CN109319760A - A kind of carbon micron-spheres and preparation method thereof - Google Patents
A kind of carbon micron-spheres and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 17
- 239000008103 glucose Substances 0.000 claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims abstract description 16
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 15
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 17
- 238000005119 centrifugation Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- GZCGUPFRVQAUEE-VANKVMQKSA-N aldehydo-L-glucose Chemical compound OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)C=O GZCGUPFRVQAUEE-VANKVMQKSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical group CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 claims 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 17
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 description 15
- 238000005352 clarification Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 239000006228 supernatant Substances 0.000 description 9
- 238000000926 separation method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 230000031709 bromination Effects 0.000 description 3
- 238000005893 bromination reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 241000143432 Daldinia concentrica Species 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical group [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of carbon micron-spheres and preparation method thereof, the preparation method is using glucose as carbon source, using dodecyl sodium sulfate and/or cetyl trimethylammonium bromide as surfactant, it is capable of forming vesica in aqueous solution using surfactant, and carbon micron-spheres are tied up in vesica to grow and be formed, particle size depends on the size of vesica, therefore, by adjusting surfactant, so that it may adjust the partial size of the carbon micron-spheres ultimately generated.Compared with traditional handicraft, preparation process of the present invention is simple, and controllability is strong, reproducible, environmentally protective;Preparation method yield of the present invention is high, can achieve 20 ﹪ or more, has the feasibility of batch production, and the carbon micron-spheres being prepared are easy to be centrifugated;The invention has the advantages of low raw material cost, is easy to get;The carbon micron-spheres that the method for the present invention is prepared can be widely applied to the fields such as catalyst carrier, drug conveying, pollutant absorption, fuel cell, supercapacitor and lithium ion battery electrode material.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of carbon micron-spheres and preparation method thereof.
Background technique
Carbon ball as a kind of new function carbon material there is good chemical stability, thermal stability, excellent conduction to lead
It is hot, intrinsic damp is good, biggish specific surface area and the advantages that lower density, in addition its regular spherical structure, makes
It becomes a kind of material with wide application prospect.Nano-micrometre carbon ball has been widely used in catalyst carrier, medicine at present
The fields such as object conveying, pollutant absorption, fuel cell, supercapacitor and lithium ion battery electrode material.
The method for having developed a variety of preparation carbon balls at present, such as hydro-thermal method, active metal reduction method, chemical vapor deposition
Method, plasma method, polymer catalyzing pyrolysismethod, ultrasonic heat solution etc..There are complex process, former material for the manufacture of these carbon balls
The problems such as waste rate is high, product yield is low is expected, as active metal reduction method needs protective atmosphere;Plasma method, CVD method,
Ultrasonic heat solution is required using equipment costly;Polymer catalyzing pyrolysismethod obtains micron-sized oval hard carbon ball
Material.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provide a kind of preparation process is simple, controllability is strong,
It is reproducible, yield is high, easy centrifuge separation, low in cost and environmentally protective carbon micron-spheres and preparation method thereof.
The technical solution of the present invention is as follows:
A kind of preparation method of carbon micron-spheres, includes the following steps:
(1) glucose is added to the water, then stirring is added surfactant, obtains mixed solution to dissolving;
(2) step (1) described mixed solution is subjected to hydro-thermal reaction in hydrothermal reaction kettle, after cooling, successively by from
The heart, washing, drying are to get the carbon micron-spheres.
Further, in step (1), the surfactant is dodecyl sodium sulfate and/or cetyl trimethyl
Ammonium bromide.
Further, when surfactant is dodecyl sodium sulfate, the glucose, water, dodecyl sodium sulfate
Mass ratio is 4-6:20-40:0.05-0.2;When surfactant is cetyl trimethylammonium bromide, the glucose,
Water, cetyl trimethylammonium bromide mass ratio be 4-6:20-40:0.3-1.5;Surfactant is dodecyl sodium sulfonate
When sodium and cetyl trimethylammonium bromide, the glucose, water, dodecyl sodium sulfate and cetyl trimethylammonium bromide
Mass ratio be 4-6:20-40:0.05-0.2:0.3-1.5.
Further, in step (2), the temperature of the hydro-thermal reaction is 160-200 DEG C, and the time of the hydro-thermal reaction is
6-20h。
Further, the temperature of the hydro-thermal reaction is 170-190 DEG C, and the time of the hydro-thermal reaction is 8-16h.
Further, in step (2), the speed of the centrifugation is 4000-5000r/min, and the time of the centrifugation is 6-
10min。
Further, in step (2), the washing is first to be washed with dehydrated alcohol, then be washed with deionized water.
Further, in step (2), the temperature of the drying is 80-100 DEG C, and the time of the drying is 6-24h.
Further, in step (2), the partial size of the carbon micron-spheres is 0.2-1.1 μm.
The carbon micron-spheres that the method is prepared.
Hydro-thermal reaction, which refers to, to be taken water as a solvent, the chemistry carried out in the pressure vessel of sealing by the condition of high temperature and pressure
Reaction.Hydro-thermal reaction is easy to operate, and mild condition can manufacture, and is contained by carbon ball surface prepared by hydro-thermal reaction
A large amount of activity oxygen-containing groups can form new function carbon material with ion, molecule or functional groups.
The invention has the benefit that
1, the preparation method of carbon micron-spheres of the present invention, using glucose as carbon source, with dodecyl sodium sulfate and/or
Cetyl trimethylammonium bromide is surfactant, is capable of forming vesica in aqueous solution using surfactant, and micron
Carbon ball is tied up to grow in vesica and be formed, and particle size depends on the size of vesica, therefore, by adjusting surfactant, just
The partial size of the adjustable carbon micron-spheres ultimately generated.Compared with traditional handicraft, preparation process of the present invention is simple, and controllability is strong,
It is reproducible, it is environmentally protective;
2, preparation method yield of the present invention is high, can achieve 20 ﹪ or more, has the feasibility of batch production, and be prepared into
To carbon micron-spheres be easy to be centrifugated;
3, the invention has the advantages of low raw material cost, is easy to get;
4, the carbon micron-spheres that the method for the present invention is prepared can be widely applied to catalyst carrier, drug conveying, pollutant
The fields such as absorption, fuel cell, supercapacitor and lithium ion battery electrode material.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of carbon micron-spheres described in embodiment 1;
Fig. 2 is the stereoscan photograph of carbon micron-spheres described in embodiment 2;
Fig. 3 is the stereoscan photograph of carbon micron-spheres described in embodiment 2;
Fig. 4 is the stereoscan photograph of carbon micron-spheres described in embodiment 3;
Fig. 5 is the stereoscan photograph of carbon micron-spheres described in embodiment 3;
Fig. 6 is the stereoscan photograph of carbon micron-spheres described in embodiment 4;
Fig. 7 is the stereoscan photograph of carbon micron-spheres described in embodiment 5;
Fig. 8 is the stereoscan photograph of carbon micron-spheres described in embodiment 6;
Fig. 9 is the IR Characterization map of carbon micron-spheres described in embodiment 6.
Specific embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 6g glucose is added in 40ml water, then 50mg dodecyl sodium sulfate, stirring is added to dissolving in stirring
15min makes to be uniformly mixed, and obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 160 DEG C of hydro-thermal reaction 9h, is cooled to room temperature
Afterwards, 6min is centrifugated with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until washing
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 8h in 80 DEG C of vacuum oven, i.e.,
Carbon micron-spheres of the particle diameter distribution between 0.489~0.678 μm are obtained, see Fig. 1, the even particle size distribution of carbon ball, and be
It is easy the carbon ball interconnected of centrifuge separation.
Embodiment 2
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 6g glucose is added in 40ml water, then 50mg dodecyl sodium sulfate, stirring is added to dissolving in stirring
15min makes to be uniformly mixed, and obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 160 DEG C of hydro-thermal reaction 11h, is cooled to room
Wen Hou is centrifugated 6min with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 8h in 80 DEG C of vacuum oven,
Up to carbon micron-spheres of the particle diameter distribution between 0.662~0.714 μm, Fig. 2, Fig. 3 are seen, the even particle size distribution of carbon ball,
It and is the carbon ball interconnected for being easy centrifuge separation.
Embodiment 3
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 6g glucose is added in 40ml water, then 50mg dodecyl sodium sulfate, stirring is added to dissolving in stirring
15min adds 300mg cetyl trimethylammonium bromide, continues to stir 30min, obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 180 DEG C of hydro-thermal reaction 8h, is cooled to room temperature
Afterwards, 8min is centrifugated with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until washing
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 8h in 80 DEG C of vacuum oven, i.e.,
Carbon micron-spheres of the particle diameter distribution between 0.213~0.386 μm, see Fig. 4, Fig. 5, the even particle size distribution of carbon ball, and
It and is the carbon ball interconnected for being easy centrifuge separation.
Embodiment 4
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 6g glucose is added in 40ml water, then 50mg dodecyl sodium sulfate, stirring is added to dissolving in stirring
15min adds 300mg cetyl trimethylammonium bromide, continues to stir 30min, obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 180 DEG C of hydro-thermal reaction 10h, is cooled to room
Wen Hou is centrifugated 8min with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 8h in 80 DEG C of vacuum oven,
Up to carbon micron-spheres of the particle diameter distribution between 0.42~0.52 μm, Fig. 6, the even particle size distribution of carbon ball are seen, and be
It is easy the carbon ball interconnected of centrifuge separation.
Embodiment 5
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 6g glucose is added in 40ml water, then 300mg cetyl trimethyl bromination is added to dissolving in stirring
Ammonium continues to stir 15min, obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 180 DEG C of hydro-thermal reaction 8h, is cooled to room temperature
Afterwards, 8min is centrifugated with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until washing
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 8h in 80 DEG C of vacuum oven, i.e.,
Carbon micron-spheres of the particle diameter distribution between 0.474~0.545 μm are obtained, see Fig. 7, the even particle size distribution of carbon ball, and be
It is easy the carbon ball interconnected of centrifuge separation.
Embodiment 6
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 6g glucose is added in 40ml water, then 300mg cetyl trimethyl bromination is added to dissolving in stirring
Ammonium continues to stir 15min, obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 180 DEG C of hydro-thermal reaction 16h, is cooled to room
Wen Hou is centrifugated 8min with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 8h in 80 DEG C of vacuum oven,
Up to carbon micron-spheres of the particle diameter distribution between 1.02~1.05 μm, Fig. 8 is seen.The even particle size distribution of carbon ball, and be
It is easy the carbon ball interconnected of centrifuge separation.Fig. 9 show the IR Characterization map of the carbon micron-spheres, in Fig. 9 there are two
Strong absworption peak, wherein 3400cm-1The strong absworption peak of left and right corresponds to the characteristic peak of hydroxyl (- OH), 1700cm-1The absorption peak of left and right
For the characteristic peak of carbonyl (- C ﹦ O), these characteristic peaks show there is a large amount of hydroxyl and carbonyl on the surface of carbon ball, these functional groups
Presence have conducive to carbon ball template adsorbing metal cation.
Embodiment 7
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 4g glucose is added in 20ml water, then 200mg dodecyl sodium sulfate, stirring is added to dissolving in stirring
15min makes to be uniformly mixed, and obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 200 DEG C of hydro-thermal reaction 6h, is cooled to room temperature
Afterwards, 10min is centrifugated with the revolving speed of 4000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 6h in 100 DEG C of vacuum oven,
Up to carbon micron-spheres of the particle diameter distribution at 0.2-0.453 μm.
Embodiment 8
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 4g glucose is added in 20ml water, then 200mg dodecyl sodium sulfate, stirring is added to dissolving in stirring
15min adds 1.5g cetyl trimethylammonium bromide, continues to stir 30min, obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 170 DEG C of hydro-thermal reaction 20h, is cooled to room
Wen Hou is centrifugated 8min with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried in 80 DEG C of vacuum oven for 24 hours,
Up to carbon micron-spheres of the particle diameter distribution at 0.923-1.1 μm.
Embodiment 9
The present embodiment provides a kind of preparation methods of carbon micron-spheres, include the following steps:
(1) 4g glucose is added in 20ml water, then 1.5g cetyl trimethyl bromination is added to dissolving in stirring
Ammonium continues to stir 15min, obtains mixed solution;
(2) step (1) mixed solution is moved into hydrothermal reaction kettle, in 190 DEG C of hydro-thermal reaction 8h, is cooled to room temperature
Afterwards, 8min is centrifugated with the revolving speed of 5000r/min, is then first washed with dehydrated alcohol, then be washed with deionized, until washing
Until the supernatant clarification being centrifuged after washing, the solid obtained after centrifugation is dried into 8h in 80 DEG C of vacuum oven, i.e.,
Obtain carbon micron-spheres of the particle diameter distribution at 575-628 μm.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of preparation method of carbon micron-spheres, which comprises the steps of:
(1) glucose is added to the water, then stirring is added surfactant, obtains mixed solution to dissolving;
(2) step (1) described mixed solution is subjected to hydro-thermal reaction in hydrothermal reaction kettle, after cooling, successively by being centrifuged, washing
It washs, dry to get the carbon micron-spheres.
2. the preparation method of carbon micron-spheres according to claim 1, which is characterized in that in step (1), the surface-active
Agent is dodecyl sodium sulfate and/or cetyl trimethylammonium bromide.
3. the preparation method of carbon micron-spheres according to claim 2, which is characterized in that surfactant is dodecyl sulphur
When sour sodium, the glucose, water, dodecyl sodium sulfate mass ratio be 4-6:20-40:0.05-0.2;
When surfactant is cetyl trimethylammonium bromide, the matter of the glucose, water, cetyl trimethylammonium bromide
The ratio between amount is 4-6:20-40:0.3-1.5;
When surfactant is dodecyl sodium sulfate and cetyl trimethylammonium bromide, the glucose, water, dodecyl
The mass ratio of sodium sulfonate and cetyl trimethylammonium bromide is 4-6:20-40:0.05-0.2:0.3-1.5.
4. the preparation method of carbon micron-spheres according to claim 1, which is characterized in that in step (2), the hydro-thermal reaction
Temperature be 160-200 DEG C, time of the hydro-thermal reaction is 6-20h.
5. the preparation method of carbon micron-spheres according to claim 4, which is characterized in that the temperature of the hydro-thermal reaction is
170-190 DEG C, the time of the hydro-thermal reaction is 8-16h.
6. the preparation method of carbon micron-spheres according to claim 1, which is characterized in that in step (2), the speed of the centrifugation
Degree is 4000-5000r/min, and the time of the centrifugation is 6-10min.
7. the preparation method of carbon micron-spheres according to claim 1, which is characterized in that in step (2), the washing is first
It is washed, then is washed with deionized water with dehydrated alcohol.
8. the preparation method of carbon micron-spheres according to claim 1, which is characterized in that in step (2), the temperature of the drying
Degree is 80-100 DEG C, and the time of the drying is 6-24h.
9. the preparation method of carbon micron-spheres according to claim 1, which is characterized in that in step (2), the carbon micron-spheres
Partial size be 0.2-1.1 μm.
10. the carbon micron-spheres that any one of claim 1-9 the method is prepared.
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CN115724419A (en) * | 2021-09-01 | 2023-03-03 | 中国科学院大连化学物理研究所 | Method for preparing hollow carbon spheres by one-pot method and application |
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CN101875489A (en) * | 2009-12-22 | 2010-11-03 | 聊城大学 | Preparation method of large-size carbon spheres |
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CN110828838A (en) * | 2019-11-22 | 2020-02-21 | 河北师范大学 | Preparation method of palladium-based catalyst with particle size larger than 10 microns and snowflake ball morphology |
CN110921896A (en) * | 2019-11-28 | 2020-03-27 | 闽南师范大学 | Method for preparing nano charcoal balls from syrup wastewater |
CN110975812A (en) * | 2019-12-18 | 2020-04-10 | 西北农林科技大学 | Tea saponin hollow carbon spheres, preparation method thereof and application thereof in heavy metal adsorption |
CN113336215A (en) * | 2020-03-02 | 2021-09-03 | 赵昆 | Preparation method and application of monodisperse hydrothermal carbon spheres |
CN113415798A (en) * | 2021-05-12 | 2021-09-21 | 江西农业大学 | Preparation method of phosphorus-doped microporous, mesoporous and macroporous coexisting grade pore structure nano carbon spheres |
CN113415798B (en) * | 2021-05-12 | 2023-02-24 | 江西农业大学 | Preparation method of phosphorus-doped microporous, mesoporous and macroporous coexisting grade pore structure carbon nanospheres |
CN115724419A (en) * | 2021-09-01 | 2023-03-03 | 中国科学院大连化学物理研究所 | Method for preparing hollow carbon spheres by one-pot method and application |
CN115260763A (en) * | 2022-09-06 | 2022-11-01 | 安徽中科宇顺科技有限公司 | Polyimide black film with high insulation strength and preparation method thereof |
CN115260763B (en) * | 2022-09-06 | 2023-09-29 | 安徽中科宇顺科技有限公司 | Polyimide black film with high insulating strength and preparation method thereof |
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