CN105819424A - Preparation method of porous carbon material - Google Patents
Preparation method of porous carbon material Download PDFInfo
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- CN105819424A CN105819424A CN201610160614.5A CN201610160614A CN105819424A CN 105819424 A CN105819424 A CN 105819424A CN 201610160614 A CN201610160614 A CN 201610160614A CN 105819424 A CN105819424 A CN 105819424A
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- 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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- 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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Abstract
The invention relates to a preparation method of a porous carbon material. Based on the requirements on performance of capacitor electrode materials, (low boiling point metal) zinc hydroxide and 2-ethyl imidazole are used to form a metal-organic porous material, which is taken as the precursor; nitrogen gas is taken as the inert protective gas, and the porous carbon material is prepared by the following steps: solution preparation, ultrasonic dispersion, suction filtration, washing, vacuum drying, and vacuum high temperature sintering. The preparation method has the advantages of advanced technology, precise data, and high product purity, which can reach 98.3%. The porous carbon material is black powder, the particle is in a prism shape, the particle size of powder is not larger than 190 nm, the generated porous carbon material is a hexagonal graphite phase and has two channels (microporous channel and mesoporous channel); and the preparation method is an advanced method for preparing porous carbon materials, which can be applied to capacitor electrodes.
Description
Technical field
The present invention relates to the preparation method of a kind of porous carbon materials, belong to material with carbon element preparation and the technical field of application.
Background technology
Capacitor is a kind of energy storage device, the critical piece of capacitor is electrode, the performance of electrode material has important impact to the chemical property of energy storage device, and the electrode material specific surface area of current capacitor is little, porosity is low, the life-span is short, is extremely difficult to the needs of high-side capacitance device.
Low boiling metal has the advantage that coordination ability is strong, metal-organic porous material can be constructed with gas chromatography coordination, doing presoma to use, metal-organic porous material thermally decomposes available porous carbon materials under an inert atmosphere, can be effectively maintained pore structure and the pattern of metal-organic porous material；Selfdecomposition by metal-organic porous material can omit the process of removing template；Construct the Organic substance of metal-organic porous material rich in substantial amounts of carbon, it is not necessary to additionally add carbon source.
It is coordinated the metal-organic porous material constructed as presoma with low boiling metal and Organic substance, porous carbon materials can be prepared by thermal decomposition, firing rate, noble gas flow velocity and the impact of heating and thermal insulation it is vulnerable in building-up process, its specific surface area, pore size, shape, distribution all will be affected by the biggest, thus affect the performance of electrode for capacitors, this synthetic technology there is also bigger drawback, also in scientific research.
Summary of the invention
Goal of the invention
It is an object of the invention to the situation for background technology; using low boiling metallic hydrogen zinc oxide and 2-ethyl imidazol(e) to construct metal-organic porous material as precursor species, nitrogen is inert protective gas; be formulated solution, ultrasound wave dispersion, sucking filtration, wash, be vacuum dried, vacuum-sintering; make porous carbon materials, to be preferably applied in electrode for capacitors.
Technical scheme
The chemical substance material that the present invention uses is: zinc hydroxide, 2-ethyl imidazol(e), ammonia, thiacyclohexane, absolute methanol, nitrogen, and it is as follows that it prepares consumption: with gram, milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) selected chemical substance material
The chemical substance material using preparation to carry out selected, and carries out quality purity, concentration control:
(2) preparation zinc hydroxide ammonia spirit
Weigh zinc hydroxide 0.4g ± 0.0001g, measure ammonia 80mL ± 0.0001mL, join in beaker, stir 10min, become the zinc hydroxide ammonia spirit of 0.05mol/L；
(3) preparation 2-ethyl imidazol(e), thiacyclohexane, absolute methanol mixed solution
Weigh 2-ethyl imidazol(e) 0.76g ± 0.0001g, measure thiacyclohexane 4mL ± 0.0001mL, absolute methanol 60mL ± 0.0001mL, add in another beaker, become mixed liquor；
The beaker filling mixed liquor is placed in ultrasound wave separating apparatus, carries out ultrasonic disperse, ultrasonic frequency 50KHz, ultrasonic disperse time 10min, become the mixed solution of 0.17mol/L；
(4) zinc hydroxide synthesizes metal-organic porous material with 2-ethyl imidazol(e)
In ultrasound wave separating apparatus, put Dropping funnel on the beaker top filling mixed solution；
The zinc hydroxide ammonia spirit of configuration is placed in Dropping funnel, drips, rate of addition 4mL/min；
Ultrasonic disperse, ultrasonic frequency 50KHz, ultrasonic disperse time 50min is carried out during dropping；
Zinc hydroxide will occur chemical reaction during 2-ethyl imidazol(e) synthesis metal-organic porous material, and reaction equation is as follows:
In formula: Zn (C5N2H7)2: 2-ethyl imidazol(e) closes zinc
H2O: water
Mixed solution is become after synthesis；
(5) sucking filtration
Mixed solution after synthesis is placed in the buchner funnel of bottle,suction, carries out sucking filtration with three layers of middling speed qualitative filter paper, retain filter cake, discard waste liquid；
(6) washing, sucking filtration
Filter cake is placed in beaker, adds dehydrated alcohol 100mL, agitator treating 5min；
Then carry out sucking filtration with three layers of middling speed qualitative filter paper, retain filter cake, discard cleaning mixture；
Washing, sucking filtration repeat 5 times；
(7) vacuum drying
Washing, filter cake after sucking filtration are placed in quartz container, are subsequently placed in vacuum drying oven and are dried, baking temperature 150 DEG C, vacuum 6Pa, drying time 360min；
Dried is metal-organic porous material；
(8) vacuum-sintering
The sintering of metal-organic porous material is carried out in vacuum sintering furnace, completes under evacuation, defeated nitrogen, Frequency Induction Heating state；
1. vacuum sintering furnace is cleared up, and by nitrogen flooding except harmful substance in stove, clean in making stove；
2. metal-organic porous material is placed in quartz container, is subsequently placed on the workbench in vacuum sintering furnace, and airtight；
3. opening vacuum pump, extract furnace air, in making stove, pressure reaches 6Pa；
4. open nitrogen cylinder, in stove, input nitrogen, nitrogen input speed 100cm3/ min, in making stove, invariablenes pressure of liquid is at 0.1MPa；
5. medium frequency induction heater, heat-agglomerating, heating-up temperature 1000 DEG C ± 2 DEG C, heating and thermal insulation time 300min are opened；
6. stop heating after sintering, cool to 25 DEG C with the furnace；
It it is porous carbon materials after cooling；
(9) detect, analyze, characterize
Carry out the pattern of the porous carbon materials of preparation, composition, Chemical Physics performance, mechanical property detecting, analyze, characterize；
1. porous carbon materials morphology analysis is carried out by scanning electron microscope；
2. porous carbon materials material phase analysis is carried out with powder x-ray diffraction；
3. porous carbon materials material phase analysis is carried out with Raman spectrometer；
4. porous carbon materials specific surface area, pore structure study are carried out with physical adsorption appearance；
Conclusion: porous carbon materials is black prismatic powder body, powder granule diameter≤190nm, and product purity reaches 98.3%, and the porous carbon of generation is six purpose square graphite phases, has micropore and mesoporous two kinds of ducts；
(10) product storage
Being stored in the glass container of amber transparent by the porous carbon materials powder granule of preparation, airtight lucifuge stores, and acid-alkali salt sun-proof, moistureproof, anti-corrodes, storing temperature 20 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, it it is the performance requirement for capacitor electrode material, using low boiling metallic hydrogen zinc oxide and 2-ethyl imidazol(e) to construct metal-organic porous material is precursor species, nitrogen is inert protective gas, it is formulated solution, ultrasound wave disperses, sucking filtration, washing, vacuum drying, vacuum high-temperature sintering, make porous carbon materials, this preparation method technique is advanced, data are the fullest and the most accurate, product purity is good, reach 98.3%, product is black powder, powder granule is prismatic, powder granule diameter≤190nm, the porous carbon generated is six purpose square graphite phases, there are micropore and mesoporous two kinds of ducts, it it is the advanced method preparing porous carbon materials, porous carbon materials can be applied in electrode for capacitors.
Accompanying drawing explanation
Fig. 1. metal-organic porous material sintering state figure
Fig. 2. porous carbon materials shape appearance figure
Fig. 3. porous carbon materials X-ray diffraction intensity collection of illustrative plates
Fig. 4. porous carbon materials Raman spectrogram
Fig. 5. porous carbon materials nitrogen adsorption-desorption isobaric chart
Fig. 6. porous carbon materials graph of pore diameter distribution
Shown in figure, list of numerals is as follows:
1, vacuum sintering furnace, 2, stove seat, 3, bell, 4, furnace chamber, 5, give vent to anger pipe valve, 6, outer water circulating cooling pipe, 7, water intaking valve, 8, outlet valve, 9, medium frequency induction heater, 10, workbench, 11, quartz container, 12, metal-organic porous material, 13, vacuum pump, 14, vacuum valve, 15, vacuum tube, 16, nitrogen cylinder, 17, nitrogen valve, 18, nitrogen tube, 19, nitrogen, 20, display screen, 21, display lamp, 22, on and off switch, 23, heating temperature control, 24, controller for vacuum pump.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, for metal-organic porous material sintering state figure, position, each portion, annexation are wanted correct, are sequentially operated.
The value of the chemical substance that preparation uses is to determine by the scope pre-set, with gram, milliliter, centimetre3For measurement unit.
The sintering of metal-organic porous material is carried out in vacuum sintering furnace, completes under evacuation, defeated nitrogen, Frequency Induction Heating state；
Vacuum sintering furnace 1 is vertical, the bottom of vacuum sintering furnace 1 be stove seat 2, top be bell 3, internal for furnace chamber 4；The outside of vacuum sintering furnace 1 is provided with outer water circulating cooling pipe 6, and outer water circulating cooling pipe 6 connects water intaking valve 7, outlet valve 8 and is connected with external water source；Vacuum sintering furnace 1 inner bottom part is provided with workbench 10, and workbench 10 is put quartz container 11, puts metal-organic porous material 12 in quartz container 11；By nitrogen 19 filling in furnace chamber 4；Right part at vacuum sintering furnace 1 is provided with vacuum pump 13, and vacuum pump 13 top is provided with vacuum valve 14, vacuum tube 15, and connects furnace chamber 4；Left part at vacuum sintering furnace 1 is provided with nitrogen cylinder 16, and nitrogen cylinder 16 top is provided with nitrogen valve 17, nitrogen tube 18, and inputs nitrogen 19 in furnace chamber 4；Stove seat 2 is provided with display screen 20, display lamp 21, on and off switch 22, heating temperature control 23, controller for vacuum pump 24.
Shown in Fig. 2, for porous carbon materials shape appearance figure, shown in figure, porous carbon materials is powder body, and powder granule diameter≤190nm, powder granule has the geometric shape of prismatic, in irregular stacking.
Shown in Fig. 3, for porous carbon materials X-ray diffraction intensity collection of illustrative plates, shown in figure, vertical coordinate is diffracted intensity, and abscissa is the angle of diffraction, and two characteristic peaks of 23 ° and 44 ° are respectively belonging to (002) and (101) interface of six purpose square graphite phases.
Shown in Fig. 4, for porous carbon materials Raman spectrogram, shown in figure, vertical coordinate is intensity, and abscissa is Raman shift, 1349cm-1And 1591cm-1The characteristic peak of two wave numbers is respectively belonging to D-peak and the G-peak of material with carbon element, illustrates that sintered product is material with carbon element.
Shown in Fig. 5, nitrogen adsorption-desorption isobaric chart for porous carbon materials, shown in figure, vertical coordinate is GAS ABSORPTION amount, abscissa is relative pressure, belonging to I type and IV type mixing and absorption isobar, illustrate that porous carbon materials exists micropore and mesoporous two kinds of pore diameter ranges, the specific surface area of porous carbon materials is 1946m2/g。
Shown in Fig. 6, for porous carbon materials graph of pore diameter distribution, shown in figure, vertical coordinate is pore volume, and abscissa is aperture, pore size distribution range 0.4nm-10nm.
Claims (2)
1. the preparation method of a porous carbon materials, it is characterised in that: the chemical substance material of use is: hydrogen
Zinc oxide, 2-ethyl imidazol(e), ammonia, thiacyclohexane, absolute methanol, nitrogen, its prepare consumption as follows: with gram,
Milliliter, centimetre3For measurement unit
Preparation method is as follows:
(1) selected chemical substance material
The chemical substance material using preparation to carry out selected, and carries out quality purity, concentration control:
(2) preparation zinc hydroxide ammonia spirit
Weigh zinc hydroxide 0.4g ± 0.0001g, measure ammonia 80mL ± 0.0001mL, join beaker
In, stir 10min, become the zinc hydroxide ammonia spirit of 0.05mol/L；
(3) preparation 2-ethyl imidazol(e), thiacyclohexane, absolute methanol mixed solution
Weigh 2-ethyl imidazol(e) 0.76g ± 0.0001g, measure thiacyclohexane 4mL ± 0.0001mL, without water beetle
Alcohol 60mL ± 0.0001mL, adds in another beaker, becomes mixed liquor；
The beaker filling mixed liquor is placed in ultrasound wave separating apparatus, carries out ultrasonic disperse, ultrasonic frequency 50
KHz, ultrasonic disperse time 10min, become the mixed solution of 0.17mol/L；
(4) zinc hydroxide synthesizes metal-organic porous material with 2-ethyl imidazol(e)
In ultrasound wave separating apparatus, put Dropping funnel on the beaker top filling mixed solution；
The zinc hydroxide ammonia spirit of configuration is placed in Dropping funnel, drips, rate of addition 4
mL/min；
Ultrasonic disperse, ultrasonic frequency 50KHz, ultrasonic disperse time 50min is carried out during dropping；
Zinc hydroxide will occur chemical reaction during 2-ethyl imidazol(e) synthesis metal-organic porous material,
Reaction equation is as follows:
In formula: Zn (C5N2H7)2: 2-ethyl imidazol(e) closes zinc
H2O: water
Mixed solution is become after synthesis；
(5) sucking filtration
Mixed solution after synthesis is placed in the buchner funnel of bottle,suction, carries out with three layers of middling speed qualitative filter paper
Sucking filtration, retains filter cake, discards waste liquid；
(6) washing, sucking filtration
Filter cake is placed in beaker, adds dehydrated alcohol 100mL, agitator treating 5min；
Then carry out sucking filtration with three layers of middling speed qualitative filter paper, retain filter cake, discard cleaning mixture；
Washing, sucking filtration repeat 5 times；
(7) vacuum drying
Filter cake after washing, sucking filtration is placed in quartz container, is subsequently placed in vacuum drying oven and is dried, dry
Dry temperature 150 DEG C, vacuum 6Pa, drying time 360min；
Dried is metal-organic porous material；
(8) vacuum-sintering
The sintering of metal-organic porous material is carried out in vacuum sintering furnace, be evacuation, defeated nitrogen,
Complete under Frequency Induction Heating state；
1. vacuum sintering furnace is cleared up, and by nitrogen flooding except harmful substance in stove, clean in making stove；
2. metal-organic porous material is placed in quartz container, the work being subsequently placed in vacuum sintering furnace
In station and airtight；
3. opening vacuum pump, extract furnace air, in making stove, pressure reaches 6Pa；
4. open nitrogen cylinder, in stove, input nitrogen, nitrogen input speed 100cm3/ min, in making stove
Invariablenes pressure of liquid is at 0.1MPa；
5. medium frequency induction heater, heat-agglomerating, heating-up temperature 1000 DEG C ± 2 DEG C, heating are opened
Temperature retention time 300min；
6. stop heating after sintering, cool to 25 DEG C with the furnace；
It it is porous carbon materials after cooling；
(9) detection is analyzed, and characterizes
Carry out the pattern of the porous carbon materials of preparation, composition, Chemical Physics performance, mechanical property detecting,
Analyze, characterize；
1. porous carbon materials morphology analysis is carried out by scanning electron microscope；
2. porous carbon materials material phase analysis is carried out with powder x-ray diffraction；
3. porous carbon materials material phase analysis is carried out with Raman spectrometer；
4. porous carbon materials specific surface area, pore structure study are carried out with physical adsorption appearance；
Conclusion: porous carbon materials is black prismatic powder body, and powder granule diameter≤190nm, product purity reaches
98.3%, the porous carbon of generation is six purpose square graphite phases, has micropore and mesoporous two kinds of ducts；
(10) product storage
Being stored in the glass container of amber transparent by the porous carbon materials powder granule of preparation, airtight lucifuge is stored up
Depositing, acid-alkali salt sun-proof, moistureproof, anti-corrodes, storing temperature 20 DEG C, relative humidity≤10%.
The preparation method of a kind of porous carbon materials the most according to claim 1, it is characterised in that: porous
The sintering of material with carbon element is carried out in vacuum sintering furnace, is in evacuation, defeated nitrogen, Frequency Induction Heating
Complete under state；Vacuum sintering furnace (1) be the bottom of vertical type vacuum sintering furnace (1) be stove seat (2),
Top is bell (3), internal for furnace chamber (4)；The outside of vacuum sintering furnace (1) is provided with outer water circulating cooling
Pipe (6), outer water circulating cooling pipe (6) connects water intaking valve (7), outlet valve (8) and connects with external water source
Connect；Vacuum sintering furnace (1) inner bottom part is provided with workbench (10), and workbench puts quartz container on (10)
(11), metal-organic porous material (12) is put in quartz container (11)；By nitrogen (19) in furnace chamber (4)
Filling；Right part at vacuum sintering furnace (1) is provided with vacuum pump (13), and vacuum pump (13) top is provided with very
Empty valve (14), vacuum tube (15), and connect furnace chamber (4)；Left part at vacuum sintering furnace (1) is provided with nitrogen
Gas cylinder (16), nitrogen cylinder (16) top is provided with nitrogen valve (17), nitrogen tube (18), and to furnace chamber (4)
Interior input nitrogen (19)；Stove seat (2) is provided with display screen (20), display lamp (21), on and off switch
(22), heating temperature control (23), controller for vacuum pump (24).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115304748A (en) * | 2022-09-02 | 2022-11-08 | 沈阳师范大学 | Preparation method of porous polymer material |
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| CN101604580A (en) * | 2009-04-03 | 2009-12-16 | 中国科学院上海硅酸盐研究所 | Single one step of source compound decomposition method prepares the method for porous carbon electrode material |
| CN103483360A (en) * | 2013-09-09 | 2014-01-01 | 太原理工大学 | Preparation method for metal complex functionalized ZIF-8 (zinc 2-methylimidazolate) material |
| CN104557718A (en) * | 2014-10-30 | 2015-04-29 | 中山大学 | Preparation method and application of RHO zeolite type 2-ethylimidazole zinc porous material |
| CN104916447A (en) * | 2014-03-12 | 2015-09-16 | 中国科学院大连化学物理研究所 | High-rate porous carbon electrode material for super capacitor and preparation method |
| CN105152281A (en) * | 2015-09-10 | 2015-12-16 | 上海大学 | Preparation method of capacitive type desalination electrode prepared from hierarchical porous carbon material with core-shell structure |
| CN105384161A (en) * | 2015-11-23 | 2016-03-09 | 南京航空航天大学 | Preparation method and application of graded porous carbon material |
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2016
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101604580A (en) * | 2009-04-03 | 2009-12-16 | 中国科学院上海硅酸盐研究所 | Single one step of source compound decomposition method prepares the method for porous carbon electrode material |
| CN103483360A (en) * | 2013-09-09 | 2014-01-01 | 太原理工大学 | Preparation method for metal complex functionalized ZIF-8 (zinc 2-methylimidazolate) material |
| CN104916447A (en) * | 2014-03-12 | 2015-09-16 | 中国科学院大连化学物理研究所 | High-rate porous carbon electrode material for super capacitor and preparation method |
| CN104557718A (en) * | 2014-10-30 | 2015-04-29 | 中山大学 | Preparation method and application of RHO zeolite type 2-ethylimidazole zinc porous material |
| CN105152281A (en) * | 2015-09-10 | 2015-12-16 | 上海大学 | Preparation method of capacitive type desalination electrode prepared from hierarchical porous carbon material with core-shell structure |
| CN105384161A (en) * | 2015-11-23 | 2016-03-09 | 南京航空航天大学 | Preparation method and application of graded porous carbon material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115304748A (en) * | 2022-09-02 | 2022-11-08 | 沈阳师范大学 | Preparation method of porous polymer material |
| CN115304748B (en) * | 2022-09-02 | 2023-06-23 | 沈阳师范大学 | Preparation method of porous polymer material |
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