CN104944405A - Preparation method of carbon spheres - Google Patents

Preparation method of carbon spheres Download PDF

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Publication number
CN104944405A
CN104944405A CN201410117371.8A CN201410117371A CN104944405A CN 104944405 A CN104944405 A CN 104944405A CN 201410117371 A CN201410117371 A CN 201410117371A CN 104944405 A CN104944405 A CN 104944405A
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China
Prior art keywords
preparation
carbon ball
solution
glucose
glucose solution
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Pending
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CN201410117371.8A
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Inventor
谭余波
沈少华
封心建
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Abstract

The invention discloses a preparation method of carbon spheres, which comprises the following steps: s1. preparing a solution with the pH value of 3-10 from acid and alkali; s2. adding glucose into the solution obtained in the step s1 to prepare a 1-10g/100ml glucose solution; s3. putting the glucose solution obtained in the step s2 into a hydrothermal kettle, keeping the temperature at 160-200 DEG C for 2-20 hours, and cooling to room temperature; and s4. washing and drying the product obtained in the step s3 to obtain the target product. The method implements mass preparation and particle size control of carbon spheres with particle size of less than 100nm, does not have the participation of any organic solvent and toxic chemical reagent in the reaction process, can effectively avoid the problems of structure defects and environmental pollution caused by impurity introduction, and can be widely used for biochemical and biological diagnosis due to the nontoxic characteristic of the carbon spheres. The whole preparation process is simple to operate, has the advantages of high controllability, favorable repetitiveness and environment friendliness, and is suitable for large-scale production.

Description

A kind of preparation method of carbon ball
Technical field
The application belongs to Nano microsphere preparation field, particularly relates to the preparation method that a kind of diameter is 50 ~ 100nm carbon ball.
Background technology
Carbon ball is as a kind of new function carbon material, have that density is low, chemistry and thermostability is high, heat-conductivity conducting is good, intrinsic damp is good, specific surface area is controlled and the characteristic of the multiple excellence such as good biocompatibility, add its regular globosity, make carbon ball have huge potential using value in many new technical field such as gas storage, support of the catalyst, drug conveying, electrode material of secondary lithium ion battery, lightweight structural material, electrode material for super capacitor and fuel cells.
Current scholar has worked out the multiple method preparing carbon ball, as solvent (water) hot method, chemical Vapor deposition process, active metal reduction method, plasma method, polymer catalyzing pyrolysis method, ultrasonic heat solution etc.These methods are Shortcomings part more or less, and such as CVD, plasma method, ultrasonic heat solution all need the specific equipment of complex and expensive; The hard carbon material of what polymer catalyzing pyrolysis method obtained is approximate ellipsoidal on micro-meter scale, and usually there is impurity; Active metal reduction rule needs protective atmosphere; Hydrothermal method wherein refers in the pressurized vessel of sealing, take water as solvent, the chemical reaction carried out under the condition of High Temperature High Pressure.It is simple to operate, and working conditions is gentle, can prepare in a large number.And surperficial because of containing a large amount of active oxy radical by the carbon ball that biomass by hydro-thermal method is obtained, new function carbon material can be formed with different kinds of molecules, ion and other functional groups.
To take glucose as carbon source prepare carbon ball by hydrothermal method dehydration carbonization is the most controlled method.But most organic solvent is prepared in the process of carbon material to be needed to add various catalyzer, and raw material and product are all toxic, not environmentally.In addition, most is at present at least hundreds of nanometer even micron order by the carbon spherolite footpath of water heat transfer, cannot prepare carbon ball (Angew. Chem.-Int. Edit., 2004,597 of particle diameter at 100 below nm; J Mater Res., 2012,1117., Adv. Mater., 2010,813), this severely limits small size carbon ball (100 below nm) at transparent optical device as the widespread use in dye sensitization solar battery, electrochromic device.
Summary of the invention
Order of the present invention is the preparation method providing a kind of carbon ball, with solve apparatus expensive in prior art, size large, there is the technical problems such as impurity.
For achieving the above object, the invention provides following technical scheme:
The embodiment of the present application discloses a kind of preparation method of carbon ball, comprising:
S1, with bronsted lowry acids and bases bronsted lowry preparation pH value be the solution of 3 ~ 10;
Add glucose in s2, the solution that obtains in step s1, compound concentration is the glucose solution of 1-10g/100ml;
S3, the glucose solution obtained by step s2 are put into water heating kettle and be incubated 2 ~ 20 hours at 160 ~ 200 DEG C of temperature, are cooled to room temperature;
S4, product that step s3 obtains is washed, dry, obtain target product.
Preferably, in the preparation method of above-mentioned carbon ball, in described step s1, described acid is dilute hydrochloric acid, and described alkali is weak ammonia.
Preferably, in the preparation method of above-mentioned carbon ball, in described step s3, described glucose solution is contained in polytetrafluoroethylliner liner, and described polytetrafluoroethylliner liner is sealed in described water heating kettle.
Preferably, in the preparation method of above-mentioned carbon ball, described glucose solution is the 30-70% of described polytetrafluoroethylliner liner volume.
Preferably, in the preparation method of above-mentioned carbon ball, described step s4 specifically comprises: step s3 is obtained product centrifugation and collect, then repeatedly rinse with dehydrated alcohol and deionized water respectively, finally dry in an oven, obtain final product carbon ball.
Preferably, in the preparation method of above-mentioned carbon ball, the speed of described centrifugation is 10000-15000r/min, and centrifugation time is 10-20 minute.
Preferably, in the preparation method of above-mentioned carbon ball, described is that ultrasonic disperse washs by the means that dehydrated alcohol and deionized water rinse repeatedly.
Preferably, in the preparation method of above-mentioned carbon ball, the temperature of drying in described baking oven is 80 ~ 100 DEG C, and the time is 4 ~ 20 hours.
Compared with prior art, the invention has the advantages that: the present invention is at lesser temps and achieve in the short period that spheroid is complete, monodispersity good, Absorbable organic halogens stores, particle diameter is in the preparation of the carbon nanometer micro ball of 100 below nm.And the diameter of Nano microsphere can regulate and control in 50-100nm.And temperature of reaction is lower, the reaction times is short, improves production efficiency, reduces production cost.
A key character lower than the nanoparticle of 100 nm be its size oneself close to or be less than the mean free path of electronics and superconduction and be concerned with wavelength, their larger specific surface make to be in the atom of surface state and number of electrons oneself be in the atom of granule interior, number of electrons is suitable.Surface effects caused thus and quantum confined effect will have a huge impact the optical characteristics of nanoparticle, even make nanoparticle have new optical characteristics not available for its block materials, as wide band absorption and blue-shifted phenomenon etc.
When preparing as being expected to during template the laminated film that thickness is 100 below nm with the carbon ball of this size, and the characteristic that the quantum size effect, small-size effect, surface effects, macro quanta tunnel effect etc. of the nanophase particle of this film make their aspect such as optical property, electric property, mechanical property, catalytic performance, biological property present conventional material not to be possessed.Therefore, nano compound film all has wide practical use in every field such as photoelectric technology, biotechnology, energy technologys.When the particle size of metal or semi-conductor is reduced to nanometer range, its electrical properties can be undergone mutation, and magnetic, optical property, photoelectric property generally also have special performance simultaneously.Its reason is that electronic level there occurs change, and metal becomes discrete energy level from quasi-continuum of level, and the bandwidth of semi-conductor also enlarges markedly.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present application or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the application, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 in the embodiment of the present invention 1 obtain the transmission electron microscope photo of carbon ball;
Fig. 2 in the embodiment of the present invention 2 obtain the transmission electron microscope photo of carbon ball;
Fig. 3 in the embodiment of the present invention 3 obtain the transmission electron microscope photo of carbon ball;
Fig. 4 in the embodiment of the present invention 4 obtain the transmission electron microscope photo of carbon ball;
Fig. 5 in the embodiment of the present invention 5 obtain the transmission electron microscope photo of carbon ball.
Embodiment
The present invention aims to provide the preparation method that a kind of novel environmental protection diameter is less than 100nm carbon ball, uses and realizes spheroid rounding, monodispersity is good, Absorbable organic halogens stores, prepared by the hydrothermal method of the carbon ball of size tunable.Existing methods condition is optimized simultaneously; while guarantee final product quality; preferentially choose the experiment condition that the reaction times is short, raw material usage is few, temperature of reaction is low as far as possible; enhance productivity, reduce production cost; and overcome problems such as in the past preparing in small size carbon ball easily reunion, be beneficial to mass-producing preparation and practical application.
The present invention is described further by the following example: according to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material ratio, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
embodiment 1
1) regulate the pH of dual deionized water to be 3 with dilute hydrochloric acid, it can be used as solvent, dissolve in glucose, be mixed with the glucose solution that concentration is 8g/100ml;
2) get appropriate above-mentioned glucose solution and be placed on 25ml specification and with in teflon-lined stainless steel cauldron, and be placed in 180 DEG C of baking ovens and react 4 hours, naturally cool to room temperature, obtain carbon ball solution;
3) by above-mentioned solution through centrifugation, and to wash with deionized water and dehydrated alcohol ultrasonic disperse, till centrifugal rear dispersion liquid clarification;
4) above-mentioned centrifugal rear gained solid is placed in 80 DEG C of vacuum drying ovens dry 8 hours, namely obtains carbon ball.
Figure 1 shows that the transmission electron microscope photo of the carbon ball that embodiment 1 obtains, as can be seen from Figure, the diameter Distribution of carbon ball is between 50-70 nm.
embodiment 2
1) regulate the pH of dual deionized water to be 6 with dilute hydrochloric acid, it can be used as solvent, dissolve in glucose, be mixed with the glucose solution that concentration is 8g/100ml;
2) get appropriate above-mentioned glucose solution and be placed on 25ml specification and with in teflon-lined stainless steel cauldron, and be placed in 180 DEG C of baking ovens and react 4 hours, naturally cool to room temperature, obtain carbon ball solution;
3) by above-mentioned solution through centrifugation, and to wash with deionized water and dehydrated alcohol ultrasonic disperse, till centrifugal rear dispersion liquid clarification;
4) above-mentioned centrifugal rear gained solid is placed in 80 DEG C of vacuum drying ovens dry 8 hours, namely obtains carbon ball.
Figure 2 shows that the transmission electron microscope photo of the carbon ball that embodiment 2 obtains, as can be seen from Figure, the diameter Distribution of carbon ball is between 60-80 nm.
embodiment 3
1) regulate the pH of dual deionized water to be 9 with dilute hydrochloric acid, it can be used as solvent, dissolve in glucose, be mixed with the glucose solution that concentration is 8g/100ml;
2) get appropriate above-mentioned glucose solution and be placed on 25ml specification and with in teflon-lined stainless steel cauldron, and be placed in 180 DEG C of baking ovens and react 4 hours, naturally cool to room temperature, obtain carbon ball solution;
3) by above-mentioned solution through centrifugation, and to wash with deionized water and dehydrated alcohol ultrasonic disperse, till centrifugal rear dispersion liquid clarification;
4) above-mentioned centrifugal rear gained solid is placed in 80 DEG C of vacuum drying ovens dry 8 hours, namely obtains carbon ball.
Figure 3 shows that the transmission electron microscope photo of the carbon ball that embodiment 3 obtains, as can be seen from Figure, the diameter Distribution of carbon ball is between 65-90 nm.
embodiment 4
1) regulate the pH of dual deionized water to be 7 with dilute hydrochloric acid and weak ammonia, it can be used as solvent, dissolve in glucose, be mixed with the glucose solution that concentration is 4g/100ml;
2) get appropriate above-mentioned glucose solution and be placed on 25ml specification and with in teflon-lined stainless steel cauldron, and be placed in 180 DEG C of baking ovens and react 4 hours, naturally cool to room temperature, obtain carbon ball solution;
3) by above-mentioned solution through centrifugation, and to wash with deionized water and dehydrated alcohol ultrasonic disperse, till centrifugal rear dispersion liquid clarification;
4) above-mentioned centrifugal rear gained solid is placed in 80 DEG C of vacuum drying ovens dry 8 hours, namely obtains carbon ball.
Figure 4 shows that the transmission electron microscope photo of the carbon ball that embodiment 4 obtains, as can be seen from Figure, the diameter Distribution of carbon ball is between 70-90nm.
embodiment 5
1) regulate the pH of dual deionized water to be 7 with dilute hydrochloric acid and weak ammonia, it can be used as solvent, dissolve in glucose, be mixed with the glucose solution that concentration is 8g/100ml;
2) get appropriate above-mentioned glucose solution and be placed on 25ml specification and with in teflon-lined stainless steel cauldron, and be placed in 180 DEG C of baking ovens and react 4 hours, naturally cool to room temperature, obtain carbon ball solution;
3) by above-mentioned solution through centrifugation, and to wash with deionized water and dehydrated alcohol ultrasonic disperse, till centrifugal rear dispersion liquid clarification;
4) above-mentioned centrifugal rear gained solid is placed in 80 DEG C of vacuum drying ovens dry 8 hours, namely obtains carbon ball.
Figure 5 shows that the transmission electron microscope photo of the carbon ball that embodiment 5 obtains, as can be seen from Figure, the diameter Distribution of carbon ball is between 70-100nm.
The inventive method achieves and be less than 100 nm carbon balls and prepare in large quantity and size control, the participation of reaction process organic solvent-free and toxic chemical, can not only effectively avoid introducing by impurity the textural defect and problem of environmental pollution that cause, simultaneously due to the characteristic that this carbon ball is nontoxic, biological chemistry and biological diagnosis can be widely used in.Whole preparation process is simple to operate, and controllability is strong, reproducible, environmental protection, is applicable to scale operation.
It should be noted that, in this article, the such as relational terms of first and second grades and so on is only used for an entity or operation to separate with another entity or operational zone, and not necessarily requires or imply the relation that there is any this reality between these entities or operation or sequentially.And, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.When not more restrictions, the key element limited by statement " comprising ... ", and be not precluded within process, method, article or the equipment comprising described key element and also there is other identical element.
The above is only the embodiment of the application; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the application's principle; can also make some improvements and modifications, these improvements and modifications also should be considered as the protection domain of the application.

Claims (7)

1. a preparation method for carbon ball, is characterized in that, comprising:
S1, with dilute hydrochloric acid and weak ammonia preparation pH value be the solution of 3 ~ 10;
Add glucose in s2, the solution that obtains in step s1, compound concentration is the glucose solution of 1-10g/100ml;
S3, the glucose solution obtained by step s2 are put into water heating kettle and be incubated 2 ~ 20 hours at 160 ~ 200 DEG C of temperature, are cooled to room temperature;
S4, product that step s3 obtains is washed, dry, obtain target product.
2. the preparation method of carbon ball according to claim 1, it is characterized in that: in described step s3, described glucose solution is contained in polytetrafluoroethylliner liner, and described polytetrafluoroethylliner liner is sealed in described water heating kettle.
3. the preparation method of carbon ball according to claim 2, is characterized in that: described glucose solution is the 30-70% of described polytetrafluoroethylliner liner volume.
4. the preparation method of carbon ball according to claim 1, it is characterized in that: described step s4 specifically comprises: step s3 is obtained product centrifugation and collect, then repeatedly rinse with dehydrated alcohol and deionized water respectively, finally dry in an oven, obtain final product carbon ball.
5. the preparation method of carbon ball according to claim 4, is characterized in that: the speed of described centrifugation is 10000-15000r/min, and centrifugation time is 10-20 minute.
6. the preparation method of carbon ball according to claim 4, is characterized in that: described is that ultrasonic disperse washs by the means that dehydrated alcohol and deionized water rinse repeatedly.
7. the preparation method of carbon ball according to claim 4, is characterized in that: the temperature of drying in described baking oven is 80 ~ 100 DEG C, and the time is 4 ~ 20 hours.
CN201410117371.8A 2014-03-27 2014-03-27 Preparation method of carbon spheres Pending CN104944405A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105582888A (en) * 2016-01-21 2016-05-18 西南科技大学 Method for preparing carbon microsphere adsorbent under catalysis of metal salt with low-temperature hydrothermal method
CN106185865A (en) * 2016-07-19 2016-12-07 西安交通大学 A kind of preparation method of hollow nano carbon microsphere
CN109516457A (en) * 2018-12-05 2019-03-26 华南师范大学 A kind of chitosan-based porous carbon ball and preparation method thereof
CN110395729A (en) * 2019-08-27 2019-11-01 贵州大学 A kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane
CN110408190A (en) * 2019-07-30 2019-11-05 湖北大学 Preparation method, product and the purposes of ultraviolet resistance radiation carbon ball modified polyurethane
CN111170296A (en) * 2020-03-30 2020-05-19 天津大学 Method for preparing carbon spheres by using low-temperature plasma to carbonize monosaccharides
CN111710882A (en) * 2020-06-28 2020-09-25 金汤杰 Process for preparing lithium battery negative electrode material by using waste zinc-manganese battery
CN113511688A (en) * 2021-08-25 2021-10-19 杭州恒毅智创科技有限公司 FeVO4Preparation method of hollow sphere
CN114015427A (en) * 2021-11-08 2022-02-08 中海油田服务股份有限公司 Nano oil displacement agent and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
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CN102173405A (en) * 2010-12-24 2011-09-07 苏州方昇光电装备技术有限公司 Preparation method of carbon nanoparticle with controllable photoluminescence
US20120178099A1 (en) * 2011-01-10 2012-07-12 Indian Association For The Cultivation Of Science Highly fluorescent carbon nanoparticles and methods of preparing the same
CN102765712A (en) * 2012-07-09 2012-11-07 陕西科技大学 Method for preparing carbon microspheres
CN103641101A (en) * 2013-12-19 2014-03-19 上海交通大学 Two-dimensional structural carbon nanomaterial and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173405A (en) * 2010-12-24 2011-09-07 苏州方昇光电装备技术有限公司 Preparation method of carbon nanoparticle with controllable photoluminescence
US20120178099A1 (en) * 2011-01-10 2012-07-12 Indian Association For The Cultivation Of Science Highly fluorescent carbon nanoparticles and methods of preparing the same
CN102765712A (en) * 2012-07-09 2012-11-07 陕西科技大学 Method for preparing carbon microspheres
CN103641101A (en) * 2013-12-19 2014-03-19 上海交通大学 Two-dimensional structural carbon nanomaterial and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105582888A (en) * 2016-01-21 2016-05-18 西南科技大学 Method for preparing carbon microsphere adsorbent under catalysis of metal salt with low-temperature hydrothermal method
CN106185865A (en) * 2016-07-19 2016-12-07 西安交通大学 A kind of preparation method of hollow nano carbon microsphere
CN109516457A (en) * 2018-12-05 2019-03-26 华南师范大学 A kind of chitosan-based porous carbon ball and preparation method thereof
CN110408190A (en) * 2019-07-30 2019-11-05 湖北大学 Preparation method, product and the purposes of ultraviolet resistance radiation carbon ball modified polyurethane
CN110395729A (en) * 2019-08-27 2019-11-01 贵州大学 A kind of preparation method for the ultra micro mesoporous activated carbon ball adsorbing coal bed gas methane
CN110395729B (en) * 2019-08-27 2022-05-17 贵州大学 Preparation method of ultramicropore activated carbon spheres for adsorbing coal bed methane
CN111170296A (en) * 2020-03-30 2020-05-19 天津大学 Method for preparing carbon spheres by using low-temperature plasma to carbonize monosaccharides
CN111710882A (en) * 2020-06-28 2020-09-25 金汤杰 Process for preparing lithium battery negative electrode material by using waste zinc-manganese battery
CN113511688A (en) * 2021-08-25 2021-10-19 杭州恒毅智创科技有限公司 FeVO4Preparation method of hollow sphere
CN114015427A (en) * 2021-11-08 2022-02-08 中海油田服务股份有限公司 Nano oil displacement agent and preparation method and application thereof

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Application publication date: 20150930