CN105621411B - A kind of method for synthesizing macropore carbon material - Google Patents
A kind of method for synthesizing macropore carbon material Download PDFInfo
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- CN105621411B CN105621411B CN201410591307.3A CN201410591307A CN105621411B CN 105621411 B CN105621411 B CN 105621411B CN 201410591307 A CN201410591307 A CN 201410591307A CN 105621411 B CN105621411 B CN 105621411B
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Abstract
The present invention provides a kind of method for synthesizing macropore carbon material, and the carbon material constituent is amorphous carbon element, with two-stage duct；The synthetic method is first handled calcium carbonate and alkali lye mixing, then calcium carbonate filtering being thermally treated resulting in is mixed with water and glucide, stir and dry solution after ultrasonication, it is subsequently placed in carbonization treatment in nitrogen atmosphere, finally by obtained material and acid solution mixed processing, carbon material is dried to obtain by washing.The inventive method is without using expensive organic additive, and operating procedure is simple and easy to apply, low production cost.
Description
Technical field
The invention belongs to porous inorganic material synthesis field, specifically a kind of synthetic method of macropore carbon material.
Background technology
According to the classification of IUPAC, porous material can be divided into three major types：Large pore material（Directly
＞ 50nm）, mesoporous material（2nm≤directly≤50nm）And poromerics（Direct ＜ 2nm）.Due to poromerics and mesoporous material
Applied with succeeding in Industrial Catalysis with the field such as separating, thus be always study and application focus.In recent years, with big
Porous materials compensate for conventional small pore molecular sieve in fields such as bulky molecular catalysis, separation and mesoporous material is difficult to allow macromolecular to enter
Shortcoming inside duct, and the advantage that some other physical chemical characteristics is embodied, the sight of the researcher gradually attracted turn into
The popular domain of research.
" utilize SiO2Opal prepares high specific surface area three-dimensional ordered big hole carbon "（Nanjing Aero-Space University's journal, 2005,
37（5）:593-593）Three-dimensional ordered macroporous carbon is prepared using colloid crystal templating, preparation process is：(1) Stobber is first used
Method synthesis single dispersing SiO2Colloid micro ball, then by centrifuge washing, ethanol disperses, and stands 10~30 days at normal temperatures and pressures,
By SiO2 Microballoon is self-assembled into orderly opal structure under gravity, and 12h is then dried at 120 DEG C.(2) sucrose is used again
The space of filling template, and the process of carbonization is repeated, prepare macropore carbon material.
" double-template method synthesising mesoporous/macropore second hole road carbon materials "（Acta PhySico-Chimica Sinica, 2007,23 (5):
757-760）Mesopore/macropore second hole road carbon material is prepared using colloid crystal templating, its synthetic method is：First according to
Stober methods be made close to monodispersed silica spheres, and under gravity self assembly and form template；Phenolic aldehyde is prepared again
Resin oligomers are dissolved, and by itself and ethanol, the organic matter mixing such as Pluronic F127 is then immersed in silica template,
Room temperature, which is placed to solution, to be dried；Then phenolic resin is polymerize completely, be carbonized under nitrogen protection atmosphere, and removed with hydrofluoric acid
Mesopore/macropore second hole road carbon material is obtained after silica, the diameter macropores of carbon material are about 230nm, and mesopore diameter is about
For 10nm.
CN102295281A, a kind of method that graded porous carbon is prepared by template of hollow mesoporous silicon sphere, by phenolic resin
Ethanol solution is impregnated into the mesopore orbit of hollow mesoporous silicon sphere, then by phenolic resin primary solidification, deep and firmization, carbonization and de-
Removing template, is finally prepared for macropore, mesoporous, micropore graded porous carbon.Wherein template is hollow mesoporous silicon sphere, hollow Jie
Hole silicon ball has hollow core and mesoporous wall, and hollow core aperture is 300-800 nm, mesoporous wall about 25-60nm.The classification of preparation is more
The aperture of hole carbon is 300-800nm, and wall thickness is 25-60nm.
A kind of CN103482597A, synthetic method of middle macropore carbon, resin is mixed with curing agent, is heating and curing；Again will
With pore creating material and mixed with proppants after solidifying substance crushing, precast body, then high temperature cabonization, macropore in preparation are pressed into after being sufficiently mixed
Charcoal, its macropore diameter is at 50nm-10 μm.Wherein pore creating material is polyvinyl alcohol, polyvinyl butyral resin, poly- phthalimide resin, is made
With being manufacture macropore, aperture can change carbonaceous material and creating material ratio, and temperature, pressing pressure and material proportion to adjust
Section；Proppant is graphite powder, activated carbon powder, NACF, CNT or graphite fibre, and effect is to prevent to a certain extent
Base shrinks in carbonisation, make the pore structure of porous charcoal tend towards stability and increase aperture.
Existing large pore material, although the existing many open reports of the preparation method of especially macropore carbon, but still has some to lack
Sunken needs overcome, such as the template assemblies of colloid crystal templating take long, preparation cost height, it is difficult to industrialized production；Some skills
The macropore ratio and content for the large pore material that art is obtained are too low, and macropore diameter is generally higher than 200nm, the excessive application value in aperture
Relatively low, pore diameter range in 100~200nm there is the macropore of high application value to be difficult to prepare.Therefore, research especially Cheap highly effective
The preparation method of macropore carbon just there is very real meaning.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of method for synthesizing macropore carbon material, the carbon that the present invention is provided
Material has abundant pore structure, and synthetic method is simple and easy to apply, and production cost is low.
The present invention provides a kind of carbon material, and the carbon material has following feature：Constituent is amorphous carbon element, tool
There is two-stage duct, the wherein aperture in first order duct is 20~40nm, and the aperture in second level duct is 100~200nm；Always than table
Area is 500~1000 m2/g。
The method of synthesis macropore carbon material of the present invention, comprises the following steps：
（1）Calcium carbonate is mixed with alkali lye, then the stir process at 50~90 DEG C filters, the solids being filtrated to get
Matter is heat-treated 1~3h at 300~500 DEG C；
（2）Will be through step（1）Calcium carbonate after processing is mixed with water and glucide, stirs 10~60min, then ultrasonic
Ripple handles 1~10h；
（3）By step（2）Obtained solution removed in the way of droplet splashes contain solution equipment, collect splash
The droplet gone out, is then dried at 50~80 DEG C；
（4）By step（3）Obtained solid matter carbonization treatment in a nitrogen atmosphere, the carbonization treatment is divided to two sections to enter
OK, 300~450 DEG C are warming up to first, and constant temperature handles 1~3h；Then heat to 800~1000 DEG C of constant temperature and handle 4~8h；
（5）By step（4）Obtained material is well mixed with acid solution, and 1~10h, Ran Houjing are handled at 50~200 DEG C
Cross washing and be dried to obtain carbon material.
In carbon material synthetic method of the present invention, step（1）Described in calcium carbonate be nano-calcium carbonate, the nano-calcium carbonate
Particle diameter be 30~50nm.
In carbon material synthetic method of the present invention, step（1）Described in alkali lye be sodium hydroxide, potassium hydroxide in one kind or
Two kinds, the concentration of lye is 0.01~0.1mol/L, and the mass ratio of calcium carbonate and alkali lye is 1：5~1：50, preferably 1：10~
1：20.
In carbon material synthetic method of the present invention, step（2）Described in glucide be sucrose, glucose in one kind or two
Kind, calcium carbonate, glucide, the mass ratio of water are 0.1~2：1：10~33, preferably 0.2~1：1：13~26.
In carbon material synthetic method of the present invention, step（3）Described in solution splendid attire is removed in the way of droplet splashes
The equipment of solution, the splashing mode, which is specifically as follows quickly to stir solution, makes solution sputter to come with the form of droplet,
Or under stirring, solution is passed through with high velocity air, solution is sputtered in droplet form；The collection is sputtered
The mode of the droplet come is to be collected with filter paper or filter cloth.
In carbon material synthetic method of the present invention, step（4）Described in carbonization treatment carried out in nitrogen atmosphere, nitrogen stream
Speed is 10~50mL/min, preferably 15~40 mL/min.
In carbon material synthetic method of the present invention, step（4）Described in carbonization treatment heating rate be 1~3 DEG C/min,
Heated up with constant heating rate.
In carbon material synthetic method of the present invention, step（5）Described in acid solution be hydrochloric acid or nitric acid, the quality of acid solution
Concentration is 20~60%.
In carbon material synthetic method of the present invention, step（5）Described in acid reaction variables to handle 2 at 100~180 DEG C
~7h.
In carbon material synthetic method of the present invention, step（5）Described in washing be with distillation water washing, the drying be
5~15h is dried at 100~140 DEG C.
The macropore carbon that the present invention is provided has abundant macropore, can be used as catalyst carrier, adsorbent, chromatographic column filler,
It also is used as the synthesis masterplate of inorganic organic material.
Compared with prior art, the macropore carbon material and its synthetic method that the present invention is provided have advantages below：
（1）In the inventive method, using the calcium carbonate through base extraction and heat treatment as hard template, required for can obtaining
Multistage pore canal carbon material, using the inventive method pre-process calcium carbonate, the Surface electric property of calcium carbonate can be made to change,
Promote the calcium carbonate of a part of single dispersing form to assemble, make several calcium carbonate particles assemble to form miniature coherent condition, with
It is easy to the template to be formed needed for macropore duct；And remaining calcium carbonate still keeps monodisperse status, medium duct institute can be used as
The template needed.Again by the ratio of control material, ultrasound is dried to adjust the effect of glucide and calcium carbonate, and segmentation
Carbonization can be formed accurately the two-stage pore canal system with template size feature.The preparation method of macropore carbon of the present invention is simply easy
OK, topmost feature is that, without using expensive poisonous organic formwork agent or additive, cost is low.
（2）In the inventive method, by controlling the ratio of various materials, ultrasound is stirred, the operating procedure such as roasting, to control
Calcium carbonate particle processed（Including single dispersing and miniature state of aggregation）Dispersity.Especially step（3）Mode of operation, by step
（2）The solution sputters to collect and then processing is dried again in droplet form, can make carbohydrate and calcium carbonate particle
All the time it is in uniform admixture, it is to avoid carbohydrate is separated with calcium carbonate, and calcium carbonate particle can largely be assembled, it is impossible to shape
Into template, the carbon material prepared is that aperture is less than the common microporous activated carbons of 2nm.
Brief description of the drawings
Fig. 1 is the SEM photograph for the carbon material that embodiment 1 is synthesized.
Embodiment
The preparation method of carbon material of the present invention is described in detail below by specific embodiment, but is not limited to
Embodiment.The granularity of calcium carbonate used is 40nm or so in embodiment, and manufacturer is Hangzhou Wanjing New Material Co., Ltd..
Embodiment 1
（1）2g calcium carbonate is mixed with 30mL 0.02mol/L sodium hydroxide solutions, 2h is stirred at 70 DEG C；Then carry out
Filtering, obtained solid sample is heat-treated 2h at 350 DEG C；
（2）To step（1）Added in obtained calcium carbonate after 50mL distilled water and 3g sucrose, stirring 30min at ultrasonic wave
Manage 5h；
（3）By step（2）Obtained solution is quickly stirred, and the equipment for containing solution is sputtered in the form of droplet, and
And with filter paper collect sputter come droplet, then by the droplet being collected at 70 DEG C drying；
（4）By step（3）Obtained solid sample is placed in tube furnace, is passed through nitrogen, and nitrogen flow rate is 30mL/min；With
2 DEG C/min is warming up to 350 DEG C, constant temperature processing 2h；850 DEG C, constant temperature 5h are warming up to 2 DEG C/min again；
（5）By step（4）Obtained material is well mixed with 50mL50% hydrochloric acid solution, is handled under the conditions of 150 DEG C
5h, is finally washed with water to neutrality, and 10h is dried under the conditions of 100 DEG C, that is, prepares macropore carbon material, numbering is CL1, gained
The duct apertures at different levels integrated distribution and reference area of sample the results are shown in Table 1.
Embodiment 2
（1）2.5g calcium carbonate is mixed with 30mL 0.02mol/L sodium hydroxide solutions, 2h is stirred at 70 DEG C；Then enter
Row filtering, obtained solid sample handles 1h at 400 DEG C；
（2）To step（1）Added in obtained calcium carbonate after 50mL distilled water and 3g sucrose, stirring 30min at ultrasonic wave
Manage 4h；
（3）By step（2）Obtained solution is quickly stirred, and the equipment for containing solution is sputtered in the form of droplet, and
And with filter paper collect sputter come droplet, then by the droplet being collected under the conditions of 60 DEG C drying；
（4）By step（3）Obtained solid sample is placed in tube furnace, is passed through nitrogen, and nitrogen flow rate is 30mL/min；With
3 DEG C/min is warming up to 320 DEG C, constant temperature processing 2h；950 DEG C, constant temperature 5h are warming up to 3 DEG C/min again；
（5）By step（4）Obtained material is well mixed with 50mL50% hydrochloric acid solution, is handled under the conditions of 150 DEG C
5h, is finally washed with water to neutrality, and 10h is dried under the conditions of 100 DEG C, that is, prepares macropore carbon material, numbering is CL2, gained
The duct apertures at different levels integrated distribution and reference area of sample the results are shown in Table 1.
Embodiment 3
（1）1.5g calcium carbonate is mixed with 50mL 0.05mol/L sodium hydroxide solutions, 2h is stirred under the conditions of 70 DEG C；So
Filtered afterwards, obtained solid sample dries 2.5h under the conditions of 500 DEG C；
（2）To step（1）Added in obtained calcium carbonate after 70mL distilled water and 3g sucrose, stirring 30min at ultrasonic wave
Manage 5h.
（3）By step（2）Obtained solution is quickly stirred, and the equipment for containing solution is sputtered in the form of droplet, and
And with filter paper collect sputter come droplet, then by the droplet being collected under the conditions of 70 DEG C drying；
（4）By step（3）Obtained solid sample is placed in tube furnace, is passed through nitrogen, and nitrogen flow rate is 30mL/min；With
2 DEG C/min is warming up to 400 DEG C, constant temperature processing 2h；900 DEG C, constant temperature 4h are warming up to 2 DEG C/min again；
（5）By step（4）Obtained material is well mixed with 50mL50% hydrochloric acid solution, is handled under the conditions of 140 DEG C
6h, is finally washed with water to neutrality, and 10h is dried under the conditions of 100 DEG C, that is, prepares macropore carbon material, numbering is CL3, gained
The duct apertures at different levels integrated distribution and reference area of sample the results are shown in Table 1.
Embodiment 4
（1）3g calcium carbonate is mixed with 60mL 0.02mol/L sodium hydroxide solutions, 1h is stirred under the conditions of 70 DEG C；Then
Filtered, obtained solid sample handles 1.5h under the conditions of 360 DEG C；
（2）To step（1）Added in obtained calcium carbonate after 50mL distilled water and 3g sucrose, stirring 30min at ultrasonic wave
Manage 5h；
（3）By step（2）Obtained solution is quickly stirred, and the equipment for containing solution is sputtered in the form of droplet, and
And with filter paper collect sputter come droplet, then by the droplet being collected under the conditions of 70 DEG C drying；
（4）By step（3）Obtained solid sample is placed in tube furnace, is passed through nitrogen, and nitrogen flow rate is 30mL/min；With
1.5 DEG C/min is warming up to 350 DEG C, constant temperature processing 2h；850 DEG C, constant temperature 5h are warming up to 1.5 DEG C/min again；
（5）By step（4）Obtained material is well mixed with 50mL50% salpeter solution, is handled under the conditions of 150 DEG C
5h, is finally washed with water to neutrality, and 10h is dried under the conditions of 100 DEG C, that is, prepares macropore carbon material, numbering is CL4, gained
The duct apertures at different levels integrated distribution and reference area of sample the results are shown in Table 1.
Embodiment 5
（1）5g calcium carbonate is mixed with 80mL 0.02mol/L sodium hydroxide solutions, 2h is stirred under the conditions of 60 DEG C；Then
Filtered, obtained solid sample handles 2h under the conditions of 400 DEG C；
（2）To step（1）Added in obtained calcium carbonate after 50mL distilled water and 3g sucrose, stirring 30min at ultrasonic wave
Manage 5h；
（3）By step（2）Obtained solution is quickly stirred, and the equipment for containing solution is sputtered in the form of droplet, and
And with filter paper collect sputter come droplet, then by the droplet being collected at 70 DEG C drying；
（4）By step（3）Obtained solid sample is placed in tube furnace, is passed through nitrogen, and nitrogen flow rate is 30mL/min；With
2 DEG C/min is warming up to 350 DEG C, constant temperature processing 3h；850 DEG C, constant temperature 6h are warming up to 2 DEG C/min again；
（5）By step（4）Obtained material is well mixed with 50mL50% hydrochloric acid solution, is handled under the conditions of 150 DEG C
5h, is finally washed with water to neutrality, and 10h is dried under the conditions of 100 DEG C, that is, prepares macropore carbon material, numbering is CL5, gained
The duct apertures at different levels integrated distribution and reference area of sample the results are shown in Table 1.
Comparative example 1
（1）By 2g calcium carbonate, 50mL distilled water and 3g sucrose stir ultrasonication 5h after 30min；
（2）By step（1）Obtained solution is quickly stirred, and the equipment for containing solution is sputtered in the form of droplet, and
And with filter paper collect sputter come droplet, then by the droplet being collected at 70 DEG C drying；
（3）By step（2）Obtained solid sample is placed in tube furnace, is passed through nitrogen, and nitrogen flow rate is 30mL/min；With
2 DEG C/min is warming up to 850 DEG C, constant temperature 5h；
（4）By step（3）Obtained material is well mixed with 50mL50% hydrochloric acid solution, is handled under the conditions of 150 DEG C
5h, is finally washed with water to neutrality, and 10h is dried under the conditions of 100 DEG C, carbon material is prepared, numbering is CL6, gained sample
Duct apertures at different levels integrated distribution and reference area the results are shown in Table 1.
Comparative example 2
（1）2g calcium carbonate is mixed with 30mL 0.02mol/L sodium hydroxide solutions, 2h is stirred under the conditions of 70 DEG C；Then
Filtered, obtained solid sample handles 2h under the conditions of 350 DEG C；
（2）To step（1）Added in obtained calcium carbonate after 50mL distilled water and 3g sucrose, stirring 30min at ultrasonic wave
Manage 5h；
（3）By step（2）The solution of preparation is dried under the conditions of 70 DEG C；It is subsequently placed in tube furnace, is passed through nitrogen, nitrogen
Flow velocity is 30mL/min；With 2 DEG C/min from room temperature to 850 DEG C, constant temperature 5h；
（4）By step（3）Obtained material is well mixed with 50mL50% hydrochloric acid solution, is handled under the conditions of 150 DEG C
5h, is finally washed with water to neutrality, and 10h is dried under the conditions of 100 DEG C, that is, prepares carbon material, numbering is CL7, gained sample
Duct apertures at different levels integrated distribution and reference area the results are shown in Table 1.
Comparative example 3
（1）2g calcium carbonate, 50mL distilled water and 3g sucrose are mixed, ultrasonication 5h after stirring 30min；
（2）By step（1）The solution of preparation is dried under the conditions of 70 DEG C.It is placed in again in tube furnace, is passed through nitrogen, nitrogen stream
Speed is 30mL/min；With 2 DEG C/min from room temperature to 850 DEG C, constant temperature 5h.
（3）By step（2）Obtained material is well mixed with 50mL50% hydrochloric acid solution, is handled under the conditions of 150 DEG C
5h, is finally washed with water to neutrality, and 10 h are dried under the conditions of 100 DEG C, that is, prepare carbon material, numbering is CL8, gained sample
Duct apertures at different levels integrated distribution and reference area the results are shown in Table 1.Sample physico-chemical property obtained by the embodiment of table 1 and comparative example
It can be drawn by embodiment and comparative example result, the inventive method can prepare high-quality macropore carbon, and
The operating procedure of the present invention is not used, and the carbon material prepared in the case of same material proportion is common micro-pore carbon material or Jie
Hole carbon material, does not contain macroporous structure.
Claims (12)
1. a kind of method for synthesizing macropore carbon material, the carbon material constituent is amorphous carbon, with two-stage duct, wherein
The aperture in first order duct is 20~40nm, and the aperture in second level duct is 100~200nm, total specific surface area is 500~
1000 m2/g；The method of the synthesis macropore carbon material comprises the following steps：
（1）Calcium carbonate is mixed with alkali lye, then the stir process at 50~90 DEG C filters, and the solid matter being filtrated to get exists
1~3h is heat-treated at 300~500 DEG C, the particle diameter of calcium carbonate is 30~50nm, and concentration of lye is 0.01~0.1mol/L, carbonic acid
The mass ratio of calcium and alkali lye is 1：5~1：50；
（2）Will be through step（1）Calcium carbonate after processing is mixed with water and glucide, 10~60min is stirred, then at ultrasonic wave
1~10h is managed, the calcium carbonate, glucide, the mass ratio of water are 0.1~2：1：10~33；
（3）By step（2）Obtained solution remove in the way of droplet splashes the equipment for containing solution, collect and sputter
Droplet, is then dried at 50~80 DEG C；
（4）By step（3）Obtained solid matter carbonization treatment in a nitrogen atmosphere, the carbonization treatment is divided to two sections of progress, first
300~450 DEG C are first warming up to, constant temperature handles 1~3h；Then heat to 800~1000 DEG C of constant temperature and handle 4~8h；
（5）By step（4）Obtained material is well mixed with acid solution, and 1~10h is handled at 50~200 DEG C, then by washing
Wash and be dried to obtain carbon material.
2. in accordance with the method for claim 1, it is characterised in that：Step（1）Described in alkali lye be sodium hydroxide, potassium hydroxide
One or both of.
3. in accordance with the method for claim 1, it is characterised in that：Step（1）The mass ratio of middle calcium carbonate and alkali lye is 1：10
~1：20.
4. in accordance with the method for claim 1, it is characterised in that：Step（2）Described in glucide be sucrose, glucose in
One or two.
5. in accordance with the method for claim 1, it is characterised in that：Step（2）Described in calcium carbonate, glucide, the matter of water
Amount is than being 0.2~1：1：13~26.
6. in accordance with the method for claim 1, it is characterised in that：Step（4）Described in carbonization treatment in nitrogen atmosphere
Carry out, nitrogen flow rate is 10~50mL/min.
7. in accordance with the method for claim 6, it is characterised in that：The nitrogen flow rate is 15~40 mL/min.
8. in accordance with the method for claim 1, it is characterised in that：Step（4）Described in carbonization treatment heating rate for 1~
3℃/min。
9. in accordance with the method for claim 1, it is characterised in that：Step（4）Described in carbonization treatment with constant heating speed
Rate heats up.
10. in accordance with the method for claim 1, it is characterised in that：Step（5）Described in acid solution be hydrochloric acid or nitric acid.
11. in accordance with the method for claim 10, it is characterised in that：Step（5）Described in the mass concentration of acid solution be
20~60%.
12. in accordance with the method for claim 1, it is characterised in that：Step（5）Described in washing be with distillation water washing, institute
State and dry to dry 5~15h at 100~140 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2055811C1 (en) * | 1994-02-10 | 1996-03-10 | Ермолаев Валерьян Андреевич | Granulated activated carbon production method |
| CN101585527A (en) * | 2008-05-23 | 2009-11-25 | 中国人民解放军63971部队 | In a kind of being rich in, the charcoal preparation methods of macropore |
| CN103855413A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院大连化学物理研究所 | Porous carbon material used for lithium-air cell anode |
-
2014
- 2014-10-30 CN CN201410591307.3A patent/CN105621411B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2055811C1 (en) * | 1994-02-10 | 1996-03-10 | Ермолаев Валерьян Андреевич | Granulated activated carbon production method |
| CN101585527A (en) * | 2008-05-23 | 2009-11-25 | 中国人民解放军63971部队 | In a kind of being rich in, the charcoal preparation methods of macropore |
| CN103855413A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院大连化学物理研究所 | Porous carbon material used for lithium-air cell anode |
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