CN105016335B - 一种石墨烯的制备方法 - Google Patents
一种石墨烯的制备方法 Download PDFInfo
- Publication number
- CN105016335B CN105016335B CN201510517547.3A CN201510517547A CN105016335B CN 105016335 B CN105016335 B CN 105016335B CN 201510517547 A CN201510517547 A CN 201510517547A CN 105016335 B CN105016335 B CN 105016335B
- Authority
- CN
- China
- Prior art keywords
- graphene
- preparation
- back flow
- thymol
- flow reaction
- 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.)
- Expired - Fee Related
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005844 Thymol Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 229960000790 thymol Drugs 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002356 single layer Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 230000032798 delamination Effects 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class 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
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- -1 bio-imaging Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
本发明涉及一种石墨烯的制备方法，按照10:1‑1:1的体积比，将质量百分比为0.1%‑10%的麝香草酚溶液与1‑100g/L的氧化石墨烯溶液混合，80‑100℃下回流反应1‑12h，抽滤、洗涤、干燥处理后得到石墨烯。本发明采用麝香草酚作为还原剂，在不添加任何稳定剂、分散剂的条件下回流反应制备得到石墨烯，绿色环保、成本低廉、工艺简单，并且制备得到的石墨烯具有良好的分散性和稳定性。
Description
技术领域
本发明属于石墨烯的合成和纳米材料技术领域，特别涉及一种石墨烯的制备方法。
背景技术
2004年，英国曼彻斯特大学物理学家安德烈•海姆和康斯坦丁•诺沃肖洛夫，利用撕透明胶带的方法，成功地从石墨中分离出单层原子排列的石墨烯，两人也因此获得2010年的诺贝尔物理学奖（Science,2004,306(
5696):666-669）。石墨烯由碳原子以sp2杂化轨道组成六角型蜂巢晶格，其结构单元为碳六元环，它是一种只有单层碳原子厚度的二维材料。石墨烯是构成碳基材料的基本机构单元。它可以包裹形成零维Fullerenes，卷成一维carbon nanotube，层层堆积成三维graphite。从石墨烯发现的那一天起，石墨烯就已经成为研究的热点和焦点，在超级电容器、透明电极、海水淡化、发光二极管、传感器、储氢、太阳能电池、催化剂载体、复合材料、生物支架材料、生物成像、药物输送、纺织、印染等领域有广泛的应用。
石墨烯具有优异的机械、电学、热学性能、抗菌性能。石墨烯是世界上最薄的材料，它只有单层原子的厚度，约为0.335nm。石墨烯几乎是完全透明的，只吸收2.3%的光，透光率高达97.7%。电阻率10-6Ω/cm，比铜或银更低，为目前世界上电阻率最小的材料。石墨烯具有极大的比表面积，其理论值高达2630m2/g。导热系数高达5300W/m•K，常温下电子迁移率超过15000cm2/V•s，比碳纳米管和单晶硅高。杨氏模量为1.1TPa，断裂强度高达130GPa。
石墨烯的制备方法主要有：微机械剥离法、***切取转印法、液相剥离法、化学气相沉积法、气溶胶高温分解法、外延生长法、无定形碳化物薄膜转化法、氧化石墨烯（GO）还原法及有机合成法等。其中GO还原法具有成本低、产率高和可批量生产等特点，得到广泛应用。目前常用的还原剂包括水合肼、二甲基肼、酚类、硼氢化钠、含硫化合物、醇类等（炭素技术,2013,32(5):30-36）。然而，由于GO还原法往往使用肼或硼氢化钠等有毒或价格昂贵的试剂作为还原剂，因此开发绿色、环保、高效和廉价的化学还原技术十分必要。
发明内容
本发明针对现有技术存在的不足，提供一种石墨烯的制备方法。
本发明通过下述技术方案予以实现：
按照10:1-1:1的体积比，将质量百分比为0.1%-10%的麝香草酚溶液与1-100g/L的氧化石墨烯溶液混合，80-100℃下回流反应1-12h，抽滤、洗涤、干燥处理后得到石墨烯。其中氧化石墨烯由氧化石墨经超声剥层制得，为单层氧化石墨烯、多层氧化石墨烯或二者的混合物。
本发明的优点：
本发明采用绿色环保的麝香草酚作为还原剂，在不添加任何稳定剂、分散剂的条件下通过水热反应的方法制备得到石墨烯，绿色环保、成本低廉、工艺简单，并且制备得到的石墨烯具有良好的分散性和稳定性。
具体实施方式
下面结合具体实施方式，进一步阐述本发明。
实施例1：
将10ml质量百分比为0.1%的麝香草酚溶液与1ml的1g/L氧化石墨烯溶液混合，80℃下回流反应1h，抽滤、洗涤、干燥处理后得到石墨烯。
实施例2：
将10ml质量百分比为1%的麝香草酚溶液与5ml的10g/L氧化石墨烯溶液混合，90℃下回流反应6h，抽滤、洗涤、干燥处理后得到石墨烯。
实施例3：
将10ml质量百分比为5%的麝香草酚溶液与10ml的50g/L氧化石墨烯溶液混合，100℃下回流反应12h，抽滤、洗涤、干燥处理后得到石墨烯。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无法对所有的实施方式予以穷举。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (1)
1.一种石墨烯的制备方法，其特征在于：按照10:1-1:1的体积比，将质量百分比0.1%-10%的麝香草酚溶液与1-100g/L的氧化石墨烯溶液混合，所述氧化石墨烯由氧化石墨经超声剥层制得，为单层氧化石墨烯、多层氧化石墨烯或二者的混合物，80-100℃下回流反应1-12h，抽滤、洗涤、干燥处理后得到石墨烯。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517547.3A CN105016335B (zh) | 2015-08-22 | 2015-08-22 | 一种石墨烯的制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517547.3A CN105016335B (zh) | 2015-08-22 | 2015-08-22 | 一种石墨烯的制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105016335A CN105016335A (zh) | 2015-11-04 |
| CN105016335B true CN105016335B (zh) | 2016-11-30 |
Family
ID=54406717
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510517547.3A Expired - Fee Related CN105016335B (zh) | 2015-08-22 | 2015-08-22 | 一种石墨烯的制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105016335B (zh) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103072981A (zh) * | 2013-02-26 | 2013-05-01 | 武汉大学 | 一种石墨烯的制备方法 |
| US8771630B2 (en) * | 2012-01-26 | 2014-07-08 | Enerage, Inc. | Method for the preparation of graphene |
| CN104261401A (zh) * | 2014-10-14 | 2015-01-07 | 钱景 | 一种石墨烯的制备方法 |
-
2015
- 2015-08-22 CN CN201510517547.3A patent/CN105016335B/zh not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8771630B2 (en) * | 2012-01-26 | 2014-07-08 | Enerage, Inc. | Method for the preparation of graphene |
| CN103072981A (zh) * | 2013-02-26 | 2013-05-01 | 武汉大学 | 一种石墨烯的制备方法 |
| CN104261401A (zh) * | 2014-10-14 | 2015-01-07 | 钱景 | 一种石墨烯的制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105016335A (zh) | 2015-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jiang et al. | Modified 2D-2D ZnIn2S4/BiOCl van der Waals heterojunctions with CQDs: Accelerated charge transfer and enhanced photocatalytic activity under vis-and NIR-light | |
| Ikram et al. | Advances in synthesis of graphene derivatives using industrial wastes precursors; prospects and challenges | |
| Giovannetti et al. | Recent advances in graphene based TiO2 nanocomposites (GTiO2Ns) for photocatalytic degradation of synthetic dyes | |
| Nasir et al. | Carbon-based nanomaterials/allotropes: A glimpse of their synthesis, properties and some applications | |
| Chen et al. | Catalyst-free growth of three-dimensional graphene flakes and graphene/g-C3N4 composite for hydrocarbon oxidation | |
| Tatykayev et al. | Synthesis of core/shell ZnO/rGO nanoparticles by calcination of ZIF-8/rGO composites and their photocatalytic activity | |
| Pham et al. | Influence of g-C3N4 precursors in g-C3N4/NiTiO3 composites on photocatalytic behavior and the interconnection between g-C3N4 and NiTiO3 | |
| Wu et al. | Temperature-controlled synthesis of porous CuO particles with different morphologies for highly sensitive detection of triethylamine | |
| Xu et al. | Coffee-ground-derived quantum dots for aqueous processable nanoporous graphene membranes | |
| Tang et al. | Two-dimensional carbon leading to new photoconversion processes | |
| Ndlwana et al. | Sustainable hydrothermal and solvothermal synthesis of advanced carbon materials in multidimensional applications: A review | |
| Srivastava et al. | Faster response of NO2 sensing in graphene–WO3 nanocomposites | |
| Zhang et al. | Enhanced photoresponsive ultrathin graphitic-phase C3N4 nanosheets for bioimaging | |
| CN105217607A (zh) | 一种基于木质素的石墨烯制备方法 | |
| Ashok Kumar et al. | A review on graphene and its derivatives as the forerunner of the two-dimensional material family for the future | |
| CN103361044A (zh) | 一种氧化石墨烯片包裹氧化锌量子点核壳结构的制备方法 | |
| CN103962102A (zh) | 一种细沙-氧化石墨烯复合吸附材料 | |
| CN104556016B (zh) | 一种石墨烯的低温环保制备方法 | |
| CN101973543B (zh) | 一种单层石墨烯的制备方法 | |
| CN104399998A (zh) | 一种石墨烯/纳米银复合材料的制备方法 | |
| CN105675664A (zh) | 一种基于rGO/α-Fe2O3异质结构复合物的丙酮传感器及其制备方法 | |
| Gopiraman et al. | Facile mechanochemical synthesis of nickel/graphene oxide nanocomposites with unique and tunable morphology: applications in heterogeneous catalysis and supercapacitors | |
| CN105036124A (zh) | 一种多聚糖制备石墨烯的方法 | |
| CN104310390A (zh) | 一种改性壳聚糖制备石墨烯的方法 | |
| Wang et al. | Snowball flower-like g-C3N4/ZnFe2O4 mesoporous hollow microspheres with enhanced triethylamine sensing properties |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Xiaogang Inventor before: Qian Jing Inventor before: Zhao Bing |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20170524 Address after: 519000 Guangdong city of Zhuhai province Hengqin Baohua Road No. 6, room 105 -14433 Patentee after: Zhuhai carbon carbon composite material Co Ltd Address before: 215001, Suzhou, Jiangsu province Xiangcheng District yuan and street Yao Yao Road No. 1165 Cambridge Creek 5-2101 Patentee before: Qian Jing |
|
| TR01 | Transfer of patent right | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Xiaogang Inventor after: Ma Ning Inventor before: Chen Xiaogang |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161130 Termination date: 20170822 |