CN104576027B - Quick preparation method of core-shell magnetic carbon microspheres - Google Patents
Quick preparation method of core-shell magnetic carbon microspheres Download PDFInfo
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- CN104576027B CN104576027B CN201410842124.4A CN201410842124A CN104576027B CN 104576027 B CN104576027 B CN 104576027B CN 201410842124 A CN201410842124 A CN 201410842124A CN 104576027 B CN104576027 B CN 104576027B
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Abstract
The invention relates to a quick preparation method of core-shell magnetic carbon microspheres and aims to solve the problem that carbon microspheres easily aggregate. According to the method, glucose is used as a carbon source, ferrous gluconate is used as an iron source, cetyl trimethyl ammonium bromide is used as surfactant, the ferrous gluconate is generated into iron compound by hydrothermal synthesis, the glucose is generated into carbon microspheres covering iron cores, core-shell carbon microspheres are formed and made into Fe3O4 cored magnetic microspheres by high-temperature calcining. The method is advanced and quick, data are accurate and detailed, the particle size of the magnetic carbon microspheres is not greater than 600 nm, product purity is up to 98%, the product is ferromagnetic and is applicable to various industrial fields, and the method is ideal.
Description
Technical field
The present invention relates to a kind of fast preparation method of core-shell type magnetic carbosphere, belong to the technology of material with carbon element preparation and application
Field.
Background technology
Carbosphere, abbreviation cmss, there is the architectural feature of uniqueness and excellent physical and chemical performance, as good in heat stability,
Chemical stability is good, has excellent conduction, heat conductivility.
The preparation method of carbosphere mainly have chemical vapour deposition technique, arc discharge method, template, solid-phase pyrolysis, from
Beamlet cosputtering method and hydrothermal synthesis method；The temperature and pressure that hydrothermal synthesis method needs is relatively low, and condition is relatively mild, and carbon source
Wide material sources, preparation cost are low, product purity is high, building-up process is simple, safety non-toxic, environmental protection, be a kind of superior conjunction
One-tenth method；With glucose as carbon source, monodispersed carbosphere can be prepared by hydrothermal synthesis method, using glucose hydrothermal carbonization
The feature of balling-up, metallic can be coated on inside carbosphere, form nucleocapsid structure；Can be prepared with core by stepwise synthesis
The magnetic carbosphere of shell structure, but need before the synthesis to carry out surface modification to magnetic nano-particle, increased preparation process
Complexity and difficulties；Composite is prepared for core with magnetic material and can give composite magnetic responsiveness, made by externally-applied magnetic field
It is rapidly separated with can achieve, is widely used as separation material and carrier, have in biomedical, cytology and separation engineering field
Using value well；The magnetic carbosphere of hydrothermal synthesis method preparation is, in hydrothermal reaction process, magnetic particle is coated on carbon
In layer, so both can stop the reunion between magnetic-particle, also can protect metallic particles from external environment influence, magnetic
Oxygen-containing functional group is contained on carbosphere surface, can make composite with other ionic interactions, expand the application model of material
Enclose.
At present, the preparation process of magnetic carbosphere is longer, and magnetic behavior is weaker, there is more drawback, need into
One step inquires into research
Content of the invention
Goal of the invention
The purpose of the present invention is the situation for background technology, with glucose as carbon source, Ferrous gluconate as source of iron, ten
Six alkyl trimethyl ammonium bromides are surfactant, through Hydrothermal Synthesiss, high-temperature calcination carbonization, quickly make magnetic carbosphere, with
Increase substantially preparation speed and the product property of magnetic carbosphere.
Technical scheme
The present invention use chemical substance material be: glucose, Ferrous gluconate, cetyl trimethylammonium bromide,
Dehydrated alcohol, deionized water, nitrogen, it is as follows that it prepares consumption: with gram, milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) prepare D/W
Weigh glucose 3.567g ± 0.001g, measure deionized water 30ml ± 0.1ml, add in beaker, stir 5min,
Become the D/W of 0.6mol/l；
(2) prepare cetyl trimethylammonium bromide aqueous solution
Weigh cetyl trimethylammonium bromide 1.2g ± 0.001g, measure deionized water 30ml ± 0.1ml, add beaker
In, beaker is placed in cleansing bath tub, stirs 10min at 50 DEG C of water bath with thermostatic control, become the cetyl trimethyl of 0.1098mol/l
Bromination aqueous ammonium；
(3) Hydrothermal Synthesiss preparation Core-shell type carbon microspheres
The preparation of Core-shell type carbon microspheres is carried out in reactor, is under air-tight state, heating, water in heating furnace
Complete during thermal synthesis；
1. dispensing, measures D/W 30ml ± 0.1ml, and cetyl trimethylammonium bromide aqueous solution 30ml ±
0.1ml, weighs Ferrous gluconate 0.3g ± 0.001g, adds in polytetrafluoroethylcontainer container, stirs 30min, becomes mixed liquor；
2. the polytetrafluoroethylcontainer container filling mixed liquor is placed in reactor, and airtight；
3. reactor is placed in heating furnace, and airtight；
4. open heating furnace, 170 DEG C ± 2 DEG C of heating-up temperature, heat time heating time 12h ± 10min；
In reactor, mixed liquor will carry out hydrothermal synthesis reaction in heating process, generate the chemical combination of hud typed carbon-encapsulated iron
Thing；
Hydrothermal synthesis reaction equation is as follows:
In formula: c18h32o19Fe@c: the compound of hud typed carbon-encapsulated iron
5., after hydrothermal synthesis reaction, stop heating, make reactor cool to 25 DEG C with the furnace；
6. after cooling down, blow-on, drive kettle, take out polytetrafluoroethylcontainer container and its interior reactant liquor；
(4) centrifugation
Place reaction liquid in the centrifugal separating tube of centrifugal separator, be centrifuged, separate rotating speed 7000r/min,
Disengaging time 20min；Retain precipitate after separating, discard waste liquid；
(5) washes of absolute alcohol, centrifugation
Put the precipitate in beaker, add dehydrated alcohol 200ml, stirring and washing 20min, become mixed liquor；
Mixed liquor is placed in the separating pipe of centrifugal separator and carries out separating, separate rotating speed 7000r/min, disengaging time
20min；
Retain precipitate after separating, discard cleanout fluid；
(6) deionized water wash, centrifugation
Put the precipitate in beaker, add deionized water 200ml, stirring and washing 30min, become mixed liquor；
Mixed liquor is placed in the separating pipe of centrifugal separator and carries out separating, separate rotating speed 7000r/min, disengaging time
30min；
Retain precipitate after separating, discard cleaning mixture；
(7) it is vacuum dried
Put the precipitate in quartz container, be subsequently placed in vacuum drying oven and be dried, 50 DEG C of baking temperature, vacuum
0.09mpa, drying time, 720min, became Core-shell type carbon microspheres after being dried；
(8) core-shell type magnetic carbosphere is prepared in calcining
The calcining of Core-shell type carbon microspheres is carried out in vacuum calcining stove, is in high-temperature heating, completes under nitrogen protection
's；
1. Core-shell type carbon microspheres are placed in quartz container, are subsequently placed in vacuum calcining stove, and airtight；
2. open vacuum calcining stove vacuum pump, extract furnace air, make pressure in stove reach 0.1mpa；
3. nitrogen, nitrogen input speed 100cm are inputted into vacuum calcining stove3/ min, makes pressure in stove be constantly maintained at
0.5mpa；
4. open vacuum calcining stove internal heater, carry out heating and calcining, 800 DEG C ± 5 DEG C of calcining heat, calcination time
120min；
Hud typed magnetic carbon microsphere is become after calcining；
Calcination reaction formula is as follows:
(9) grind, sieve
Magnetic carbosphere agate mortar after calcining, pestle are ground, are then sieved with 600 eye mesh screens, grind,
Sieve and be repeated；
Grind, sieve after, magnetic carbon microspherulite diameter≤600nm；
(10) detection, analysis, sign
The pattern of the magnetic carbosphere of preparation, color and luster, Chemical Physics performance are carried out detecting, analyze, characterize；
Carry out morphology analysis with field emission scanning electron microscope；
Carry out crystal structure analyses with x-ray diffraction instrument；
Carry out magnetometric analysis with vibration gaussmeter；
Conclusion: magnetic carbosphere is black powder, particle diameter≤600nm, magnetic behavior is ferromagnetism, product purity
98%；
(11) product storage
The magnetic carbosphere of preparation is stored in the glass container of amber transparent, airtight keeps in Dark Place, moistureproof, anti-
Shine, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, is situation about easily reuniting for carbosphere, using Portugal
Grape sugar is carbon source, and Ferrous gluconate is source of iron, and cetyl trimethylammonium bromide is surfactant, through Hydrothermal Synthesiss, Portugal
The ferrous compound generating ferrum of grape saccharic acid, glucose generates carbosphere, and coats ferrum core, forms Core-shell type carbon microspheres, through high temperature
Calcining, makes magnetic carbosphere, this preparation method technique is advanced, quick, and data is accurately full and accurate, and magnetic carbon microspherulite diameter≤
600nm, product purity reaches 98%, and magnetic behavior is ferromagnetism, can apply in multiple industrial circles, be very good magnetic carbon
The fast preparation method of microsphere.
Brief description
Fig. 1, Hydrothermal Synthesiss prepare Core-shell type carbon microspheres state diagram
Fig. 2, core-shell type magnetic carbosphere state diagram is prepared in calcining
Fig. 3, core-shell type magnetic carbosphere shape appearance figure
Fig. 4, core-shell type magnetic carbosphere diffracted intensity collection of illustrative plates
Fig. 5, core-shell type magnetic carbosphere magnetic property collection of illustrative plates
Shown in figure, list of numerals is as follows:
1st, heating furnace, the 2, first electric cabinet, 3, bell, the 4, first display screen, the 5, first display lamp, the 6, first power supply is opened
Close, the 7, first heating temperature control, 8, first heat time heating time controller, the 9, first workbench, 10, reactor, 11, kettle cover,
12nd, polytetrafluoroethylcontainer container, 13, mixed liquor, the 14, second electric cabinet, 15, second display screen, the 16, second display lamp, 17, second
On and off switch, the 18, second heating temperature control, 19, second heat time heating time controller, 20, controller for vacuum pump, 21, vacuum
Calcining furnace, 22, furnace chamber, the 23, second workbench, 24, quartz container, 25 Core-shell type carbon microspheres, 26, pipe valve of giving vent to anger, 27, vacuum
Pump, 28, vacuum valve, 29, vacuum tube, 30, nitrogen cylinder, 31, nitrogen valve, 32, nitrogen tube, 33, nitrogen.
Specific embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, it is Hydrothermal Synthesiss preparation Core-shell type carbon microspheres state diagram, each portion position is correct, proportioning according to quantity, sequentially
Operation.
The value of the chemical substance that preparation uses is to determine by the scope pre-setting, with gram, milliliter, centimetre3For meter
Amount unit.
Hydrothermal Synthesiss preparation Core-shell type carbon microspheres are carried out in reactor, are heating, Hydrothermal Synthesiss in heating furnace
During complete；
Heating furnace is vertical, is the first electric cabinet 2 in the bottom of heating furnace 1, top is bell 3, in heating furnace 1 inner bottom part
For the first workbench 9, put reactor 10 on the first workbench 9 top, in reactor 10, put polytetrafluoroethylcontainer container 12, gather
It is mixed liquor 13 in tetrafluoroethene container 12, and airtight by kettle cover 11；First display screen 4, first is provided with the first electric cabinet 2
Display lamp 5, the first on and off switch 6, the first heating temperature control 7, first heat time heating time controller 8.
Shown in Fig. 2, prepare core-shell type magnetic carbosphere state diagram for calcining, each portion position is correct, sequentially operates.
The calcining of Core-shell type carbon microspheres is carried out in vacuum calcining stove, is to complete under high-temperature heating, nitrogen protection
's；
Vacuum calcining stove is vertical, is the second electric cabinet 14 in the bottom of vacuum calcining stove 21；In vacuum calcining stove 21
Portion is furnace chamber 22, is provided with the second workbench 23 in the inner bottom part of furnace chamber 22, puts quartz container 24 on the second workbench 23,
It is Core-shell type carbon microspheres 25 in quartz container 24, by nitrogen 33 filling in furnace chamber 22；It is provided with the upper right quarter of vacuum calcining stove 21
Give vent to anger pipe valve 26；It is provided with nitrogen cylinder 30 in the left part of vacuum calcining stove 21, nitrogen cylinder 30 top is provided with nitrogen valve 31, nitrogen tube
32, and input nitrogen 33 into furnace chamber 22；It is provided with vacuum pump 27 in the right lower quadrant of vacuum calcining stove 21, vacuum pump 27 top is passed through
Vacuum valve 28, vacuum tube 29 are connected with furnace chamber 22；Second electric cabinet 14 is provided with second display screen 15, the second display lamp 16,
Second source switch the 17, second heating temperature control 18, second heat time heating time controller 19, controller for vacuum pump 20.
Shown in Fig. 3, it is core-shell type magnetic carbosphere shape appearance figure, as illustrated, magnetic carbosphere is spherical powder granule, point
Scattered property is good, even particle size distribution, and particle diameter≤600nm, in irregular stacking.
Shown in Fig. 4, it is core-shell type magnetic carbosphere diffracted intensity collection of illustrative plates, as seen from the figure, does not go out in the product before calcining
The diffraction maximum of the oxide of existing ferroso-ferric oxide and ferrum, after calcining carbonization treatment, xrd spectrogram occurs in that fe3o4Diffraction
Peak, the degree of graphitization of carbon improves.
Shown in Fig. 5, it is core-shell type magnetic carbosphere magnetic property collection of illustrative plates, as seen from the figure, product assumes ferromagnetism, saturated magnetization
Rate is 2.0emu/g.
Claims (3)
1. a kind of fast preparation method of core-shell type magnetic carbosphere it is characterised in that: the chemical substance material of use is: Fructus Vitis viniferae
Sugar, Ferrous gluconate, cetyl trimethylammonium bromide, dehydrated alcohol, deionized water, nitrogen, it is as follows that it prepares consumption: with
Gram, milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) prepare D/W
Weigh glucose 3.567g ± 0.001g, measure deionized water 30ml ± 0.1ml, add in beaker, stir 5min, become
The D/W of 0.6mol/l；
(2) prepare cetyl trimethylammonium bromide aqueous solution
Weigh cetyl trimethylammonium bromide 1.2g ± 0.001g, measure deionized water 30ml ± 0.1ml, add in beaker,
Beaker is placed in cleansing bath tub, stirs 10min at 50 DEG C of water bath with thermostatic control, become the cetyl trimethyl bromine of 0.1098mol/l
Change aqueous ammonium；
(3) Hydrothermal Synthesiss preparation Core-shell type carbon microspheres
The preparation of Core-shell type carbon microspheres is carried out in reactor, is under air-tight state, and in heating furnace, heating, hydro-thermal are closed
Complete during one-tenth；
1. dispensing, measures D/W 30ml ± 0.1ml, and cetyl trimethylammonium bromide aqueous solution 30ml ±
0.1ml, weighs Ferrous gluconate 0.3g ± 0.001g, adds in polytetrafluoroethylcontainer container, stirs 30min, becomes mixed liquor；
2. the polytetrafluoroethylcontainer container filling mixed liquor is placed in reactor, and airtight；
3. reactor is placed in heating furnace, and airtight；
4. open heating furnace, 170 DEG C ± 2 DEG C of heating-up temperature, heat time heating time 12h ± 10min；
In reactor, mixed liquor will carry out hydrothermal synthesis reaction in heating process, generate the compound of hud typed carbon-encapsulated iron；
Hydrothermal synthesis reaction equation is as follows:
In formula: c18h32o19Fe@c: the compound of hud typed carbon-encapsulated iron
5., after hydrothermal synthesis reaction, stop heating, make reactor cool to 25 DEG C with the furnace；
6. after cooling down, blow-on, drive kettle, take out polytetrafluoroethylcontainer container and its interior reactant liquor；
(4) centrifugation
Place reaction liquid in the centrifugal separating tube of centrifugal separator, be centrifuged, separate rotating speed 7000r/min, separate
Time 20min；Retain precipitate after separating, discard waste liquid；
(5) washes of absolute alcohol, centrifugation
Put the precipitate in beaker, add dehydrated alcohol 200ml, stirring and washing 20min, become mixed liquor；
Mixed liquor is placed in the separating pipe of centrifugal separator and carries out separating, separate rotating speed 7000r/min, disengaging time 20min；
Retain precipitate after separating, discard cleanout fluid；
(6) deionized water wash, centrifugation
Put the precipitate in beaker, add deionized water 200ml, stirring and washing 30min, become mixed liquor；
Mixed liquor is placed in the separating pipe of centrifugal separator and carries out separating, separate rotating speed 7000r/min, disengaging time 30min；
Retain precipitate after separating, discard cleaning mixture；
(7) it is vacuum dried
Put the precipitate in quartz container, be subsequently placed in vacuum drying oven and be dried, 50 DEG C of baking temperature, vacuum
0.09mpa, drying time, 720min, became Core-shell type carbon microspheres after being dried；
(8) calcining of Core-shell type carbon microspheres
The calcining of Core-shell type carbon microspheres is carried out in vacuum calcining stove, completes under high-temperature heating, nitrogen protection；
1. Core-shell type carbon microspheres are placed in quartz container, are subsequently placed in vacuum calcining stove, and airtight；
2. open vacuum calcining stove vacuum pump, extract furnace air, make pressure in stove reach 0.1mpa；
3. nitrogen, nitrogen input speed 100cm are inputted into vacuum calcining stove3/ min, makes pressure in stove be constantly maintained at
0.5mpa；
4. open vacuum calcining stove internal heater, carry out heating and calcining, 800 DEG C ± 5 DEG C of calcining heat, calcination time 120min；
Hud typed magnetic carbon microsphere is become after calcining；
Calcination reaction formula is as follows:
(9) grind, sieve
Magnetic carbosphere agate mortar after calcining, pestle are ground, are then sieved with 600 eye mesh screens, grind, sieve
It is repeated；
Grind, sieve after, magnetic carbon microspherulite diameter≤600nm；
(10) detection, analysis, sign
The pattern of the magnetic carbosphere of preparation, color and luster, Chemical Physics performance are carried out detecting, analyze, characterize；
Carry out morphology analysis with field emission scanning electron microscope；
Carry out crystal structure analyses with x-ray diffraction instrument；
Carry out magnetometric analysis with vibration gaussmeter；
Conclusion: magnetic carbosphere is black powder, particle diameter≤600nm, magnetic behavior is ferromagnetism, product purity 98%；
(11) product storage
The magnetic carbosphere of preparation is stored in the glass container of amber transparent, airtight keeps in Dark Place, moistureproof, sun-proof,
Anti- acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
2. a kind of core-shell type magnetic carbosphere according to claim 1 fast preparation method it is characterised in that: hydro-thermal close
Become preparation Core-shell type carbon microspheres to carry out in reactor, in heating furnace heating, complete during Hydrothermal Synthesiss；
Heating furnace is vertical, is the first electric cabinet (2) in the bottom of heating furnace (1), is bell (3) on heating furnace top, in heating furnace
(1) inner bottom part is the first workbench (9), puts to put in reactor (10), reactor (10) on the first workbench (9) top and gathers
Tetrafluoroethene container (12), is mixed liquor (13) in polytetrafluoroethylcontainer container (12), and airtight by kettle cover (11)；Automatically controlled first
Case (2) be provided with the first display screen (4), the first display lamp (5), the first on and off switch (6), the first heating temperature control (7),
First controller heat time heating time (8).
3. a kind of core-shell type magnetic carbosphere according to claim 1 fast preparation method it is characterised in that: hud typed
The calcining of carbosphere is carried out in vacuum calcining stove, completes under high-temperature heating, nitrogen protection；
Vacuum calcining stove is vertical, is the second electric cabinet (14) in the bottom of vacuum calcining stove (21)；In vacuum calcining stove (21)
Internal is furnace chamber (22), is provided with the second workbench (23) in the inner bottom part of furnace chamber (22), in the second workbench (23) upper storing stone
English container (24), is Core-shell type carbon microspheres (25), by nitrogen (33) filling in furnace chamber (22) in quartz container (24)；In vacuum
The upper right quarter of calcining furnace (21) is provided with pipe valve of giving vent to anger (26)；It is provided with nitrogen cylinder (30), nitrogen in the left part of vacuum calcining stove (21)
Bottle (30) top is provided with nitrogen valve (31), nitrogen tube (32), and input nitrogen (33) into furnace chamber (22)；In vacuum calcining stove
(21) right lower quadrant is provided with vacuum pump (27), and vacuum valve (28), vacuum tube (29) and furnace chamber (22) are passed through in vacuum pump (27) top
Connection；Second electric cabinet (14) is provided with second display screen (15), the second display lamp (16), second source switch (17), the
Two heating temperature control (18), the second controller heat time heating time (19), controller for vacuum pump (20).
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| CN107185547B (en) * | 2017-06-07 | 2020-04-14 | 齐齐哈尔大学 | C/Fe-FeVO4Composite photocatalyst and preparation method and application thereof |
| CN113680291B (en) * | 2021-09-09 | 2023-12-01 | 吉林农业大学 | Preparation method of paramagnetic metal oxide/spinel/carbon composite microsphere |
| CN114130392A (en) * | 2021-11-29 | 2022-03-04 | 哈尔滨工业大学 | Preparation method of iron-carbon-based material, product and application thereof |
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| FR1378803A (en) * | 1959-09-30 | 1964-11-20 | Merck & Co Inc | Iron-based, coated and tasteless compositions |
| CN101640088A (en) * | 2009-07-21 | 2010-02-03 | 江南大学 | Precipitation-oxidation method for preparing glucan ferroferric oxide magnetic nano particle and application thereof |
| CN101941077A (en) * | 2010-09-02 | 2011-01-12 | 太原理工大学 | Method for preparing magnetic metal iron-encapsulated fullerene carbon spheres |
| CN104001474A (en) * | 2014-05-20 | 2014-08-27 | 江苏大学 | Carbon-coated ferroferric oxide core-shell nano particle and preparation method thereof |
| CN104117329A (en) * | 2014-07-21 | 2014-10-29 | 太原理工大学 | Preparation method of carbon-coated ferroferric oxide magnetic microspheres |
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2014
- 2014-12-30 CN CN201410842124.4A patent/CN104576027B/en not_active Expired - Fee Related
Patent Citations (5)
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|---|---|---|---|---|
| FR1378803A (en) * | 1959-09-30 | 1964-11-20 | Merck & Co Inc | Iron-based, coated and tasteless compositions |
| CN101640088A (en) * | 2009-07-21 | 2010-02-03 | 江南大学 | Precipitation-oxidation method for preparing glucan ferroferric oxide magnetic nano particle and application thereof |
| CN101941077A (en) * | 2010-09-02 | 2011-01-12 | 太原理工大学 | Method for preparing magnetic metal iron-encapsulated fullerene carbon spheres |
| CN104001474A (en) * | 2014-05-20 | 2014-08-27 | 江苏大学 | Carbon-coated ferroferric oxide core-shell nano particle and preparation method thereof |
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