CN106082175B - 一种熔融碳酸钠高温制备碳化物衍生碳的方法 - Google Patents
一种熔融碳酸钠高温制备碳化物衍生碳的方法 Download PDFInfo
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- 229910021401 carbide-derived carbon Inorganic materials 0.000 title claims abstract description 42
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910000029 sodium carbonate Inorganic materials 0.000 title claims abstract description 15
- 238000002844 melting Methods 0.000 title claims abstract description 13
- 230000008018 melting Effects 0.000 title claims abstract description 13
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 8
- 150000003624 transition metals Chemical class 0.000 claims abstract description 8
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 3
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 239000010936 titanium Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910003074 TiCl4 Inorganic materials 0.000 description 4
- 229910003080 TiO4 Inorganic materials 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- LYJTXJJPTFISDL-UHFFFAOYSA-L C([O-])([O-])=O.[Ti+4].[Al+3] Chemical compound C([O-])([O-])=O.[Ti+4].[Al+3] LYJTXJJPTFISDL-UHFFFAOYSA-L 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
一种熔融碳酸钠高温制备碳化物衍生碳的方法，属于碳材料技术领域。将过渡金属碳化物和碳酸钠固相混合，在惰性气体保护下于500~1000°C高温煅烧，用盐酸洗去金属杂质，抽滤、洗涤得到碳化物衍生碳材料。本发明制备过程简单，操作方便，对环境污染小，易于控制，制备出的碳材料具有类石墨烯的二维层状结构。
Description
技术领域
本发明涉及一种熔融碳酸钠高温制备碳化物衍生碳的方法，属于碳材料技术领域。
背景技术
碳化物衍生碳是以碳化物为前驱体，去除其晶格中的金属原子剩下骨架碳结构，从而得到的一种新型碳材料。由于具有导电性好、比表面高、孔径分布可调等优点，碳化物衍生碳在超级电容器电极材料、水处理、催化剂载体、气体储存等领域具有独特的应用优势。
目前制备碳化物衍生碳的方法主要有高温卤化法、超临界水过滤法、真空热分解法等方法（Encyclopedia of Nanoscience and Nanotechnology, 2004, 10, 1-22）。超临界水过滤和真空热分解法存在制备效率低、纯度不高等不足。相比之下，高温卤化法是制备碳化物衍生碳的最有效方法，采用氯气高温刻蚀可高效去除碳化物中的金属元素，得到高比表面的碳化物衍生碳。但是氯气腐蚀性强，有毒性，操作不便，安全风险大。专利号为CN103436904B的《一种熔盐电解法制备碳化物衍生碳的方法》中介绍了通过电解法制备碳化物衍生碳的方法。但这种方法耗能高，装置复杂。
发明内容
针对现有技术的不足，本发明提出了一种熔融碳酸钠高温刻蚀过渡金属碳化物中的金属元素制备碳化物衍生碳的方法，其目的是提供制备方法简单、低能耗、无污染、安全性能高、便于工业化生产的碳化物衍生碳的制备方法。
本发明所采用的技术方案包括如下步骤：
1）将过渡金属碳化物与无水碳酸钠按质量比1:3~1:20固相混合均匀；
2）将步骤1）所得混合物放于高温管式炉内，在惰性气体保护下，在500-1000°C煅烧1-10 h，待炉温降至室温后取出；
3）将步骤2）所得煅烧产物中加入过量盐酸水溶液中，其中盐酸水溶液的温度保持在0-25°C，至反应完全；
4）将步骤3）反应后的产物减压抽滤，用去离子水洗至中性，干燥，即得碳化物衍生碳。
其中，所述步骤1）中的过渡金属碳化物优选为Ti3AlC2、Ti2AlC、Ti3SiC2、Ti2SiC、Ti3C2和Ti2C中的一种或几种。
其中，所述步骤（2）中的惰性气氛为氮气、氦气、氩气中的一种或几种，升温速度为0.1~200°C/min。
其中，所述步骤3）中的盐酸的浓度为1~7mol/L。
其中，所得碳化物衍生碳具有类石墨烯的二维层状结构。
优选的，所述步骤3）的反应时间在2-72h。
本发明使用熔融碳酸钠高温刻蚀过渡金属碳化物制备碳化物衍生碳，其反应机理为：
2Ti3AlC2 + 15Na2CO3 (l) = 6Na4TiO4 + 2Na3AlO3 + 4C + 15CO (g)
Na2CO3 + 2HCl = 2NaCl + H2O+ CO2 (g)
Na3AlO3 + 6HCl = AlCl3 + 3NaCl + 3H2O
Na4TiO4 + 8HCl = TiCl4 + 4NaCl + 4H2O
TiCl4 + 2H2O = TiO2 + 4HCl
首先，碳化铝钛和熔融碳酸钠在高温下反应生成Na4TiO4、Na3AlO3及C，然后Na4TiO4和Na3AlO3及多余的Na2CO3分别与HCl反应生成TiCl4、AlCl3和NaCl。在低温（0-25°C）条件下，TiCl4不发生水解，且与AlCl3和NaCl在抽滤过程中与碳材料分离，从而制得碳化物衍生碳。
本发明得到的碳化物衍生碳可作为锂离子电池负极材料和超级电容器的电极材料，均具有高的比容量和良好的循环稳定性。
本发明与现有技术相比具有以下优点：
1）本发明的制备工艺简单，易于控制，所制备出的碳材料纯度高。
2)本发明的制备过程安全程度高，对环境污染小，制备成本低。
3）本发明制备的碳化物衍生碳具有类石墨烯的二维层状结构。
附图说明
图1为实施方案1中的碳化物衍生碳材料的XRD图。
图2为实施方案1中的碳化物衍生碳材料的SEM图。
图3为实施方案1中的碳化物衍生碳材料的拉曼图。
图4为实施方案1中的碳化物衍生碳材料的充放电曲线图。
图5为实施方案1中的碳化物衍生碳材料的循环性能曲线图。
图6为实施方案2中的碳化物衍生碳材料的SEM图。
具体实施方式
下面结合实施例对本发明作进一步说明，但本发明并不限于以下实施例。
实施例1
将2g Ti3AlC2和6g无水碳酸钠混合均匀，盛于镍舟中放置在管式炉中央，在氮气保护下升温至500°C，500°C保温10h。物料自然冷却到室温后，将煅烧后的产物溶解于3M HCl中，室温（20±5°C）下反应2h。将反应产物抽滤，水洗至中性，120°C烘干，即得碳化物衍生碳材料。所得碳化物衍生碳的XRD曲线如图1所示，经检测可知，上述方法制备出了一种碳化物衍生碳材料。所得碳材料的扫描电镜如图2所示，该碳材料具有类石墨烯的二维层状结构。所得碳化物衍生碳的拉曼光谱如图3所示，明显的2D峰表明该碳化物衍生碳材料为二维片层结构。将该碳化物衍生碳用于锂离子电池负极，其充放电曲线和循环性能分别如图4、5所示，可以看出其首次可逆容量达到696mAh/g，循环性能较好。
实施例2
将2g Ti3SiC2和20g无水碳酸钠混合均匀，盛于镍舟中放置在管式炉中央，在氩气保护下升温至880°C，保温5h。将煅烧后的产物溶解于5M HCl中，在室温下反应2h。将反应产物抽滤，水洗至中性，120°C烘干，得到碳化物衍生碳材料。所得碳化物衍生碳材料的扫描电镜图如图6所示，表明制备出一种二维层状材料。将该碳化物衍生碳用于超级电容器电极材料，在6mol/L KOH电解液中质量比电容220 F/g，循环10000次容量保持91%。
实施例3
将1g Ti2AlC和20g无水碳酸钠混合均匀放于镍舟中，将镍舟放置于管式炉内，在氮气和氩气混合气体（体积比1:1）保护下升温至1000°C，保温1h。将煅烧后的产物溶解于3MHCl中，在室温下反应2h。将反应产物抽滤，水洗至中性，120°C烘干，即得碳化物衍生碳材料。
实施例4
将1g Ti2C和15g无水碳酸钠混合均匀放于镍舟中，将镍舟放置于管式炉内，在氮气和氦气混合气体（体积比1:1）保护下升温至850°C，保温10h。将煅烧后的产物溶解于5MHCl中，在室温下反应72h。将反应产物抽滤，水洗至中性，120°C烘干，即得碳化物衍生碳材料。
Claims (5)
1.一种熔融碳酸钠高温制备碳化物衍生碳的方法，其特征在于，采用熔融无水碳酸钠高温刻蚀过渡金属碳化物中的金属元素，制备碳化物衍生碳材料，包括如下步骤：
1)将过渡金属碳化物与无水碳酸钠按质量比1:3～1:20固相混合均匀；
2)将步骤1)所得混合物放于高温管式炉内，在惰性气氛保护下，在500-1000℃煅烧1-10h，待炉温降至室温后取出；
3)将步骤2)所得煅烧产物中加入过量盐酸水溶液中，其中盐酸溶液的温度保持在0-25℃，至反应完全；
4)将步骤3)反应后的产物减压抽滤，用去离子水洗至中性，干燥，即得碳化物衍生碳；
所述步骤1)中的过渡金属碳化物为Ti3AlC2、Ti2AlC、Ti3SiC2、Ti2SiC、Ti3C2和Ti2C中的一种或几种。
2.按照权利要求1所述的一种熔融碳酸钠高温制备碳化物衍生碳的方法，其特征在于，所述步骤2)中的惰性气氛为氮气、氦气、氩气中的一种或几种，升温速度为0.1～200℃/min。
3.按照权利要求1所述的一种熔融碳酸钠高温制备碳化物衍生碳的方法，其特征在于，所述步骤3)中的盐酸的浓度为1～7mol/L。
4.按照权利要求1所述的一种熔融碳酸钠高温制备碳化物衍生碳的方法，其特征在于，所述步骤3)的反应时间在2-72h。
5.按照权利要求1所述的一种熔融碳酸钠高温制备碳化物衍生碳的方法，其特征在于，所得碳化物衍生碳具有类石墨烯的二维层状结构。
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