CN106430147B - A kind of Ultrasound-microwave preparation has the functional mesoporous hollow carbon sphere of open architecture - Google Patents
A kind of Ultrasound-microwave preparation has the functional mesoporous hollow carbon sphere of open architecture Download PDFInfo
- Publication number
- CN106430147B CN106430147B CN201610574730.1A CN201610574730A CN106430147B CN 106430147 B CN106430147 B CN 106430147B CN 201610574730 A CN201610574730 A CN 201610574730A CN 106430147 B CN106430147 B CN 106430147B
- Authority
- CN
- China
- Prior art keywords
- silica composite
- carbon
- open architecture
- composite nano
- medium hole
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention discloses the functional mesoporous hollow Nano carbon balls that a kind of preparation of Ultrasound-microwave has open architecture.Belong to mesoporous material preparation field.Method particularly includes: 3- amino phenols, paraformaldehyde, silicic acid are added separately to carry out the ultrasonic reaction of certain power in water and organic solvent mixed-alkali solvent in suitable surfactant, generate the polymeric/silica composite mesopore hollow nano-sphere with " penetration twin " structure.Microwave carbonization is carried out to polymeric/silica composite mesopore hollow nano-sphere with microwave equipment, obtains that there is the carbon of specific structure and pattern/silica composite mesopore hollow nano-sphere.The silica in the composite material is removed, the functional mesoporous hollow Nano carbon ball with open architecture is obtained.The product can be used for supercapacitor, lithium ion battery, catalyst carrier, lithium-sulfur cell, medicament transport, bio-imaging, the multiple fields such as water process.
Description
Technical field
The present invention relates to the functional mesoporous hollow carbon spheres that a kind of preparation of Ultrasound-microwave has open architecture, belong to Jie
Hole field of nano material preparation.
Background technique
In the 1940s, the superiority of natural porous material is by it has been found that started artificial synthesized porous material
Upsurge.International pure and applied chemistry federation (International Union of Pure and Applied
Chemistry, IUPAC) porous material is divided into poromerics, mesoporous material and large pore material, wherein aperture is less than the hole of 2nm
Referred to as micropore, aperture is referred to as mesoporous between the hole of 2~50nm, and hole of the aperture greater than 50nm is known as macropore.In numerous porous materials
In, porous carbon materials are because of high-specific surface area, high porosity, good electric conductivity and thermal conductivity, regulatable aperture and superficiality
Many advantages, such as energy, is widely used in fields such as catalyst carrier, supercapacitor, catalyst, adsorbent and gas storages.
Porous carbon materials refer to the carbon material with Different Pore Structures, and aperture can be according to the requirement of practical application (such as
Institute's binding molecule size etc.) regulated and controled, so that its size is in nanometer level microporous between micron order macropore.Porous carbon ball material
Preparation method it is varied, common preparation method has two classes: activation method and template, template be divided into again hard template method and
Soft template method.Wherein not only step is more under normal conditions for hard template method, and it is cumbersome it is time-consuming (J.Mater.Chem., 2011,21,
5290.Adv.Mater.2010,22,838.J.Phys.Chem.C,2011,115,17717.Adv.Mater.2014,26,
4294.Nat.Nanotechnol.2014,9,618.Adv.Mater.2014,26,3176.Adv.Mater.2014,26,
3741.).And utilize the usual pattern of the obtained material of soft template method it is inhomogenous (Chem.Commun.2008,
2629.J.Am.Chem.Soc.2007,129,14576.J.Am.Chem.Soc.2010,132,
15144.Nat.Mater.2014,13,293.Nat.Commun.2014,4,2798.Nanoscale,2016,8,451.).It is right
For functionalization hollow carbon sphere, the method that current preparation method predominantly stays in hard template, other are including soft template
The also rare report of simple preparation method.The problems such as at high cost, synthesis technology is complicated, time-consuming existing for these conventional methods,
Hinder the development of porous carbon materials.
Summary of the invention
The technical problem to be solved by the present invention is to prepare the functional mesoporous carbon ball material of high quality, furthermore utilize easy way
Diameter synthesizes the uniform, monodisperse of height and nucleocapsid precision is controllable, especially has open skeleton structure and its Jie interconnected
Hole path.Provide a kind of functional mesoporous hollow carbon sphere of the Ultrasound-microwave preparation with open architecture.
The invention is realized by the following technical scheme, includes the following steps:
Step 1: it is separately added into water, organic solvent and basic catalyst in reaction vessel, is then separately added into 3- amino again
Phenol, paraformaldehyde, surfactant；
Step 2: then the mixed solution that ultrasound is above-mentioned, and silicate solution is added, the sediment of reaction is to have " to pass through
Wear twin " polymeric/silica composite Nano medium hole hollow ball of structure；
Step 3: microwave is carried out to polymeric/silica composite Nano medium hole hollow ball with microwave reactor
Carbon/silica composite Nano medium hole hollow ball can be obtained in carbonization treatment；
Step 4: dioxy in carbon elimination/silica composite Nano medium hole hollow ball is removed with hydrofluoric acid or dense aqueous slkali
SiClx can be obtained the functional mesoporous hollow carbon sphere with open architecture.
Wherein organic solvent is one of ethyl alcohol, ether, ethylene glycol, propyl alcohol or isopropyl acetone；Wherein water and organic solvent
Volume ratio be 1:0.01~100.Wherein basic catalyst is that all can ionize in water and generate the examination of hydroxide ion
Agent.Wherein basic catalyst is one of KOH, NaOH or ammonium hydroxide；Wherein surfactant is cetyl trimethyl chlorination
Ammonium, cetyl trimethylammonium bromide, nonionic surface active agent F127 or P123 are one or more kinds of, and silicic acid is positive silicon
One or more of propyl propionate, ethyl orthosilicate or non-hydrate sodium metasilicate；Wherein ultrasonic time is 3-25 minutes, and power is
100-2000W is directly stirred 12-24 hours；Microwave carbonization time is 10-500 minutes, and power is 300~3000W.It can also
To use common tube formula furnace to be carbonized, 400-1200 DEG C of carburizing temperature, soaking time 0.5-20 hours.
Beneficial effect
1, the present invention be a kind of method for preparing the functional mesoporous hollow carbon sphere with open architecture, it is easy to operate, at
This is lower, and substantially reduces the reaction time, it can be achieved that extensive quickly production.
2, the present invention provides a kind of method for preparing the functional mesoporous hollow carbon sphere with open architecture, pass through adjusting
The different-shape carbon nanomaterial with open architecture can be obtained in the proportion of water and alcohols reaction dissolvent.
3, the present invention provides a kind of methods for preparing the functional mesoporous hollow carbon sphere with open architecture, have higher
Surface area (> 2500m2/ g) and pore volume (> 3.2cm3/ g) more adsorbable active sites, and pore-size distribution aperture point are provided
It is adjustable in cloth (3.5nm-36nm) and porosity a certain range.
4, the material prepared by the present invention can be by with catalyst carrier, supercapacitor, catalyst, adsorbent and gas
The numerous areas such as storage.
Detailed description of the invention
Fig. 1 is the flow diagram of preparation method of the present invention；
Fig. 2 is the scanning electron microscope (SEM) of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1
Fig. 2 a and transmission electron microscope (TEM) Fig. 2 b and corresponding amplification factor Fig. 2 c；
Fig. 3 is the XRD diagram of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1；
Fig. 4 is the XPS figure of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1；
Fig. 5 is the Raman spectrogram of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1；
Fig. 6 is the specific surface area distribution of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1
Fig. 6 (a) and pore volume distribution Fig. 6 (b)；
Fig. 7 is the scanning electron microscope (SEM) of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 2
Fig. 7 a and transmission electron microscope (TEM) Fig. 7 b and corresponding amplification factor Fig. 7 c；
Fig. 8 is the scanning electron microscope (SEM) of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 3
Fig. 8 a and transmission electron microscope (TEM) Fig. 8 b and corresponding amplification factor Fig. 8 c.
Fig. 9 is the scanning electron microscope (SEM) of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 3
Fig. 9 a and transmission electron microscope (TEM) Fig. 9 b and corresponding amplification factor Fig. 9 c.
Specific embodiment
Embodiment 1
Step 1: being separately added into 8mL ethyl alcohol, 21mL water and 0.3mL mass concentration in reaction vessel is 25%~30%
Then ammonia spirit is separately added into the 3- amino phenols, 0.18g paraformaldehyde and 0.5g hexadecyltrimethylammonium chloride of 0.3g again
(CTAC)；
Step 2: mixed solution is placed in ultrasonic transmitter addition 1.5mL positive silicic acid propyl ester in 500W ultrasonic procedure
(TPOS) solution, and continual ultrasonic 5 minutes, the sediment of reaction be have the polymeric of " penetration twin " structure/
Silica composite Nano medium hole hollow ball；
Step 3: above-mentioned reaction product 500W microwave reactor standing wave is reacted 140 minutes, can be obtained has
The carbon of open architecture/silica composite Nano medium hole hollow ball；
Step 4: removing silica in carbon elimination/silica composite Nano medium hole hollow ball with 5% hydrofluoric acid solution, and
Obtained solid powder after the abundant cleaning, drying of hydrofluoric acid is as had to the functional mesoporous hollow carbon of open architecture with distilled water
Ball.(N-MHCSs-260 for being shown in Table 2 that material prepared pattern is shown in attached drawing 2 and specific surface area and pore volume numerical value)
Product identification
The element percentage composition of the prepared functional mesoporous hollow carbon sphere with open architecture in 1. embodiment 1 of table
| Sample | C wt% | N wt% | O wt% | F wt% | Si wt% |
| N-MHCSs-260 | 91.07 | 4.28 | 3.97 | 0.05 | 0.63 |
Table 1 is that the element of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1 forms table.From
As can be seen that the main component of obtained carbon ball is C, N, O in table.
Fig. 2 is the scanning electron microscope (SEM) of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1
Fig. 2 a and transmission electron microscope (TEM) Fig. 2 b and corresponding amplification factor Fig. 2 c；
Fig. 3 is the XRD diagram of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1.It is shown in figure
Show that two wide characteristic peaks are located at 2 θ=26 °, corresponding crystal face (002)；2 θ=44 °, crystal face are corresponding (101).These diffraction
Face is that hexagon graphite (JCPDS card no.41-1487) is distinctive, shows the really carbon material of material obtained；
Fig. 4 is the XPS figure of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1.N member in figure
The peak of element shows that obtained carbon ball is the carbon ball of functionalization.
Fig. 5 is the Raman spectrogram of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1.Table
The degree of graphitization of bright obtained carbon ball is higher.
Fig. 6 is the specific surface area distribution of the functional mesoporous hollow carbon sphere with open architecture prepared in embodiment 1
Fig. 6 (a) and pore volume distribution Fig. 6 (b)；
Table 2 shows the specific surface area and pore volume numerical value of N-MHCSs-260；It can be seen that obtained carbon ball is with very high
Specific surface area, up to 2500m2/ g, and with it is mesoporous based on.
Embodiment 2
Step 1: being separately added into 7mL propyl alcohol, 21mL water and 0.3mL mass concentration in the reaction vessel is 25%~30%
Ammonia spirit, be then separately added into the 3- amino phenols, 0.18g paraformaldehyde, 0.5g cetyl trimethyl chlorination of 0.3g again
Ammonium (CTAC) and 1.2g non-hydrate sodium metasilicate (Na2SiO3·9H2O)；
Step 2: mixed solution is placed in ultrasonic transmitter, and 360W continual ultrasonic 10 minutes, the sediment of reaction was
Polymeric with " penetration twin " structure/silica composite Nano medium hole hollow ball；
Step 3: above-mentioned reaction product 500W microwave reactor standing wave is reacted 180 minutes, can be obtained has
The carbon of open architecture/silica composite Nano medium hole hollow ball；
Step 4: silica in carbon elimination/silica composite Nano medium hole hollow ball is removed with 6M NaOH solution, is used in combination
Obtained solid powder is the functional mesoporous hollow carbon sphere with open architecture after the abundant cleaning, drying of distilled water.It is (prepared
Material morphology is shown in the N-MHCSs-180 for being shown in Table 2 of attached drawing 7 and specific surface area and pore volume numerical value)
Embodiment 3
Step 1: being separately added into 6mL ethyl alcohol, 21mL water and 0.3mL mass concentration in reaction vessel is 25%~30%
Then ammonia spirit is separately added into the 3- amino phenols, 0.18g paraformaldehyde and 0.5g hexadecyltrimethylammonium chloride of 0.3g again
(CTAC)；
Step 2: mixed solution is placed in ultrasonic transmitter addition 1.5mL positive silicic acid propyl ester in 270W ultrasonic procedure
(TPOS) solution, and continual ultrasonic 15 minutes, the sediment of reaction be have the polymeric of " penetration twin " structure/
Silica composite Nano medium hole hollow ball；
Step 3: above-mentioned reaction product 1000W microwave reactor standing wave is reacted 30 minutes, can be obtained has
The carbon of open architecture/silica composite Nano medium hole hollow ball；
Step 4: removing silica in carbon elimination/silica composite Nano medium hole hollow ball with 5% hydrofluoric acid solution, and
It is the functional mesoporous hollow carbon sphere with open architecture with obtained solid powder after the abundant cleaning, drying of distilled water.It is (made
Standby material morphology is shown in the N-MHCSs-90 for being shown in Table 2 of attached drawing 8 and specific surface area and pore volume numerical value)
In 2. embodiment 1,2,3 of table the specific surface area of the prepared functional mesoporous hollow carbon sphere with open architecture and
Pore volume feature
Embodiment 4
Step 1: be separately added into the reaction vessel 6mL isopropyl acetone, 18mL water and 0.2mL mass concentration be 25%~
Then 30% ammonia spirit is separately added into the 3- amino phenols, 0.18g paraformaldehyde, 0.5g cetyl trimethyl of 0.3g again
Ammonium chloride (CTAC) and 1.2g non-hydrate sodium metasilicate (Na2SiO3·9H2O)；
Step 2: mixed solution is placed in ultrasonic transmitter, and 360W continual ultrasonic 5 minutes, the sediment of reaction was
Polymeric with " penetration twin " structure/silica composite Nano medium hole hollow ball；
Step 3: above-mentioned reaction product 800W microwave reactor standing wave is reacted 140 minutes, can be obtained has
The carbon of open architecture/silica composite Nano medium hole hollow ball；
Step 4: silica in carbon elimination/silica composite Nano medium hole hollow ball is removed with the NaOH solution of 6M, is used in combination
Obtained solid powder is the functional mesoporous hollow carbon sphere with open architecture after the abundant cleaning, drying of distilled water.
Embodiment 5
Step 1: being separately added into 7mL ethyl alcohol, 17mL water and 0.2mL mass concentration in reaction vessel is 25%~30%
Then ammonia spirit is separately added into the 3- amino phenols, 0.18g paraformaldehyde and 0.5g hexadecyltrimethylammonium chloride of 0.3g again
(CTAC)；
Step 2: mixed solution is placed in ultrasonic transmitter addition 1.5mL positive silicic acid propyl ester in 900W ultrasonic procedure
(TPOS) solution, and continual ultrasonic 6 minutes, the sediment of reaction be have the polymeric of " penetration twin " structure/
Silica composite Nano medium hole hollow ball；
Step 3: above-mentioned reaction product 700W microwave reactor standing wave is reacted 180 minutes, can be obtained has
The carbon of open architecture/silica composite Nano medium hole hollow ball；
Step 4: removing silica in carbon elimination/silica composite Nano medium hole hollow ball with 5% hydrofluoric acid solution, and
It is the functional mesoporous hollow carbon sphere with open architecture with obtained solid powder after the abundant cleaning, drying of distilled water.
Embodiment 6
Step 1: being separately added into 7mL propyl alcohol, 17mL water and 0.2mL mass concentration in the reaction vessel is 25%~30%
Ammonia spirit, be then separately added into the 3- amino phenols, 0.18g paraformaldehyde, 0.5g cetyl trimethyl chlorination of 0.3g again
Ammonium (CTAC) and 1.2g non-hydrate sodium metasilicate (Na2SiO3·9H2O)；
Step 2: mixed solution is placed in ultrasonic transmitter, and 500W continual ultrasonic 12 minutes, the sediment of reaction was
Polymeric with " penetration twin " structure/silica composite Nano medium hole hollow ball；
Step 3: above-mentioned reaction product 800W microwave reactor standing wave is reacted 180 minutes, can be obtained has
The carbon of open architecture/silica composite Nano medium hole hollow ball；
Step 4: silica in carbon elimination/silica composite Nano medium hole hollow ball is removed with the NaOH solution of 5M, is used in combination
Obtained solid powder is the functional mesoporous hollow carbon sphere with open architecture after the abundant cleaning, drying of distilled water.
Embodiment 7
Step 1: it is separately added into 8mL ethyl alcohol, 16mL water and 0.2g urea in reaction vessel, is then separately added into 0.3g again
3- amino phenols, 0.18g paraformaldehyde and 0.5g hexadecyltrimethylammonium chloride (CTAC)；
Step 2: mixed solution is placed in ultrasonic transmitter addition 1.5mL positive silicic acid propyl ester in 900W ultrasonic procedure
(TPOS) solution, and continual ultrasonic 6 minutes, the sediment of reaction be have the polymeric of " penetration twin " structure/
Silica composite Nano medium hole hollow ball；
Step 3: 800 DEG C step 3: are warming up to 1 DEG C per minute in inert gas to above-mentioned reaction product tube furnace
And 2 hours are kept the temperature, the carbon with open architecture/silica composite Nano medium hole hollow ball can be obtained；
Step 4: removing silica in carbon elimination/silica composite Nano medium hole hollow ball with 5% hydrofluoric acid solution, and
It is the functional mesoporous hollow carbon sphere with open architecture with obtained solid powder after the abundant cleaning, drying of distilled water.
Embodiment 8
Step 1: it is separately added into 8mL propyl alcohol, 16mL water and 0.2g urea in the reaction vessel, is then separately added into again
3- amino phenols, 0.18g paraformaldehyde, 0.5g hexadecyltrimethylammonium chloride (CTAC) and the 1.2g non-hydrate sodium metasilicate of 0.3g
(Na2SiO3·9H2O)；
Step 2: mixed solution is continued into stirring 24 hours, the sediment of reaction is to have " penetration twin " structure
Polymeric/silica composite Nano medium hole hollow ball；
Step 3: 750 DEG C and heat preservation 3 are warming up to 3 DEG C per minute in inert gas to above-mentioned reaction product tube furnace
Hour, the carbon with open architecture/silica composite Nano medium hole hollow ball can be obtained；
Step 4: silica in carbon elimination/silica composite Nano medium hole hollow ball is removed with the NaOH solution of 5M, is used in combination
Obtained solid powder is the functional mesoporous hollow carbon sphere with open architecture after the abundant cleaning, drying of distilled water.
Claims (6)
1. the functional mesoporous hollow Nano carbon ball that a kind of Ultrasound-microwave preparation has open architecture, it is characterised in that including
Following steps:
Step 1: being separately added into water, organic solvent and basic catalyst in reaction vessel, be then separately added into again 3- amino phenols,
Paraformaldehyde, surfactant；
Step 2: then the mixed solution that ultrasound is above-mentioned, and silicate solution is added, the sediment of reaction is to have " through twin
Polymeric/silica composite mesopore hollow nano-sphere of crystalline substance " structure；Wherein ultrasonic time is 3-25 minutes, power
For 100-2000W or directly stir 12-24 hours；Microwave carbonization time is 10-500 minutes, and power is 300 ~ 3000W；
Step 3: microwave carbonization is carried out to polymeric/silica composite Nano medium hole hollow ball with microwave reactor
Processing, can be obtained carbon/silica composite Nano meso-porous hollow nanosphere；
Step 4: removing silica in carbon elimination/silica composite Nano medium hole hollow ball with hydrofluoric acid or dense aqueous slkali,
It can be obtained the functional mesoporous hollow Nano carbon ball with open architecture.
2. preparing carbon/silica composite Nano medium hole hollow ball method as described in claim 1, which is characterized in that its
Middle organic solvent is one of ethyl alcohol, ether, ethylene glycol, propyl alcohol or isopropyl acetone.
3. preparing carbon/silica composite Nano medium hole hollow ball method as described in claim 1, which is characterized in that its
The volume ratio of middle water and organic solvent is 1:0.01 ~ 100.
4. preparing carbon/silica composite Nano medium hole hollow ball method as described in claim 1, which is characterized in that its
Neutral and alkali catalyst is that all can ionize in water and generate the reagent of hydroxide ion.
5. preparing carbon/silica composite Nano medium hole hollow ball method as claimed in claim 4, which is characterized in that its
Neutral and alkali catalyst is one of KOH, NaOH or ammonium hydroxide.
6. preparing carbon/silica composite Nano medium hole hollow ball method as described in claim 1, which is characterized in that its
Middle surfactant is hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, nonionic surface active agent
F127 or P123 are one or more kinds of, silicic acid be one of positive silicic acid propyl ester, ethyl orthosilicate or non-hydrate sodium metasilicate or
Person is a variety of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610574730.1A CN106430147B (en) | 2016-07-20 | 2016-07-20 | A kind of Ultrasound-microwave preparation has the functional mesoporous hollow carbon sphere of open architecture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610574730.1A CN106430147B (en) | 2016-07-20 | 2016-07-20 | A kind of Ultrasound-microwave preparation has the functional mesoporous hollow carbon sphere of open architecture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106430147A CN106430147A (en) | 2017-02-22 |
| CN106430147B true CN106430147B (en) | 2018-12-04 |
Family
ID=58184587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610574730.1A Active CN106430147B (en) | 2016-07-20 | 2016-07-20 | A kind of Ultrasound-microwave preparation has the functional mesoporous hollow carbon sphere of open architecture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106430147B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108598446A (en) * | 2018-06-22 | 2018-09-28 | 北京理工大学 | A kind of preparation method of high performance silicon carbon composite nano hollow ball negative material |
| CN109824030A (en) * | 2019-03-25 | 2019-05-31 | 中国科学院福建物质结构研究所 | A kind of hollow carbon sphere and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439858A (en) * | 2008-11-19 | 2009-05-27 | 南京航空航天大学 | Microwave assisted method for rapidly synthesizing ordered mesoporous carbon |
| CN102642843A (en) * | 2012-05-10 | 2012-08-22 | 北京理工大学 | Method for simultaneously preparing multilevel-structure mesoporous silicon dioxide and carbon nano material |
| CN103193223A (en) * | 2013-04-02 | 2013-07-10 | 中国矿业大学 | Controllable synthetic method of graphitized carbon spheres with hollow structure |
-
2016
- 2016-07-20 CN CN201610574730.1A patent/CN106430147B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439858A (en) * | 2008-11-19 | 2009-05-27 | 南京航空航天大学 | Microwave assisted method for rapidly synthesizing ordered mesoporous carbon |
| CN102642843A (en) * | 2012-05-10 | 2012-08-22 | 北京理工大学 | Method for simultaneously preparing multilevel-structure mesoporous silicon dioxide and carbon nano material |
| CN103193223A (en) * | 2013-04-02 | 2013-07-10 | 中国矿业大学 | Controllable synthetic method of graphitized carbon spheres with hollow structure |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106430147A (en) | 2017-02-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105923623A (en) | Preparation method of graphene powder with three-dimensional hierarchical porous structure | |
| CN106883818B (en) | Hud typed carbon ball/carbon nano tube composite wave-absorbing material and preparation method | |
| CN105502342A (en) | Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source | |
| CN105384164A (en) | Crumpled graphene with characteristics of high specific surface area and graded pore structure, and preparation method thereof | |
| CN105621384B (en) | A kind of synthetic method of carbon material | |
| CN103991864B (en) | A kind of preparation method of graphene aerogel | |
| CN108101010B (en) | Preparation method of graphite phase carbon nitride quantum dots | |
| CN106910640A (en) | Controllable graphene nanometer sheet electrode material of a kind of form and its preparation method and application | |
| CN101585529A (en) | Method for in-situ preparation of ordered mesoporous carbon/metal composite material by organic template method | |
| CN106430147B (en) | A kind of Ultrasound-microwave preparation has the functional mesoporous hollow carbon sphere of open architecture | |
| CN106927451B (en) | Three-dimensional structure graphene and its carbon source self-template catalytic pyrolysis preparation method | |
| CN110002423B (en) | Preparation method of phenolic resin-based hollow carbon spheres | |
| CN106391094B (en) | The preparation method of the composite material of the silica supported nanometer MoO3 of mesoporous carbon-and nano-metal particle | |
| CN107161989A (en) | A kind of preparation method of cellular three-dimensional grapheme | |
| CN106540733A (en) | A kind of method for preparing graphite phase carbon nitride material | |
| CN104130004A (en) | Preparation method of high-strength block-shaped porous alumina nano-ceramic | |
| CN110078521A (en) | A kind of submicron order silicon nitride hollow microsphere and preparation method | |
| CN109748282A (en) | A kind of method of low temperature preparation nanometer silicon carbide | |
| CN102849750A (en) | Mesoporous silica with radial tunnels and preparation method thereof | |
| CN108996486B (en) | Hierarchical porous carbon and preparation method and application thereof | |
| CN107570698A (en) | A kind of graphene coated titanium composite powder material and preparation method thereof | |
| CN107098343A (en) | A kind of CaCl2Gu the method that sulphur prepares nitrogen sulphur codope porous carbon materials | |
| CN110451498A (en) | A kind of graphene-boron nitride nanosheet composite construction and preparation method thereof | |
| CN105060272B (en) | A kind of using artemia chorion as carbon source low temperature under prepare the method for CNT | |
| CN105621386B (en) | A kind of method for preparing carbon material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |