CN110078050A - A kind of nano carbon microsphere and preparation method thereof - Google Patents
A kind of nano carbon microsphere and preparation method thereof Download PDFInfo
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- CN110078050A CN110078050A CN201910500924.0A CN201910500924A CN110078050A CN 110078050 A CN110078050 A CN 110078050A CN 201910500924 A CN201910500924 A CN 201910500924A CN 110078050 A CN110078050 A CN 110078050A
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- 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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Abstract
The invention discloses a kind of nano carbon microsphere, this carbon ball is solid construction, and monodispersity is good, and surface is smooth, and free from admixture, partial size is small, and particle diameter distribution is relatively uniform on the whole.The nano carbon microsphere prepared simultaneously through microwave-hydrothermal method, has many advantages, such as high density, high intensity, high-specific surface area.The invention also discloses a kind of preparation methods of nano carbon microsphere, comprising: the glucose of certain mass is taken to be put into inner liner of reaction kettle；It takes a certain amount of deionized water to be added in aforesaid reaction vessel, dissolves glucose all, be then charged into reaction kettle and be put into baking oven, do hydro-thermal reaction；After reaction, solution in kettle is filtered, sample is wrapped with filter paper and is put into drying in drying box.Present invention process process is simple, can continuous production, raw material it is cheap, safe and non-toxic；Particle size is small to be evenly distributed, particle agglomeration is light, good crystalline and it is controllable, be not required to high temperature sintering, eliminate grinding and thus bring impurity, avoid defect.
Description
Technical field
The present invention relates to a kind of nano carbon microspheres and preparation method thereof.
Background technique
Carbosphere material is since it is with high density, high intensity, high-specific surface area and answering in terms of lithium ion battery
With prospect, the interest of many researchers is caused.The shapes and sizes of carbosphere significantly affect its electric property.
Many chemical reactions can occur under hydrothermal conditions for glucose, the results showed that working as the glucose of 0.5mol/L
Solution not will form carbon ball when being lower than 140 DEG C or the reaction time is less than 1h.When reaction condition is 0.5mol/L, 160 DEG C, 3h
Start nucleation occur, this carburising step Producing reason: first is that due to caused by dehydration intermolecular between oligosaccharide
Cross-linking reaction；Second is that there is the formation of other macromoleculars in previous steps, the core then formed isotropic growth in the solution.
Existing result of study shows that glucose initial concentration, reaction temperature and reaction time in preparation process can all directly affect
The particle diameter distribution of carbon ball, wherein the reaction time influences grain diameter very big.
Preparing nano carbon microsphere by glucose water thermal method has the characteristics that green and pollution-free, does not introduce in experimentation
Any initiator and toxic solvent, the carbon ball uniform particle sizes being prepared, size is controllable, while a large amount of active officials are contained on surface
It can roll into a ball, there is excellent hydrophily and surface reaction activity, can be applied to biochemistry, biological diagnosis and drug delivery neck
Domain can also be used as preparation Core-shell structure material or the template of porous material etc., have fabulous application prospect.
Summary of the invention
The technical problems to be solved by the present invention are: overcoming the deficiencies of the prior art and provide a kind of nano carbon microsphere and its system
Preparation Method, the carbon ball are solid construction, and monodispersity is good, and surface is smooth, and free from admixture, partial size is small, on the whole particle diameter distribution ratio
It is more uniform；This method prepares nano carbon microsphere in addition, the features such as density is high, intensity is high, surface area is big, multi-party in lithium ion battery etc.
Face has vast application prospect.
In order to solve the above-mentioned technical problem, the technical scheme is that using glucose as presoma, pass through hydro-thermal method
Prepare nano carbon microsphere.
Further, the nano carbon microsphere is solid construction, and monodispersity is good, and surface is smooth, and free from admixture exists, and partial size is about
For 200nm, particle diameter distribution is relatively uniform on the whole, the present invention also provides a kind of preparation method of nano carbon microsphere, including it is following
Step: step S1: directly configuring a certain proportion of glucose solution in inner liner of reaction kettle, and it is anti-that liner is then fixed on high pressure
Answer kettle back；Step S2: setting reaction condition does hydro-thermal reaction；Step S3: dark brown solution in kettle is filtered, cleaning, drying
Obtain nano carbon microsphere.
Further, the preparation method of the nano carbon microsphere, it is characterised in that in step S1: the Portugal 6g is weighed with electronic balance
Grape sugar is put into 50mL inner liner of reaction kettle, and 35mL deionized water is accurately pipetted with pipette, and (concentration of glucose solution is
It 0.78mol/L) is added in aforesaid reaction vessel, with glass bar agitating solution, dissolves glucose all, be then charged into reaction kettle
In, screw up with a wrench reaction kettle, is put into baking oven.
Further, the preparation method of the nano carbon microsphere, it is characterised in that in the step S2: setting reaction condition
For, 180 DEG C of temperature, reaction time 4-12 h.
Further, the preparation method of the nano carbon microsphere, it is characterised in that in the step S3: to after reaction,
It is down to room temperature, takes out reaction kettle, dark brown solution in kettle is filtered and (uses the organic filter membrane of 220nm), and is cleaned in reaction kettle in time
Lining, deionized water and washes of absolute alcohol to filtrate are colourless when suction filtration, and sample is wrapped with filter paper and is put into 70 in drying box
DEG C dry 4h.
After above-mentioned technical proposal, the invention has the following advantages: 1) nano carbon microsphere of the invention is solid
Structure, monodispersity is good, and surface is smooth, and free from admixture exists, and partial size is about 200nm, and particle diameter distribution is relatively uniform on the whole；2)
Compared with conventional carbon method of modifying, the present invention have it is easy to operate, high-efficient, product is purer, environmental-friendly etc. a series of
Advantage；3) present invention process process it is simple, can continuous production raw material it is cheap, safe and non-toxic；4) products therefrom partial size of the present invention is small
Be evenly distributed, particle agglomeration is light, good crystalline and it is controllable, be not required to high temperature sintering, eliminate grinding and thus bring impurity.
Detailed description of the invention
Fig. 1 is transmission electron microscope (TEM) photo of nano carbon microsphere of the invention；Fig. 2 is the infrared spectroscopy of carbon ball of the invention
Figure.
Specific embodiment
In order that the present invention can be more clearly and readily understood, right below according to specific embodiment and in conjunction with attached drawing
The present invention is described in further detail.
Embodiment one: a kind of nano carbon microsphere is used glucose as presoma, is prepared by hydro-thermal method.Fig. 1 is experiment gained
The transmission electron microscope photo of carbon ball, it is seen that this carbon ball is solid construction, and monodispersity is good, and surface is smooth, and free from admixture exists, partial size
About 200nm, particle diameter distribution is relatively uniform on the whole；Fig. 2 is the resulting carbon ball infrared spectrogram of experiment, is more satisfactory carbon
The infrared spectrogram of ball can be used to the functional group's information for analyzing product: 3400cm-1Left and right corresponds to the absorption peak of-OH,
l030cm-1Left and right corresponds to the absorption peak of C-OH, this two peak shows that this carbon ball surface has a large amount of-OH.2950cm-1Neighbouring
Small peak is caused by C-H stretching vibration.1707cm-1The stretching vibration of corresponding C=O, the presence of aldehyde radical should be in 2900-2700cm-1, but it is bimodal unobvious on spectrogram, therefore not can determine that the presence of aldehyde radical.1600cm-1It is to be caused by gripping olefin skeletal vibration altogether
's.1000-1500cm-1Between vibration may C-C or C-O-C skeletal vibration cause.1500cm-1And 1450cm-1It deposits at peak
Showing that glucose produces aromatization in hydrolytic process.Just due to these hydrophily functions of a large amount of-OH and C=O in carbon ball surface
The presence of group, improves its dispersibility, stability in aqueous solution, can be applied to biochemistry, catalyst carrier, system
Standby nuclear case structure hybridization material, hollow or porous material etc..
Embodiment two: it uses glucose as presoma the present invention also provides a kind of, nano carbon microsphere is prepared by hydro-thermal method
Method, the nano carbon microsphere are solid construction, and monodispersity is good, and surface is smooth, and free from admixture exists, and partial size is about 200nm, whole
Particle diameter distribution is relatively uniform on body, the preparation method of the nano carbon microsphere, comprising the following steps: step S1: directly in reaction kettle
A certain proportion of glucose solution is configured in liner, and liner is then fixed on autoclave back；Step S2: setting reaction
Condition does hydro-thermal reaction；Step S3: dark brown solution in kettle is filtered, clean, is dried to obtain nano carbon microsphere.
Preferably, the preparation method of the nano carbon microsphere, it is characterised in that in step S1: the Portugal 6g is weighed with electronic balance
Grape sugar is put into 50mL inner liner of reaction kettle, and 35mL deionized water is accurately pipetted with pipette, and (concentration of glucose solution is
It 0.78mol/L) is added in aforesaid reaction vessel, with glass bar agitating solution, dissolves glucose all, be then charged into reaction kettle
In, screw up with a wrench reaction kettle, is put into baking oven.
Preferably, the preparation method of the nano carbon microsphere, it is characterised in that in the step S2: setting reaction condition
For, 180 DEG C of temperature, reaction time 4-12 h.
Preferably, the preparation method of the nano carbon microsphere, it is characterised in that in the step S3: to after reaction,
It is down to room temperature, takes out reaction kettle, dark brown solution in kettle is filtered and (uses the organic filter membrane of 220nm), and is cleaned in reaction kettle in time
Lining, deionized water and washes of absolute alcohol to filtrate are colourless when suction filtration, and sample is wrapped with filter paper and is put into 70 in drying box
DEG C dry 4h.
The present invention uses glucose as presoma, is prepared by hydro-thermal method, and nano carbon microsphere obtained is solid construction, single
Favorable dispersibility, surface is smooth, and free from admixture exists, and partial size is about 200nm, and particle diameter distribution is relatively uniform on the whole；It is living with tradition
Property charcoal method of modifying compare, the present invention have it is easy to operate, high-efficient, product is purer, the series of advantages such as environmental-friendly；This hair
Bright process flow is simple, can continuous production raw material it is cheap, safe and non-toxic；Products therefrom partial size of the present invention is small to be evenly distributed, particle
Reunite light, good crystalline and it is controllable, be not required to high temperature sintering, eliminate grinding and thus bring impurity.
Particular embodiments described above, pair present invention solves the technical problem that, technical scheme and beneficial effects carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection scope.
Claims (5)
1. a kind of nano carbon microsphere, it is characterised in that: carbon ball is solid construction, and monodispersity is good, and surface is smooth, free from admixture, grain
Diameter is small, and particle diameter distribution is relatively uniform on the whole；This method prepares nano carbon microsphere in addition, spies such as density are high, intensity is high, surface area is big
Point, the carbon ball are many-sided all with good application prospect in lithium ion battery etc.；The preparation of the carbon ball is also disclosed in the present invention
Method.
2. a kind of nano carbon microsphere according to claim 1 and preparation method thereof, which comprises the following steps: step
Rapid S1: a certain proportion of glucose solution is configured in inner liner of reaction kettle, then liner is placed in autoclave；Step
S2: setting reaction condition completes hydro-thermal reaction；Step S3: dark brown solution in kettle is filtered, clean, is dried to obtain nano-sized carbon
Ball.
3. a kind of nano carbon microsphere according to claim 2 and preparation method thereof, it is characterised in that: in the step S1: using
Electronic balance weighs 6g glucose and is put into 50mL inner liner of reaction kettle, and 35mL deionized water (glucose is accurately pipetted with pipette
The concentration of solution is 0.78mol/L) it is added in aforesaid reaction vessel, with glass bar agitating solution, dissolve glucose all, so
It is fitted into reaction kettle afterwards, screw up with a wrench reaction kettle, is put into baking oven.
4. a kind of nano carbon microsphere according to claim 2 and preparation method thereof, it is characterised in that: in the step S2: setting
Determine reaction condition are as follows: 180 DEG C of temperature, reaction time 4-12 h.
5. a kind of nano carbon microsphere according to claim 2 and preparation method thereof, it is characterised in that: in the step S3: to
After reaction, it is down to room temperature, takes out reaction kettle, dark brown solution in kettle is filtered and (uses the organic filter membrane of 220nm), and is clear in time
Wash inner liner of reaction kettle, deionized water and washes of absolute alcohol to filtrate are colourless when suction filtration, and sample is wrapped with filter paper and is put into
70 DEG C of dry 4h in drying box.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591287A (en) * | 2019-09-06 | 2019-12-20 | 中国科学院兰州化学物理研究所 | Preparation method of epoxy resin-based nano composite material suitable for water lubrication working condition |
| CN113633576A (en) * | 2021-07-14 | 2021-11-12 | 郑小青 | Dandruff-removing itching-relieving hair washing composition |
| CN114289006A (en) * | 2021-12-06 | 2022-04-08 | 上海大学 | For Li-CO2Preparation method and application of battery carbon sphere catalyst |
| CN114813494A (en) * | 2022-06-24 | 2022-07-29 | 江苏省计量科学研究院(江苏省能源计量数据中心) | Application of carbon nanospheres and calibration method of PM2.5 mass concentration determinator |
-
2019
- 2019-06-11 CN CN201910500924.0A patent/CN110078050A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591287A (en) * | 2019-09-06 | 2019-12-20 | 中国科学院兰州化学物理研究所 | Preparation method of epoxy resin-based nano composite material suitable for water lubrication working condition |
| CN110591287B (en) * | 2019-09-06 | 2021-11-02 | 中国科学院兰州化学物理研究所 | Preparation method of epoxy resin-based nano composite material suitable for water lubrication working condition |
| CN113633576A (en) * | 2021-07-14 | 2021-11-12 | 郑小青 | Dandruff-removing itching-relieving hair washing composition |
| CN114289006A (en) * | 2021-12-06 | 2022-04-08 | 上海大学 | For Li-CO2Preparation method and application of battery carbon sphere catalyst |
| CN114813494A (en) * | 2022-06-24 | 2022-07-29 | 江苏省计量科学研究院(江苏省能源计量数据中心) | Application of carbon nanospheres and calibration method of PM2.5 mass concentration determinator |
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Application publication date: 20190802 |