CN108584915A - A kind of cellular carbon nanomaterial of regular hexagon and preparation method thereof - Google Patents
A kind of cellular carbon nanomaterial of regular hexagon and preparation method thereof Download PDFInfo
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- CN108584915A CN108584915A CN201810560150.6A CN201810560150A CN108584915A CN 108584915 A CN108584915 A CN 108584915A CN 201810560150 A CN201810560150 A CN 201810560150A CN 108584915 A CN108584915 A CN 108584915A
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- pmma
- honeycomb
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- carbon nanomaterial
- emulsion
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 30
- 230000001413 cellular effect Effects 0.000 title claims abstract description 21
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 34
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 34
- 239000000839 emulsion Substances 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 11
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 6
- 239000002243 precursor Substances 0.000 abstract description 6
- 238000000197 pyrolysis Methods 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- DGXAGETVRDOQFP-UHFFFAOYSA-N 2,6-dihydroxybenzaldehyde Chemical compound OC1=CC=CC(O)=C1C=O DGXAGETVRDOQFP-UHFFFAOYSA-N 0.000 abstract 1
- 241000264877 Hippospongia communis Species 0.000 description 23
- 239000003575 carbonaceous material Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000007789 sealing Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 150000005207 1,3-dihydroxybenzenes Chemical class 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- KVBYPTUGEKVEIJ-UHFFFAOYSA-N benzene-1,3-diol;formaldehyde Chemical compound O=C.OC1=CC=CC(O)=C1 KVBYPTUGEKVEIJ-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical class [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000002061 vacuum sublimation Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Filtering Materials (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of the cellular carbon nanomaterial of regular hexagon, including step：（1）The synthesis of PMMA emulsion；（2）PMMA emulsion is sealed at different conditions and places certain time, obtains PMMA honeycomb templates；（3）Resorcinol formaldehyde resin is formed in the gap of PMMA honeycomb templates, to form cellular carbon matrix precursor；（4）In a nitrogen atmosphere by above-mentioned presoma, pass through substep pyrolysis way, cellular carbon matrix precursor starts to soften after the heating, and it is constantly flowed to the gap of honeycomb template, and finally connected in the periphery of template, with the continuous raising of pyrolysis temperature, template is removed, and the carbon matrix precursor to link together constantly adjusts its internal structure, and finally obtains the honeycomb carbon nanomaterial with rock-steady structure.
Description
Technical field
The invention belongs to novel carbon Material Fields, and in particular to arrive a kind of cellular carbon nanomaterial of regular hexagon
Preparation method
Background technology
Light material has unique physical property, has very extensive application in various Practical Project fields.For example, having
The light material of high mechanical strength can be used as space material, and the light material with good thermal conductivity can be applied to
Heat exchanger；In addition, these novel light materials also have a wide range of applications in electrochemical energy source field.In these lightweight materials
In material, carbon materials are most representative.Carbon arrives low dimensional there are many allotrope from block-like diamond, graphite
Fullerene, carbon nanotube and graphene, they are all research field of the material science rich in rich connotation, are also greatly extended
The research contents of material science.The carbon material of low dimensional, as graphene and carbon nanotube not only have high mechanical strength and good
Good thermal conductivity, and be the catalyst carrier that electrochemical energy source field has very excellent properties.Utilize this low dimensional
Material can build three-dimensional（3D）Carbon material, the latter have performance more outstanding and application prospect.
In these 3D carbon materials, cellular carbon material is one of the field that nearest people pay close attention to the most.Currently, this kind of bee
The preparation process of nest shape carbon material it is more complicated with it is cumbersome, generally the graphite of vacuum sublimation is deposited cellular to prepare
Carbon.In recent years, it is attempted to prepare the carbon material with honeycomb structure, but obtained honeycomb structure using different methods
Irregular, not regular hexagon occurs, and cell size is different, the existing circle of shape, also there is rectangular, and these shapes
Shape have it is big also have it is small.Therefore, the cellular carbon with regular hexagon is prepared, the application field for expanding carbon materials has
Important application value.
Invention content
The object of the present invention is to provide a kind of cellular carbon nanomaterial of regular hexagon, the purpose of the present invention additionally provides one
The cellular carbon nanomaterial and preparation method thereof of the regular hexagon of kind.
In order to achieve the above objectives, embodiment of the present invention is：A kind of cellular carbon nanomaterial of regular hexagon
Preparation method includes the following steps：
（1）The synthesis of PMMA emulsion；
（2）The synthesis of PMMA honeycomb templates：At different conditions, PMMA emulsion is sealed and places certain time, obtain PMMA
Honeycomb template；
（3）Resorcinol is dissolved in pure water, after stirring evenly, is added a concentration of 40%（wt%）Formalin, continue to stir
After mixing, PMMA honeycomb templates are added, after stirring evenly, gained mixture is kept into for certain time in 85 DEG C of constant temperature；Then will
Mixture filters, dry under 40C after obtained solid is washed with pure water, obtains presoma；
（4）In a nitrogen atmosphere by above-mentioned presoma, it is warming up to 200-350 DEG C with the speed of 3 DEG C of min 1 first, in this temperature
Lower holding certain time；It then is continuously heating to 500-600 DEG C with the speed of 4 DEG C × min 1, and is kept at this temperature certain
Time；850 DEG C finally are continuously heating to the speed of 4 DEG C × min-1, and keeps certain time at this temperature；Later, natural
It is cooled to room temperature, obtains honeycomb carbon nanomaterial.
The different condition refers to：Static placement, or be constantly passed through into solution with the speed of 3 bubbles per second or so
N2, or emulsion is stirred into 5min every 12h;The placement certain time refers to 7 days or 3 days or 1 hour；
A kind of cellular carbon nanomaterial of regular hexagon prepared by a kind of method described in basis.
The present invention prepares cellular carbon nanomaterial by PMMA soft template methods：Pass through the preparation process in PMMA emulsion
In be passed through nitrogen, certain gap is formed between PMMA emulsion drops, for subsequent carbon package leave a void；By the way that PMMA is newborn
Shape liquid places the regular hour at room temperature, and the soft template of emulsion is made constantly to adjust, and ultimately forms cellular soft template；It is logical
The reaction between resorcinol and formaldehyde is crossed, resorcinol formaldehyde resin is formed in the gap of PMMA honeycomb templates, to shape
At cellular carbon matrix precursor；By substep pyrolysis way, cellular carbon matrix precursor starts to soften after the heating, and constantly to
The gap of honeycomb template is flowed, and is finally connected in the periphery of template, with the continuous raising of pyrolysis temperature, template by except
The carbon matrix precursor for going, and linking together constantly adjusts its internal structure, and finally obtains the honeycomb carbon with rock-steady structure
Nano material.
Description of the drawings
Fig. 1 is the preparating mechanism schematic diagram of the cellular carbon nanomaterial of regular hexagon；
Fig. 2 is the SEM figures of honeycomb carbon nanomaterial prepared by embodiment 1；
Fig. 3 is the SEM figures of honeycomb carbon nanomaterial prepared by embodiment 2.
Specific implementation mode
Embodiment 1：
（1）The synthesis of PMMA emulsion
Using the prior art（Yu Tong, Yang Junhe, Shi Meiren, soap-free emulsion prepare PMMA dynamics and its model, Nanjing industry
College journal, 2006,28 (2):10-14）, PMMA emulsion is synthesized after making improvements:
It is 1 by 500mL volume ratios:The mixed solution merging three of 15 methyl methacrylate (MMA) monomer and redistilled water
In neck reaction flask, magnetic agitation is opened, while accessing N2Ingress pipe, and by N2Ingress pipe is inserted into solution bottom, N when beginning2
It is about 10 per second that bubble, which escapes speed, and keeps 5min；Then keep N2It is about 3 per second or so that bubble, which escapes speed, directly
Terminate to reaction；75 DEG C are then heated to, and 90 g potassium peroxydisulfates are added；It is again heated to 80 DEG C later, and keeps 8h, obtains white
Color emulsion, as PMMA emulsion.
（2）The synthesis of PMMA honeycomb templates
Under static state, the sealing of gained emulsion is placed 7 days, obtains PMMA honeycomb templates.
（3）3g resorcinols are dissolved in 25mL pure water, after stirring evenly, 5mL a concentration of 40% is added（wt%）Formaldehyde
Aqueous solution continues after stirring 10mim, the above-mentioned PMMA honeycombs template emulsions of 145mL is added, after stirring evenly, by gained mixture
After being transferred to reactor and sealing, then the reactor is placed in 85 DEG C of insulating boxs and is kept for 3 days；Then mixture is filtered, is obtained
To solid wash 2 times with pure water after, be transferred in vacuum drying chamber, dry 12h, obtains presoma under 40C.
（4）Above-mentioned presoma is transferred in pipe reaction stove, in a nitrogen atmosphere, first with 3 DEG C × min-1Speed liter
Temperature keeps 1h at this temperature to 200 ~ 350 DEG C；Then with 4 DEG C × min-1Speed be continuously heating to 500 ~ 600 DEG C, and
1h is kept at a temperature of this；Finally with 4 DEG C × min-1Speed be continuously heating to 850 DEG C, and keep 3h at this temperature；Later,
Cooled to room temperature obtains honeycomb carbon nanomaterial.
Embodiment 2：
Step（1）The step of with embodiment 1（1）It is identical.
（2）The synthesis of PMMA honeycomb templates
Under static state, the sealing of gained emulsion is placed 3 days, obtains PMMA honeycomb templates.
Step（3）With（4）The step of with embodiment 1（3）With（4）It is identical.
Embodiment 3：
Step（1）The step of with embodiment 1（1）It is identical.
（2）The synthesis of PMMA honeycomb templates
Under static state, the sealing of gained emulsion is placed 1 hour, obtains PMMA honeycomb templates.
Step（3）With（4）The step of with embodiment 1（3）With（4）It is identical.
Embodiment 4：
Step（1）The step of with embodiment 1（1）It is identical.
（2）The synthesis of PMMA honeycomb templates
N is constantly passed through into emulsion with the speed of 3 bubbles per second or so2, and kept for 7 days, obtain PMMA honeycomb templates.
Step（3）With（4）The step of with embodiment 1（3）With（4）It is identical.
Embodiment 5：
Step（1）The step of with embodiment 1（1）It is identical.
（2）The synthesis of PMMA honeycomb templates
Emulsion is stirred into 5min every 12h, sealing is continued thereafter with and is kept for 7 days, obtain PMMA honeycomb templates.
Claims (3)
1. a kind of preparation method of the cellular carbon nanomaterial of regular hexagon, which is characterized in that include the following steps：
（1）The synthesis of PMMA emulsion；
（2）The synthesis of PMMA honeycomb templates：At different conditions, PMMA emulsion is sealed and places certain time, obtain PMMA
Honeycomb template；
（3）Resorcinol is dissolved in pure water, after stirring evenly, is added a concentration of 40%（wt%）Formalin, continue to stir
After mixing, PMMA honeycomb templates are added, after stirring evenly, gained mixture is kept into for certain time in 85 DEG C of constant temperature；Then will
Mixture filters, dry under 40C after obtained solid is washed with pure water, obtains presoma；
（4）In a nitrogen atmosphere by above-mentioned presoma, it is warming up to 200-350 DEG C with the speed of 3 DEG C of min 1 first, in this temperature
Lower holding certain time；It then is continuously heating to 500-600 DEG C with the speed of 4 DEG C × min 1, and is kept at this temperature certain
Time；850 DEG C finally are continuously heating to the speed of 4 DEG C × min-1, and keeps certain time at this temperature；Later, natural
It is cooled to room temperature, obtains honeycomb carbon nanomaterial.
2. the preparation method of the cellular carbon nanomaterial of regular hexagon according to claim 1, which is characterized in that step
Suddenly（2）Described in different condition refer to：Static placement, or be constantly passed through into solution with the speed of 3 bubbles per second or so
N2, or emulsion is stirred into 5min every 12h;The placement certain time refers to 7 days or 3 days or 1 hour.
3. a kind of a kind of cellular carbon nanomaterial of the regular hexagon prepared method according to claim 1 or 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810560150.6A CN108584915B (en) | 2018-06-03 | 2018-06-03 | Regular hexagonal honeycomb-shaped carbon nano material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810560150.6A CN108584915B (en) | 2018-06-03 | 2018-06-03 | Regular hexagonal honeycomb-shaped carbon nano material and preparation method thereof |
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| CN108584915A true CN108584915A (en) | 2018-09-28 |
| CN108584915B CN108584915B (en) | 2021-09-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101088916A (en) * | 2007-05-14 | 2007-12-19 | 同济大学 | O/W emulsion process of preparing carbon foam |
| CN101531358A (en) * | 2009-04-28 | 2009-09-16 | 湖南理工学院 | Method for preparing porous carbon electrode material used for super capacitor |
| CN101798077A (en) * | 2010-04-08 | 2010-08-11 | 哈尔滨工业大学 | Preparation method of hollow carbon sphere with resorcinol and formaldehyde as raw materials |
| CN103855412A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院大连化学物理研究所 | Porous carbon material used for anode of lithium-air cell |
| CN104518218A (en) * | 2013-09-29 | 2015-04-15 | 中国科学院大连化学物理研究所 | Applications of porous carbon material in lithium-thionyl chloride battery positive electrode |
| CN104518226A (en) * | 2013-09-29 | 2015-04-15 | 中国科学院大连化学物理研究所 | Lithium.air or lithium-oxygen battery positive electrode porous carbon material |
| CN104518219A (en) * | 2013-09-29 | 2015-04-15 | 中国科学院大连化学物理研究所 | Applications of porous carbon material in lithium-thionyl chloride battery positive electrode |
| CN106744859A (en) * | 2017-01-22 | 2017-05-31 | 广西大学 | Graphene three-dimensional multistage pore structure powder prepared by a kind of low temperature polymer cracking |
| CN106744787A (en) * | 2016-11-15 | 2017-05-31 | 安徽安达新能源材料有限公司 | Cellular porous hard carbon lithium ion battery negative material and preparation method thereof and lithium ion battery |
| CN106999903A (en) * | 2014-10-06 | 2017-08-01 | 康宁股份有限公司 | Non-extruded type honeycomb active carbon structure |
-
2018
- 2018-06-03 CN CN201810560150.6A patent/CN108584915B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101088916A (en) * | 2007-05-14 | 2007-12-19 | 同济大学 | O/W emulsion process of preparing carbon foam |
| CN101531358A (en) * | 2009-04-28 | 2009-09-16 | 湖南理工学院 | Method for preparing porous carbon electrode material used for super capacitor |
| CN101798077A (en) * | 2010-04-08 | 2010-08-11 | 哈尔滨工业大学 | Preparation method of hollow carbon sphere with resorcinol and formaldehyde as raw materials |
| CN103855412A (en) * | 2012-11-28 | 2014-06-11 | 中国科学院大连化学物理研究所 | Porous carbon material used for anode of lithium-air cell |
| CN104518218A (en) * | 2013-09-29 | 2015-04-15 | 中国科学院大连化学物理研究所 | Applications of porous carbon material in lithium-thionyl chloride battery positive electrode |
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| CN106999903A (en) * | 2014-10-06 | 2017-08-01 | 康宁股份有限公司 | Non-extruded type honeycomb active carbon structure |
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| CN106744859A (en) * | 2017-01-22 | 2017-05-31 | 广西大学 | Graphene three-dimensional multistage pore structure powder prepared by a kind of low temperature polymer cracking |
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Effective date of registration: 20230511 Address after: No. 56 Yezhi Road, Quzhou City, Zhejiang Province, 324000 Patentee after: Quzhou Qufarui New Energy Materials Co.,Ltd. Address before: 411201 stone horse head in Yuhu District, Xiangtan, Hunan Patentee before: HUNAN University OF SCIENCE AND TECHNOLOGY |