CN108975310A - A kind of preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension and the hydro-thermal carbon ball of preparation - Google Patents
A kind of preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension and the hydro-thermal carbon ball of preparation Download PDFInfo
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- CN108975310A CN108975310A CN201811095913.0A CN201811095913A CN108975310A CN 108975310 A CN108975310 A CN 108975310A CN 201811095913 A CN201811095913 A CN 201811095913A CN 108975310 A CN108975310 A CN 108975310A
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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
- C01B32/15—Nano-sized carbon materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
Abstract
The present invention provides a kind of preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension and the hydro-thermal carbon ball of preparation, includes the following steps: S1, configuration glucose solution；S2, the step S1 glucose solution configured is put into autoclave, autoclave is sealed, and gas pressurized is passed through to 0.6~3.1MPa by the air inlet on autoclave；S3, the autoclave heating of step S2 is subjected to hydro-thermal reaction；S4, product obtained in step S3 is washed, is dry, obtaining hydro-thermal carbon ball.The present invention can efficiently prepare adjustable dimension in 60nm~2 μm, the hydro-thermal carbon ball of good dispersion, size uniformity, therefore can be improved the stability of carbon ball performance by changing pressure.
Description
Technical field
The invention belongs to micro-nano carbon ball preparation fields, more particularly to a kind of controllable hydro-thermal carbon ball of pressure auxiliary dimension
Preparation method and the hydro-thermal carbon ball of preparation.
Background technique
Hydro-thermal carbon ball is widely used in catalyst and carries because of its mild preparation condition and surface oxygen functional group abundant
Body, supercapacitor carry medicine, template and absorption aspect.Hydro-thermal carbon ball compared to traditional chemical vapor deposition, high temperature cabonization,
Arc discharge method preparation carbon ball is more environmentally protective, and used raw material such as glucose also has renewable, sustainable developability.
The homogeneity of controllable size and size is extremely important to the stability of carbon ball performance, however the carbon that traditional hydro-thermal method is prepared
Often dimensional controllability is poor for ball, adjustable dimension narrow range.Therefore, the efficient controllable and wider adjustable dimension range pair of size
The synthesis of hydro-thermal carbon ball is most important.
Up to the present, the example of only a small number of controlledly synthesis hydro-thermal carbon balls.For example, Sun and Li report passes through change
Concentration, hydro-thermal time and the temperature of glucose solution prepare size range in the carbon ball of 200nm~1.5 μm, and size is larger.
Chen and Li prepares monodisperse hydro-thermal carbon ball using two-step method, preparation~93nm carbon first in 0.1M glucose solution
Then carbon seed is put into secondary hydrothermal carbonization in 0.1M~0.4M glucose solution by seed, prepare size 167nm~
The preferable carbosphere of 400nm dispersibility, size are larger.Gong prepares hydro-thermal carbon as dispersing agent by addition Sodium Polyacrylate
Ball can obtain the carbon ball of the μ m in size range of 400nm~1 by extending the time, but this method introduced in hydrothermal system it is miscellaneous
It is difficult to increase subsequent cleaning for matter.Zhang prepares size range using ionic liquid as size controlling agent, by changing dosage
In the nitrogen-doped carbon nanosphere of 20~110nm size range, but the dispersibility of carbon ball is poor.Therefore, how do not introduce it is miscellaneous
Under the premise of matter, hydro-thermal carbon ball of the one kettle way controlledly synthesis from tens nanometers to several microns is still a technological difficulties, especially
It is the carbon ball for being less than 100nm, because its size is smaller, surface can be larger, in order to keep hydrothermal system more stable, presoma meeting
Quickly in its surface continued growth, finally grow up to the carbon ball greater than 100nm size.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of preparation of controllable hydro-thermal carbon ball of pressure auxiliary dimension
Method and the hydro-thermal carbon ball of preparation, to solve the problems, such as that carbon ball adjustable dimension is narrow in the prior art, dimensional controllability is poor.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension, includes the following steps:
S1, configuration glucose solution；
S2, the step S1 glucose solution configured is put into autoclave, autoclave is sealed, and by autoclave
Air inlet is passed through gas pressurized to 0.6~3.1MPa；
S3, the autoclave heating of step S2 is subjected to hydro-thermal reaction；
S4, product obtained in step S3 is washed, is dry, obtaining hydro-thermal carbon ball.
Preferably, in step S1, glucose concentration is 0.1M~2M.
Preferably, in step S3, the temperature of hydro-thermal reaction is 160~220 DEG C, and the time is 2~12h.
Preferably, in step S2, the gas being passed through is nitrogen, argon gas or carbon dioxide.
Preferably, in step S2, glucose solution dosage is the 1/3-2/3 of autoclave volume.
Preferably, in step S4, product washing is repeatedly ultrasonic, eccentric cleaning using dehydrated alcohol, deionized water, until
Cleaning solution is transparent.
Further, centrifugal speed is 3000~10000r/min, 20~30min of centrifugation time.
Preferably, drying is that the product after washing is put into vacuum oven, 60~80 DEG C of dry 6~12h.
A kind of hydro-thermal carbon ball that the preparation method is prepared, the diameter of hydro-thermal carbon ball are 60nm~2 μm.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention only need by change pressure, can efficiently prepare adjustable dimension 60nm~2 μm, good dispersion,
The hydro-thermal carbon ball of size uniformity.Reason is: the synthesis mechanism for being not pressurized hydro-thermal carbon ball is as follows, the H that glucose is separated out in water power+
Isomery generates 5 hydroxymethyl furfural by dehydration at fructose, fructose under ionic catalysis, then raw using polymerization-condensation-dehydration
At fragrant cluster, fragrant cluster erupts into carbon core after reaching critical supersaturation point, and the small molecule that carbon core absorbs in hydrolytic process is grown into
Carbon ball.After pressurization, water density increases, and can ionize out more H+Ion promotes glucose quickly to generate 5- methylol chaff
Aldehyde concentrates the subsequent nuclear blast hair stage more, and the carbon ball dimensional homogeneity of generation is more preferable.Simultaneously with the raising 5- hydroxyl of pressure
The yield of methyl furfural improves, and then generates more carbon cores, is limited by initial feed, carbon core is difficult to grow up.Side of the present invention
Method can be realized the controllable preparation of carbon ball, therefore can be improved the stability of carbon ball performance.Preparation method of the invention is not present
It is easy to reunite, introduces the technical problems such as impurity.
The diameter of hydro-thermal carbon ball prepared by the present invention is 60nm~2 μm, and diameter can control in 100nm hereinafter, dispersibility
Good, size uniformity can guarantee the stabilization of carbon ball performance.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of carbon ball obtained in the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of carbon ball obtained in the embodiment of the present invention 2；
Fig. 3 is the scanning electron microscope (SEM) photograph of carbon ball obtained in the embodiment of the present invention 3；
Fig. 4 is the scanning electron microscope (SEM) photograph of carbon ball obtained in the embodiment of the present invention 4.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The present invention is intended to provide a kind of method of the efficient control hydro-thermal carbon ball size of novel environment friendly, to realize that carbon ball is adjustable
Size range is wide, carbon ball monodispersity is good, size uniformity, and efficiency of pcr product is high, in favor of prepare with scale and industrial production.
The preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension of the present invention, includes the following steps:
S1, configuration glucose concentration are 0.1M~2M；
S2, the obtained glucose solution of step S1 is put into autoclave, autoclave is sealed, and by autoclave
Air inlet is passed through gas, makes 0.5~3.0MPa of pressure increase, that is, is forced into 0.6~3.1MPa；
S3, the autoclave of step S2 is heated at 160~220 DEG C after 2~12h of constant temperature, is cooled to room temperature；
S4, product obtained in step S3 is washed, is dry, obtaining target product.
In the step S2, the glucose solution, which is put in autoclave, uses thread seal.
The glucose solution dosage is the 1/3-2/3 of autoclave volume.
The pressurization is removed outside the self-produced pressure that autoclave pressure generates at room temperature, additional increased pressure.
In the step S4, product washing is to use dehydrated alcohol, deionized water ultrasound/eccentric cleaning repeatedly, until clear
Washing lotion is transparent.
The centrifugal speed is 3000~10000r/min, 20~30min of centrifugation time.
The drying is that the product after washing is put into vacuum oven, 60~80 DEG C of dry 6~12h.
Specific embodiment is as follows.
Embodiment 1
1) configuration glucose concentration is 1M；
2) the glucose solution 60mL for taking above-mentioned concentration, is put into the autoclave of 100mL, and sealing, being passed through nitrogen makes pressure
Increase 0.5MPa, be heated to 200 DEG C of constant temperature 12h, after reaction cooled to room temperature, obtains carbon ball solution.
3) above-mentioned solution is centrifugated with 3000r/min, and with dehydrated alcohol and deionized water repeatedly ultrasonic disperse, from
The heart, until cleaning solution is clarified.
4) carbon ball after above-mentioned cleaning is arrived into hydro-thermal carbon ball as 12h dry in 60 DEG C of vacuum ovens.
Fig. 1 show the scanning electron microscope (SEM) photograph of the carbon ball obtained of case study on implementation 1, and as can be seen from Figure, carbon ball size is equal
One, good dispersion, size is in 200nm or so.
Embodiment 2
1) configuration glucose concentration is 0.5M；
2) the glucose solution 60mL for taking above-mentioned concentration, is put into the autoclave of 100mL, and sealing, being passed through nitrogen makes pressure
Increase 1.0MPa, be heated to 180 DEG C of constant temperature 10h, after reaction cooled to room temperature, obtains carbon ball solution.
3) above-mentioned solution is centrifugated with 5000r/min, and with dehydrated alcohol and deionized water repeatedly ultrasonic disperse, from
The heart, until cleaning solution is clarified.
4) carbon ball after above-mentioned cleaning is arrived into hydro-thermal carbon ball as 12h dry in 60 DEG C of vacuum ovens.
Fig. 2 show the scanning electron microscope (SEM) photograph of the carbon ball obtained of case study on implementation 2, and as can be seen from Figure, carbon ball diameter is equal
One, good dispersion, size is in 800nm or so.
Embodiment 3
1) configuration glucose concentration is 0.5M；
2) the glucose solution 60mL for taking above-mentioned concentration, is put into the autoclave of 100mL, and sealing, being passed through carbon dioxide makes
Pressure increase 1.5MPa is heated to 180 DEG C of constant temperature 5h, after reaction cooled to room temperature, obtains carbon ball solution.
3) above-mentioned solution is centrifugated with 8000r/min, and with dehydrated alcohol and deionized water repeatedly ultrasonic disperse, from
The heart, until cleaning solution is clarified.
4) carbon ball after above-mentioned cleaning is arrived into hydro-thermal carbon ball as 12h dry in 60 DEG C of vacuum ovens.
Fig. 3 show the scanning electron microscope (SEM) photograph of the carbon ball obtained of case study on implementation 3, and as can be seen from Figure, carbon ball diameter is equal
One, good dispersion, size is in 400nm or so.
Embodiment 4
1) configuration glucose concentration is 1.5M；
2) the glucose solution 60mL for taking above-mentioned concentration, is put into the autoclave of 100mL, and sealing, being passed through nitrogen makes pressure
Increase 3.0MPa, be heated to 180 DEG C of constant temperature 3h, after reaction cooled to room temperature, obtains carbon ball solution.
3) above-mentioned solution is centrifugated with 10000r/min, and with dehydrated alcohol and deionized water repeatedly ultrasonic disperse,
Centrifugation, until cleaning solution is clarified.
4) carbon ball after above-mentioned cleaning is arrived into hydro-thermal carbon ball as 12h dry in 60 DEG C of vacuum ovens.
Fig. 4 show the scanning electron microscope (SEM) photograph of the carbon ball obtained of case study on implementation 4, and as can be seen from Figure, carbon ball diameter is equal
One, good dispersion, size is in 60nm or so.
Embodiment 5
1) configuration glucose concentration is 0.1M；
2) the glucose solution 33mL for taking above-mentioned concentration, is put into the autoclave of 100mL, and sealing, being passed through nitrogen makes pressure
2MPa is increased to, is heated to 160 DEG C of constant temperature 3h, after reaction cooled to room temperature, obtains carbon ball solution.
3) above-mentioned solution is centrifugated with 10000r/min, and with dehydrated alcohol and deionized water repeatedly ultrasonic disperse,
Centrifugation, until cleaning solution is clarified.
4) carbon ball after above-mentioned cleaning is arrived into hydro-thermal carbon ball as 10h dry in 70 DEG C of vacuum ovens.
Embodiment 6
1) configuration glucose concentration is 2M；
2) the glucose solution 40mL for taking above-mentioned concentration, is put into the autoclave of 100mL, and sealing, being passed through nitrogen makes pressure
Increase 2.5MPa, be heated to 170 DEG C of constant temperature 2h, after reaction cooled to room temperature, obtains carbon ball solution.
3) above-mentioned solution is centrifugated with 10000r/min, and with dehydrated alcohol and deionized water repeatedly ultrasonic disperse,
Centrifugation, until cleaning solution is clarified.
4) carbon ball after above-mentioned cleaning is arrived into hydro-thermal carbon ball as 8h dry in 75 DEG C of vacuum ovens.
Embodiment 7
1) configuration glucose concentration is 1.5M；
2) the glucose solution 50mL for taking above-mentioned concentration, is put into the autoclave of 100mL, and sealing, being passed through argon gas makes pressure
Increase 3.0MPa, be heated to 220 DEG C of constant temperature 2h, after reaction cooled to room temperature, obtains carbon ball solution.
3) above-mentioned solution is centrifugated with 10000r/min, and with dehydrated alcohol and deionized water repeatedly ultrasonic disperse,
Centrifugation, until cleaning solution is clarified.
4) carbon ball after above-mentioned cleaning is arrived into hydro-thermal carbon ball as 6h dry in 80 DEG C of vacuum ovens.
Claims (9)
1. a kind of preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension, which comprises the steps of:
S1, configuration glucose solution；
S2, the step S1 glucose solution configured is put into autoclave, autoclave is sealed, and pass through the air inlet on autoclave
Mouth is passed through gas pressurized to 0.6~3.1MPa；
S3, the autoclave heating of step S2 is subjected to hydro-thermal reaction；
S4, product obtained in step S3 is washed, is dry, obtaining hydro-thermal carbon ball.
2. the preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension according to claim 1, which is characterized in that step S1
In, glucose concentration is 0.1M~2M.
3. the preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension according to claim 1, which is characterized in that step S3
In, the temperature of hydro-thermal reaction is 160~220 DEG C, and the time is 2~12h.
4. the preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension according to claim 1, which is characterized in that step S2
In, the gas being passed through is nitrogen, argon gas or carbon dioxide.
5. the preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension according to claim 1, which is characterized in that step S2
In, glucose solution dosage is the 1/3-2/3 of autoclave volume.
6. the preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension according to claim 1, which is characterized in that step S4
In, product washing is repeatedly ultrasonic, eccentric cleaning using dehydrated alcohol, deionized water, until cleaning solution is transparent.
7. the preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension according to claim 6, which is characterized in that centrifugation speed
Degree is 3000~10000r/min, 20~30min of centrifugation time.
8. the preparation method of the controllable hydro-thermal carbon ball of pressure auxiliary dimension according to claim 1, which is characterized in that drying is
Product after washing is put into vacuum oven, 60~80 DEG C of dry 6~12h.
9. a kind of hydro-thermal carbon ball that the described in any item preparation methods of claim 1-8 are prepared, which is characterized in that hydro-thermal carbon
The diameter of ball is 60nm~2 μm.
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Cited By (8)
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| CN110368928A (en) * | 2019-07-29 | 2019-10-25 | 陕西科技大学 | A kind of catalyst and its preparation method and application for benzyl alcohol oxidation synthesizing benzaldehyde |
| CN111153396A (en) * | 2020-01-19 | 2020-05-15 | 南昌航空大学 | Method for preparing camellia seed husk carbon microspheres based on two-step hydrothermal method |
| CN112079347A (en) * | 2020-09-21 | 2020-12-15 | 陕西地建土地工程技术研究院有限责任公司 | Method for preparing nano carbon spheres by cooperation of pressure and dispersing agent |
| CN113336215A (en) * | 2020-03-02 | 2021-09-03 | 赵昆 | Preparation method and application of monodisperse hydrothermal carbon spheres |
| CN113648968A (en) * | 2021-08-31 | 2021-11-16 | 广东工业大学 | Macroscopic preparation method of oxygen-rich group superfine hydrothermal carbon spheres, prepared hydrothermal carbon sphere adsorbent and application |
| CN113697794A (en) * | 2021-08-31 | 2021-11-26 | 广东工业大学 | Method for preparing dendritic superfine hydrothermal carbon by slow temperature control method, prepared hydrothermal carbon adsorption ball and application |
| CN113980720A (en) * | 2021-11-19 | 2022-01-28 | 陕西科技大学 | Preparation method of carbon sphere/polyacrylamide/two-dimensional covalent organic polymer particles |
| CN115872402A (en) * | 2022-07-13 | 2023-03-31 | 武汉科技大学 | Hollow mesoporous carbon sphere self-assembly porous carbon microsphere and preparation method thereof |
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| CN110368928A (en) * | 2019-07-29 | 2019-10-25 | 陕西科技大学 | A kind of catalyst and its preparation method and application for benzyl alcohol oxidation synthesizing benzaldehyde |
| CN110368928B (en) * | 2019-07-29 | 2022-05-17 | 陕西科技大学 | Catalyst for synthesizing benzaldehyde by oxidizing benzyl alcohol and preparation method and application thereof |
| CN111153396A (en) * | 2020-01-19 | 2020-05-15 | 南昌航空大学 | Method for preparing camellia seed husk carbon microspheres based on two-step hydrothermal method |
| CN113336215A (en) * | 2020-03-02 | 2021-09-03 | 赵昆 | Preparation method and application of monodisperse hydrothermal carbon spheres |
| CN112079347A (en) * | 2020-09-21 | 2020-12-15 | 陕西地建土地工程技术研究院有限责任公司 | Method for preparing nano carbon spheres by cooperation of pressure and dispersing agent |
| CN113648968A (en) * | 2021-08-31 | 2021-11-16 | 广东工业大学 | Macroscopic preparation method of oxygen-rich group superfine hydrothermal carbon spheres, prepared hydrothermal carbon sphere adsorbent and application |
| CN113697794A (en) * | 2021-08-31 | 2021-11-26 | 广东工业大学 | Method for preparing dendritic superfine hydrothermal carbon by slow temperature control method, prepared hydrothermal carbon adsorption ball and application |
| CN113697794B (en) * | 2021-08-31 | 2023-08-08 | 广东工业大学 | Method for preparing dendritic superfine hydrothermal carbon by slow temperature control method, prepared hydrothermal carbon adsorption ball and application |
| CN113648968B (en) * | 2021-08-31 | 2023-08-22 | 广东工业大学 | Macroscopic quantity preparation method of oxygen-enriched group superfine hydrothermal carbon spheres, hydrothermal carbon sphere adsorbent prepared by using same and application of hydrothermal carbon sphere adsorbent |
| CN113980720A (en) * | 2021-11-19 | 2022-01-28 | 陕西科技大学 | Preparation method of carbon sphere/polyacrylamide/two-dimensional covalent organic polymer particles |
| CN113980720B (en) * | 2021-11-19 | 2022-04-29 | 陕西科技大学 | Preparation method of carbon sphere/polyacrylamide/two-dimensional covalent organic polymer particles |
| CN115872402A (en) * | 2022-07-13 | 2023-03-31 | 武汉科技大学 | Hollow mesoporous carbon sphere self-assembly porous carbon microsphere and preparation method thereof |
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