CN106882788A - A kind of preparation method of meso-porous carbon material - Google Patents
A kind of preparation method of meso-porous carbon material Download PDFInfo
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- CN106882788A CN106882788A CN201710223098.0A CN201710223098A CN106882788A CN 106882788 A CN106882788 A CN 106882788A CN 201710223098 A CN201710223098 A CN 201710223098A CN 106882788 A CN106882788 A CN 106882788A
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- C01P2002/00—Crystal-structural characteristics
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention relates to a kind of preparation method of meso-porous carbon material, belong to the technical field of preparation and the application of carbon material；The present invention has obvious advanced compared with background technology, it is with organic molecule as carbon source, with Na-K alloy as reducing agent, with toluene as solvent, through magnetic agitation at room temperature, reaction solution is made, through suction filtration, washing, vacuum drying, meso-porous carbon material is made, this preparation method technique is advanced, and informative data is accurate, prepare speed fast, without high-temperature calcination, product is black powder, with mesopore orbit structure, products collection efficiency is high, up to 75.6%, can be matched with various chemical substances, be the very good method for preparing meso-porous carbon material.
Description
Technical field
The present invention relates to a kind of preparation method of meso-porous carbon material, belong to the technical field of preparation and the application of carbon material.
Background technology
Meso-porous carbon material has good adjustability of structure and stability, is incomparable other materials, mesoporous carbon materials
Material has specific surface area and larger pore volume higher, is widely applied in absorption, catalysis, optics, electricity field.
The synthetic method and process of meso-porous carbon material can directly affect the architectural feature and performance of material, for example template and
The selection of presoma is conclusive influence factor, reaction temperature, solvent, the ratio of reactant, the pH value of reaction system, roasting
Temperature also has important influence.
Template is the element of synthesising mesoporous carbon material, organic precursor and template by self assembly or
The method of nanometer casting forms meso-hole structure.The structure and species of template will influence the pore passage structure of meso-porous carbon material, therefore
The selection of template and using being highly important.
Using organic molecule or polymer as during precursor synthesis carbon material, it is required for greatly in inert atmosphere
Lower high-temperature roasting carbonization, because the chemical substance selected is different, the difference of synthetic parameters, the difference of building-up process, carburizing temperature
From 600 DEG C to 1800 DEG C, gained carbon material Chemical Physics performance difference is larger, it is difficult to meet the requirement of synthetic, makes such
The application of material receives significant limitation.
The content of the invention
To solve the above problems, the purpose of the present invention is, using a kind of new metal reduction synthesis process, to be made with Na-K alloy
Metallic reducing agent, with tetrachloromethane as organic precursor, prepares meso-porous carbon material at ambient temperature, and mesoporous carbon is greatly lowered
The synthesis temperature of material, improves Chemical Physics performance, meso-porous carbon material is more widely used.
To achieve the above object, the present invention uses following technical proposals：A kind of preparation method of meso-porous carbon material, its feature
It is that the chemical substance material needed for the preparation method includes：Metallic sodium, metallic potassium, carbon tetrachloride, toluene, ethanol and go from
Sub- water, preparation method comprises the following steps：
(1) Na-K alloy is prepared：It is 1 according to mass ratio：4 ratio weighs metallic sodium and metallic potassium, 1min is stirred, into sodium
Potassium-sodium alloy；
(2) synthesising mesoporous carbon material：The synthesis of meso-porous carbon material is carried out under nitrogen protection, is in room temperature 25~28
Stir what is completed under conditions of DEG C；
1. hybrid reaction mixture is prepared
It is 1.2 according to mass ratio：1.8 weigh carbon tetrachloride and Na-K alloy is placed in round-bottomed flask, then are added thereto to
Toluene 200mL~300mL, into mixed reaction solution；
2. magnetic agitation is opened, mixing time 10h, mixed reaction solution is reacted, and reaction equation is as follows：
CCl4+ 4Na=4NaCl+C
CCl4+ 4K=4KCl+C
3. after the completion of reacting, stop stirring, add 100~150mL of ethanol；
(3) suction filtration：Reacted mixture is placed in the Buchner funnel of bottle,suction, suction filtration is carried out with miillpore filter, filtered
Remaining product filter cake on film, waste liquid is evacuated in filter flask；
(4) washing, suction filtration：Product cake is placed in beaker, ethanol 100mL, agitator treating 5min is added；By cleaning solution
It is placed in the Buchner funnel of bottle,suction, suction filtration is carried out with miillpore filter, remaining product filter cake on filter membrane, cleaning solution is evacuated to filter flask
In；Washing, suction filtration are carried out 2 times；Product cake is placed in beaker, 100~150mL of deionized water, agitator treating 5min is added；
(5) it is vacuum dried：Product cake after washing is placed in quartz container, being subsequently placed in vacuum drying chamber is carried out
Dry, 55~65 DEG C of drying temperature, 50~60Pa of vacuum, 8~12h of drying time, meso-porous carbon material is after drying；To system
Standby meso-porous carbon material is stored in the glass container of amber transparent, closed to keep in dark place, and waterproof, protection against the tide, sun-proof, anti-soda acid
Salt corrosion, 20 DEG C ± 2 DEG C of storage temperature, relative humidity≤10%.
The beneficial effects of the invention are as follows：
The present invention has obvious advance compared with background technology, is that carbon tetrachloride is carbon source, with Na-K alloy as also
Former agent, with toluene as solvent, through magnetic agitation at room temperature, is made reaction solution, through suction filtration, washing, vacuum drying, is made Jie
Hole carbon material, this preparation method technique is advanced, and informative data is accurate, prepares speed soon, and without high-temperature calcination, product is black powder
End, with mesopore orbit structure, products collection efficiency is high, up to 75.6%, can be matched with various chemical substances, is very good preparation
The method of meso-porous carbon material.
Brief description of the drawings
Fig. 1 is the synthetically prepared state diagram of meso-porous carbon material；
1st, iron clamp, 2, round-bottomed flask, 3, mixing platform, 4, fix bar, 5, magnetic stir bar, 6, plastics plug, 7, agitator
Seat, 8, display screen, 9 indicator lamps, 10 power switches, 11 rotation speed regulating and controlling devices；
Fig. 2 is meso-porous carbon material transmission electron microscope photo；
Fig. 3 is meso-porous carbon material nitrogen adsorption desorption curve figure；
Fig. 4 is meso-porous carbon material Raman spectrogram.
Specific embodiment
With reference to the accompanying drawings, by specific embodiment, the invention will be further described, to more fully understand the present invention.
Embodiment 1
Chemical substance material is：Metallic sodium, metallic potassium, carbon tetrachloride, toluene, ethanol, deionized water, its combination prepare to use
Amount is as follows：It is measurement unit with gram, milliliter
(1) selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity control：
(2) Na-K alloy is prepared
Metallic sodium 0.4g ± 0.03g are weighed, metallic potassium 1.6g ± 0.04g are weighed, 1min is stirred, into Na-K alloy；
(3) synthesising mesoporous carbon material at room temperature
The synthesis of meso-porous carbon material is carried out under nitrogen is protected, and is that stirring is completed at room temperature；
1. hybrid reaction mixture is prepared
1.2 ± 0.04g of carbon tetrachloride, 1.8 ± 0.05g of Na-K alloy are weighed, toluene 200mL ± 0.5mL are measured；
In addition round-bottomed flask, into mixed reaction solution；
2. magnetic agitation is opened, mixing time 10h, mixed reaction solution is reacted, and reaction equation is as follows：
CCl4+ 4Na=4NaCl+C
CCl4+ 4K=4KCl+C
3. after the completion of reacting, stirring is stopped；Add ethanol 100mL.
(4) suction filtration
Reacted mixture is placed in the Buchner funnel of bottle,suction, suction filtration is carried out with miillpore filter, retained on filter membrane
Product cake, waste liquid is evacuated in filter flask；
(5) washing, suction filtration
Product cake is placed in beaker, ethanol 100mL, agitator treating 5min is added；
Cleaning solution is placed in the Buchner funnel of bottle,suction, suction filtration is carried out with miillpore filter, remaining product filter cake on filter membrane,
Cleaning solution is evacuated in filter flask；
Washing, suction filtration are carried out 2 times；
Product cake is placed in beaker, deionized water 100mL, agitator treating 5min is added；
Washing, suction filtration are carried out 2 times；
(6) it is vacuum dried
Product cake after washing is placed in quartz container, is subsequently placed in vacuum drying chamber and is dried, dry temperature
55 DEG C ± 1 DEG C of degree, vacuum 50Pa, drying time 10h；
Meso-porous carbon material is after drying；
(7) detect, analyze, characterize
The pattern of the mesoporous carbon body material to preparing, composition, Chemical Physics performance are detected, analyzed, characterized；
The Micro-Structure Analysis of material is carried out with transmission electron microscope；
The pore passage structure analysis of material is carried out with nitrogen physisorption instrument；
The structural analysis of material is carried out with Raman spectrometer；
Graphics process is carried out with material operating room software program；
Conclusion：Synthesis carbon material is black powder at room temperature, and material has mesopore orbit structure, and products collection efficiency is
75.6%；
(8) product storage
Meso-porous carbon material to preparing is stored in the glass container of amber transparent, closed to keep in dark place, and waterproof, is prevented
Damp, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C ± 2 DEG C of storage temperature, relative humidity≤10%.
As shown in figure 1, being the synthetically prepared state diagram of meso-porous carbon material, shown in figure, each portion position is correct, matches somebody with somebody according to quantity
Than sequentially operating；The value of the chemical substance that preparation is used is determined by the scope for pre-setting, and is metering with gram, milliliter
Unit.
The synthesis of meso-porous carbon material is carried out in glass round bottom flask, is completed during being stirred at room temperature；
Agitator is rectangle, and round-bottomed flask 2 is fixed in the fix bar 4 of mixing platform 3 using iron clamp 1, magnetic stir bar 5
Drag is placed in, round-bottomed flask bottleneck plastics plug 6 is sealed.Display screen 8, indicator lamp 9, electricity are provided with blender base 7
Source switch 10, rotation speed regulating and controlling device 11；
It is meso-porous carbon material transmission electron microscope photo shown in Fig. 2, visible in figure, carbon material has pore passage structure.
It is meso-porous carbon material nitrogen adsorption desorption curve figure shown in Fig. 3, visible in figure, carbon material has mesopore orbit knot
Structure.
It is meso-porous carbon material Raman spectrogram shown in Fig. 4, visible in figure, carbon material has unformed structure.
Claims (7)
1. a kind of preparation method of meso-porous carbon material, it is characterised in that as follows including step：Be with organic molecule as carbon source,
With Na-K alloy as reducing agent, with toluene as solvent, under nitrogen protective condition, through magnetic agitation at room temperature reaction 10~
12h, is made reaction solution, through suction filtration, washing, vacuum drying, is made meso-porous carbon material.
2. the preparation method of a kind of meso-porous carbon material according to claim 1, it is characterised in that the Na-K alloy is matched somebody with somebody
Process processed is：It is 1 according to mass ratio：4 ratio weighs metallic sodium and metallic potassium, 1min is stirred, into Na-K alloy.
3. a kind of preparation method of meso-porous carbon material according to claim 1, it is characterised in that the magnetic agitation reaction
Concretely comprise the following steps：
1. hybrid reaction mixture is prepared
It is 1.2 according to mass ratio：1.8 weigh carbon tetrachloride and Na-K alloy is placed in round-bottomed flask, then are added thereto to toluene
200mL~300mL, into mixed reaction solution；
2. magnetic agitation is opened, mixing time 10h, mixed reaction solution is reacted, and reaction equation is as follows：
CCl4+ 4Na=4NaCl+C
CCl4+ 4K=4KCl+C
3. after the completion of reacting, stop stirring, add 100~150mL of ethanol.
4. a kind of preparation method of meso-porous carbon material according to claim 1, it is characterised in that the operation step of the suction filtration
Suddenly it is：Reacted mixture is placed in the Buchner funnel of bottle,suction, suction filtration is carried out with miillpore filter, remaining product on filter membrane
Filter cake, waste liquid is evacuated in filter flask.
5. the preparation method of a kind of meso-porous carbon material according to claim 1, it is characterised in that the washing for twice,
Operating procedure is：Product cake is placed in beaker, ethanol 100mL, agitator treating 5min is added；Cleaning solution is placed in bottle,suction
Buchner funnel in, carry out suction filtration with miillpore filter, remaining product filter cake on filter membrane, cleaning solution is evacuated in filter flask；Washing, suction filtration
Carry out 2 times；Product cake is placed in beaker, deionized water 100mL, agitator treating 5min is added.
6. a kind of preparation method of meso-porous carbon material according to claim 1, it is characterised in that the vacuum drying behaviour
It is as step：Product cake after washing is placed in quartz container, is subsequently placed in vacuum drying chamber and is dried, dry temperature
55~65 DEG C of degree, 50~60Pa of vacuum, 8~12h of drying time are meso-porous carbon material after drying.
7. the preparation method of a kind of meso-porous carbon material according to claim 1, it is characterised in that the preparation method is wrapped
The chemicals for containing is the pure level of analysis.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441652A (en) * | 2018-03-16 | 2018-08-24 | 沈阳师范大学 | A kind of preparation method of mesoporous germanium material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129771A (en) * | 2015-09-09 | 2015-12-09 | 上海大学 | Preparation method of mesoporous carbon with adjustable aperture |
| CN105731414A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Methodof preparing mesoporous carbon material |
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- 2017-04-07 CN CN201710223098.0A patent/CN106882788B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731414A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Methodof preparing mesoporous carbon material |
| CN105129771A (en) * | 2015-09-09 | 2015-12-09 | 上海大学 | Preparation method of mesoporous carbon with adjustable aperture |
Non-Patent Citations (2)
| Title |
|---|
| FANG DAI ET AL.: "Bottom-up synthesis of high surface area mesoporous crystalline silicon and evaluation of its hydrogen evolution performance", 《NATURE COMMUNICATIONS》 * |
| TANG DUIHAI ET AL.: "Self-templated synthesis of mesoporous carbon from carbon tetrachloride precursor for supercapacitor electrodes", 《ACS APPLIED MATERIALS & INTERFACES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441652A (en) * | 2018-03-16 | 2018-08-24 | 沈阳师范大学 | A kind of preparation method of mesoporous germanium material |
| CN108441652B (en) * | 2018-03-16 | 2020-01-14 | 沈阳师范大学 | Preparation method of mesoporous germanium material |
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