
Fig. 1 gives the scanning electron microscope shape appearance figure of magnetic Nano carbon balls.As can be seen from the figure prepared magnetic carbon is received
Rice ball sphericity is preferable, and pattern is uniform, and particle size distribution range is relatively narrow, and partial size is in 300nm or so.
From the magnetic Nano carbon balls images of transmissive electron microscope of Fig. 2, it can obviously observe that product is that carbon-coating coats Fe3O4Carbon
Nanosphere has certain magnetism, Fe3O4The partial size of nano particle is about 20nm.
In the magnetic Nano carbon balls X-ray diffraction intensity figure of Fig. 3, there are a wider diffraction within the scope of 10 ° to 30 °
Peak, (002) crystal face of corresponding carbon；There is apparent diffraction at 30.0 °, 35.4 °, 43.0 °, 53.4 °, 57.0 ° and 62.5 °
Peak is respectively belonging to Fe3O4(220), (311), (400), (422), (511), (440) crystal face, illustrate the magnetism being prepared
Nano carbon balls are amorphous carbon structure, and the secondary evidence Nano carbon balls have magnetism.
Fig. 4 is the infrared spectrogram of magnetic Nano carbon balls.585cm-1Place is Fe3O4Fe-O characteristic peak, 1036 cm-1With
1258cm-1Place is C-O stretching vibration peak, 1380cm-1Place is C-H stretching vibration peak, 1627cm-1Place is the flexible vibration of C=O of carboxyl
Dynamic peak, and 3431cm-1Place is the O-H stretching vibration peak of carboxyl.Illustrate that there are hydroxyls on the magnetic Nano carbon balls surface being prepared
Base, carboxyl isoreactivity oxygen-containing functional group have certain hydrophily.
The thermogravimetric curve that magnetic Nano carbon balls are measured under nitrogen atmosphere is as shown in Figure 5.As seen from the figure, the total weightlessness of product
Rate is 37%, the weightlessness between 100 DEG C to 400 DEG C mostly come from Nano carbon balls surface moisture evaporation and some stability it is poor
Functional group decomposition, 400 DEG C to 780 DEG C of weightlessness corresponds to the decomposition and carbonization of oligomer at high temperature on carbon-coating, when
When temperature reaches 800 DEG C, carbothermic reduction reaction occurs, carbon and being largely lost for oxygen cause weight loss to quickly increase.
Embodiment 2.
1,5- dihydroxy naphthlene 0.05g, PF127 0.5g, ferrocene 0.3g are weighed, is added in polytetrafluoroethylcontainer container, then plus
Enter dehydrated alcohol 20mL, 30% hydrogen peroxide 1mL, is uniformly mixed and obtains mixed solution.It is carried out later according to 1 method of embodiment, preparation
Obtain the magnetic Nano carbon balls that partial size is about 300nm.
Embodiment 3.
1,5- dihydroxy naphthlene 0.1g, PF127 0.45g, ferrocene 0.2g are weighed, is added in polytetrafluoroethylcontainer container, then plus
Enter dehydrated alcohol 20mL, 30% hydrogen peroxide 1mL, is uniformly mixed and obtains mixed solution.
The polytetrafluoroethylcontainer container for filling mixed solution is put into reaction kettle, reaction kettle is sealed, is placed in heating furnace, is risen
6h is reacted in temperature to 220 DEG C of heating.It is carried out later according to 1 method of embodiment, the magnetic carbon nanometer that partial size is about 180nm is prepared
Ball.
Embodiment 4.
1,5- dihydroxy naphthlene 0.08g, PF127 0.4g, ferrocene 0.25g are weighed, is added in polytetrafluoroethylcontainer container, then
Dehydrated alcohol 20mL, 30% hydrogen peroxide 0.8mL is added, is uniformly mixed and obtains mixed solution.
The polytetrafluoroethylcontainer container for filling mixed solution is put into reaction kettle, reaction kettle is sealed, is placed in heating furnace, is risen
12h is reacted in temperature to 220 DEG C of heating.It is carried out later according to 1 method of embodiment, the magnetic carbon that partial size is about 220nm is prepared and receives
Rice ball.
Embodiment 5.
Naphthalene 0.07g, PF127 0.4g, ferrocene 0.25g are weighed, is added in polytetrafluoroethylcontainer container, adds anhydrous second
Alcohol 20mL, 30% hydrogen peroxide 0.7mL are uniformly mixed and obtain mixed solution.
The polytetrafluoroethylcontainer container for filling mixed solution is put into reaction kettle, reaction kettle is sealed, is placed in heating furnace, is risen
20h is reacted in temperature to 220 DEG C of heating.It is carried out later according to 1 method of embodiment, the magnetic carbon that partial size is about 200nm is prepared and receives
Rice ball.
Embodiment 6.
Naphthalene 0.1g, PF127 0.5g, ferrocene 0.3g are weighed, is added in polytetrafluoroethylcontainer container, adds dehydrated alcohol
20mL, 30% hydrogen peroxide 1mL are uniformly mixed and obtain mixed solution.
The polytetrafluoroethylcontainer container for filling mixed solution is put into reaction kettle, reaction kettle is sealed, is placed in heating furnace, is risen
Temperature to 220 DEG C of heating are reacted for 24 hours.It is carried out later according to 1 method of embodiment, the magnetic carbon that partial size is about 225nm is prepared and receives
Rice ball.
Claims (7)
1. a kind of preparation method of magnetism Nano carbon balls, is with naphthalene or 1,5- dihydroxy naphthlene is carbon source, triblock copolymer PF127
For surfactant, it is anti-that solvent heat is carried out in the presence of source of iron ferrocene, in the anhydrous ethanol solvent system of Yu Hanyou hydrogen peroxide
It answers, to prepare the magnetic Nano carbon balls.
2. the preparation method of magnetism Nano carbon balls according to claim 1, it is characterized in that the dosage of the source of iron ferrocene
It is 2~3 times of carbon source quality.
3. the preparation method of magnetism Nano carbon balls according to claim 1, it is characterized in that the dosage of the PF127 is carbon source
3~5 times of quality.
4. the preparation method of magnetism Nano carbon balls according to claim 1, it is characterized in that according to H2O2With mole of ferrocene
Than for (4~6): 1, hydrogen peroxide is added in the anhydrous ethanol solvent system.
5. the preparation method of magnetism Nano carbon balls according to claim 1, it is characterized in that the solvent thermal reaction is 210
Airtight heating reaction carries out at~220 DEG C.
6. the preparation method of magnetism Nano carbon balls according to claim 1, it is characterized in that the time of the solvent thermal reaction
For 6~30h.
7. the magnetic Nano carbon balls that preparation method described in claim 1 is prepared, coat Fe by carbon-coating3O4Nano particle is constituted,
The Fe3O410~25nm of nano particle diameter, 285~305nm of magnetic Nano carbon balls partial size.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114291811A (en) * | 2021-12-29 | 2022-04-08 | 山西大学 | Simple carbon material magnetizing method |
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| CN114291811A (en) * | 2021-12-29 | 2022-04-08 | 山西大学 | Simple carbon material magnetizing method |
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