CN106238082A - 一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法 - Google Patents
一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法 Download PDFInfo
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- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910039444 MoC Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 34
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 21
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011780 sodium chloride Substances 0.000 claims abstract description 20
- 238000006722 reduction reaction Methods 0.000 claims abstract description 18
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims abstract description 15
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000011343 solid material Substances 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 4
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000003763 carbonization Methods 0.000 abstract description 3
- 229910001868 water Inorganic materials 0.000 description 11
- LKDRXBCSQODPBY-VRPWFDPXSA-N D-fructopyranose Chemical compound OCC1(O)OC[C@@H](O)[C@@H](O)[C@@H]1O LKDRXBCSQODPBY-VRPWFDPXSA-N 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 10
- 238000004108 freeze drying Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910052738 indium Inorganic materials 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
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- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000222065 Lycoperdon Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 241000768494 Polymorphum Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
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- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- KDRIEERWEFJUSB-UHFFFAOYSA-N carbon dioxide;methane Chemical compound C.O=C=O KDRIEERWEFJUSB-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- JAGQSESDQXCFCH-UHFFFAOYSA-N methane;molybdenum Chemical compound C.[Mo].[Mo] JAGQSESDQXCFCH-UHFFFAOYSA-N 0.000 description 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
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- 230000010287 polarization Effects 0.000 description 1
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- 238000010189 synthetic method Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- B01J27/22—Carbides
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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Abstract
本发明提供了一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,按照以下步骤进行:将四水合钼酸铵、葡萄糖和氯化钠溶解到去离子水中,得到混合液,将混合液通过冷冻干燥的方法得到均匀混合的固体原料,然后将得到的固体原料通过碳热还原反应方法,在氢气/氮气混合气体下高温反应,从而得到石墨烯负载碳化钼纳米颗粒复合结构。本发明采用高温碳热还原反应方法,通过改变反应温度实现葡萄糖的碳化,同时将原料四水合钼酸铵还原成碳化钼纳米颗粒,进而获得石墨烯负载碳化钼纳米颗粒复合结构。
Description
技术领域
本发明涉及一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,属于能源和催化材料领域。
背景技术
近年来过渡金属碳化物因其独特的电子结构和优良的催化性能成为了新型无机催化材料研究领域的一个研究热点。碳化钼(Mo2C)是碳原子进入过渡金属钼晶格而产生的一类具有金属性质的间充型化合物;它结合了3种不同物质的特性:共价固体、离子晶体和过渡金属,从而具有特殊的物理和化学性质,碳化钼表现出了和共价固体一样的硬度和脆度,和典型的离子晶体一样具有简单的晶体结构和高的熔点,具有硬度大、熔点高、抗腐蚀等特点。
碳化钼是具有金属光泽的灰色粉末,具有很高的熔点和硬度、良好的热稳定性和机械稳定性、极好的抗腐蚀性等优点。研究表明碳化钼还具有类似贵金属的电子结构和催化特性,碳化钼催化剂在加氢脱氮、加氢脱硫、选择加氢、烷烃异构化、甲烷二氧化碳重整、水汽转变等反应中都表现出了较高催化活性,在一些反应中其催化性能可以与铂、铱等贵金属催化剂相媲美,被誉为“类铂催化剂”,因此碳化钼催化剂正引起国内外学者的广泛关注。Mo2C催化剂的合成方法有:高温合成发、程序升温反应法(TPR)、溶胶凝胶法(Sel-gel)、化学气相沉积法(CVD)、碳热还原法(CTR)等。
发明内容
本发明目的在于提供一种简易的石墨烯负载碳化钼纳米颗粒复合结构的制备方法。该方法具有工艺流程简单,极易操作,有望大量生产等优点,因此可作为一种适于大量制备石墨烯负载碳化钼纳米颗粒复合结构的理想方法。
本发明的技术方案是:
一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,按照以下步骤进行:
将四水合钼酸铵、葡萄糖和氯化钠溶解到去离子水中,得到混合液,将混合液通过冷冻干燥的方法得到均匀混合的固体原料,然后将得到的固体原料通过碳热还原反应方法,在氢气/氮气混合气体下高温反应,从而得到石墨烯负载碳化钼纳米颗粒复合结构。
在制备混合液时,葡萄糖在去离子水中的浓度为6~8mg/mL,所使用的葡萄糖、四水合钼酸铵的质量比为1~4:1,葡萄糖、氯化钠的质量比为3~4:147。
在制备混合液时,所使用的葡萄糖、四水合钼酸铵的质量比为2:1。
所述的冷冻干燥的温度为-40℃,冷冻干燥的时间为24h。
所述氢气/氮气混合气体为5%H2/95%N2,气流流速为流速100sccm。
所述的高温反应的温度为750~950℃,升温速率为5℃/min,在750~950℃下保持的反应时间为120min。
所述的高温反应的温度为优选为850℃。
有益效果:
1.本发明将不同质量比例的葡萄糖和四水合钼酸铵溶解到水溶液中,通过冷冻干燥的方法得到混合均匀的固体原料,实现原料的充分均匀混合。
2.本发明采用高温碳热还原反应方法,通过改变反应温度实现葡萄糖的碳化,同时将原料四水合钼酸铵还原成碳化钼纳米颗粒,进而获得石墨烯负载碳化钼纳米颗粒的复合结构。
3.本发明工艺流程简单,操作容易,成本低,可有望大量生产。
总之,通过冷冻干燥不同质量比例的葡萄糖和四水合钼酸铵的水溶液实现原料的充分混合,采用高温碳热还原反应方法,通过改变反应温度实现葡萄糖的碳化和钼酸铵的还原,成功制备了石墨烯负载碳化钼纳米颗粒的复合结构。
附图说明
图1为各实施例中不同条件下合成的石墨烯负载碳化钼纳米颗粒复合结构的XRD图,图中曲线1~5依次为实施例1~5的所得样品XRD图谱;
图2为石墨烯负载碳化钼纳米颗粒复合结构的透射电镜图片;
图3为石墨烯负载碳化钼纳米颗粒复合结构的电催化制氢性能图。
具体实施方式
以下通过实施例对本发明进行具体描述或作进一步说明,其目的在于更好的理解本发明的技术内涵,但是本发明的保护范围不限于以下的实施范围。
实施例1:
原料葡萄糖(C6H12O6·H2O)、四水合钼酸铵(H24Mo7N6O24·4H2O)和氯化钠(NaCl)质量分别为0.3g、0.3g和14.7g,将H24Mo7N6O24·4H2O、C6H12O6·H2O和NaCl溶于50mL去离子水中,-40℃下冷冻干燥24h后,在5%H2/95%N2(流速100sccm)下以5℃/min升温至850℃,保温120min后自然冷却。
X射线衍射(XRD)表明,所得产物为纯的Mo2C晶相。
实施例2:
与实施例1不同之处在于:
原料葡萄糖(C6H12O6·H2O)、四水合钼酸铵(H24Mo7N6O24·4H2O)和氯化钠(NaCl)质量分别为0.4g、0.2g和14.7g,将H24Mo7N6O24·4H2O、C6H12O6·H2O和NaCl溶于50mL去离子水中,-40℃下冷冻干燥24h后,在5%H2/95%N2(流速100sccm)下以5℃/min升温至850℃,保温120min后自然冷却。
X射线衍射(XRD)表明,所得产物为纯的Mo2C晶相。
实施例3:
与实施例1不同之处在于:
原料葡萄糖(C6H12O6·H2O)、四水合钼酸铵(H24Mo7N6O24·4H2O)和氯化钠(NaCl)质量分别为0.32g、0.08g和14.7g,将H24Mo7N6O24·4H2O、C6H12O6·H2O和NaCl溶于50mL去离子水中,-40℃下冷冻干燥24h后,在5%H2/95%N2(流速100sccm)下以5℃/min升温至850℃,保温120min后自然冷却。
X射线衍射(XRD)表明,所得产物为纯的Mo2C晶相。
实施例4:
与实施例2不同之处在于:
原料葡萄糖(C6H12O6·H2O)、四水合钼酸铵(H24Mo7N6O24·4H2O)和氯化钠(NaCl)质量分别为0.4g、0.2g和14.7g,将H24Mo7N6O24·4H2O、C6H12O6·H2O和NaCl溶于50mL去离子水中,-40℃下冷冻干燥24h后,在5%H2/95%N2(流速100sccm)下以5℃/min升温至750℃,保温120min后自然冷却。
X射线衍射(XRD)表明,所得产物为纯的Mo2C晶相。
实施例5:
与实施例2不同之处在于:
原料葡萄糖(C6H12O6·H2O)、四水合钼酸铵(H24Mo7N6O24·4H2O)和氯化钠(NaCl)质量分别为0.4g、0.2g和14.7g,将H24Mo7N6O24·4H2O、C6H12O6·H2O和NaCl溶于50mL去离子水中,-40℃下冷冻干燥24h后,在5%H2/95%N2(流速100sccm)下以5℃/min升温至950℃,保温120min后自然冷却。
X射线衍射(XRD)表明,所得产物为纯的Mo2C晶相。
图1的XRD图样表明碳化钼相的XRD峰和JCPDS卡片的35-787号图案(碳化钼)相符,图中1-5依次为实施例1-实施例5的所得样品XRD图谱结果。
图2的TEM图像揭示复合物的结构为碳化钼颗粒均匀负载在石墨烯片上。
图3给出的是石墨烯负载碳化钼纳米颗粒复合结构的极化曲线。可以看出该方法制备的石墨烯负载碳化钼纳米颗粒复合结构,在电流密度为20mA/cm2时过电位199mV,说明该方法可以直接制备得到具有优异电催化性能的碳化钼催化剂。
Claims (7)
1.一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,其特征在于,按照以下步骤进行:
将四水合钼酸铵、葡萄糖和氯化钠溶解到去离子水中,得到混合液,将混合液通过冷冻干燥的方法得到均匀混合的固体原料,然后将得到的固体原料通过碳热还原反应方法,在氢气/氮气混合气体下高温反应,从而得到石墨烯负载碳化钼纳米颗粒复合结构。
2.根据权利要求1所述的一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,其特征在于,在制备混合液时,葡萄糖在去离子水中的浓度为6~8mg/mL,所使用的葡萄糖、四水合钼酸铵的质量比为1~4:1,葡萄糖、氯化钠的质量比为3~4:147。
3.根据权利要求1或2所述的一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,其特征在于,在制备混合液时,所使用的葡萄糖、四水合钼酸铵的质量比为2:1。
4.根据权利要求1所述的一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,其特征在于,所述的冷冻干燥的温度为-40℃,冷冻干燥的时间为24h。
5.根据权利要求1所述的一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,其特征在于,所述氢气/氮气混合气体为5%H2/95%N2,气流流速为流速100sccm。
6.根据权利要求1所述的一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,其特征在于,所述的高温反应的温度为750~950℃,升温速率为5℃/min,在750~950℃下保持的反应时间为120min。
7.根据权利要求6所述的一种利用碳热反应制备石墨烯负载碳化钼纳米颗粒复合结构的方法,其特征在于,所述的高温反应的温度为为850℃。
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