CN108862387A - 一种异形纳米二硫化钼材料的制备方法 - Google Patents
一种异形纳米二硫化钼材料的制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 37
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 19
- 238000004073 vulcanization Methods 0.000 claims abstract description 13
- 238000003486 chemical etching Methods 0.000 claims abstract description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 9
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 9
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 9
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 9
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 9
- 239000011733 molybdenum Substances 0.000 claims abstract description 9
- 238000005470 impregnation Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 18
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 239000012876 carrier material Substances 0.000 claims description 2
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
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- 238000006392 deoxygenation reaction Methods 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 abstract description 6
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- 229910052739 hydrogen Inorganic materials 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000005518 electrochemistry Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003208 petroleum Substances 0.000 abstract description 3
- 238000012827 research and development Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
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- 239000003054 catalyst Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提出了一种异形纳米级MoS2材料的制备方法。其制备工艺的特点是先使用多种氧化物纳米颗粒为载体,以钼酸铵为钼前驱物种浸渍氧化物载体,烘干、焙烧后于特定的硫化条件(选取特殊的硫化气氛与硫化温度)下制得负载型MoS2材料,最后以氢氟酸化学刻蚀去除氧化物载体,即可得到尺寸在几纳米~几十纳米范围,形状由三角形‑切角三角形‑六边形变化的异形纳米级MoS2材料。异型纳米级MoS2具有特殊的催化活性,其合成与研发可望在相关领域获得后续应用;特别是二硫化钼(MoS2)材料在石油馏分油加氢、电化学制氢、固体润滑剂等领域具有广泛的应用。
Description
技术领域
本发明涉及化工材料领域中的一种异形纳米二硫化钼材料的制备方法,其制备的二硫化钼(MoS2)材料在石油馏分油加氢精制、电化学制氢、固体润滑剂等领域具有广泛的应用。
背景技术
目前,以水热法、溶剂热法等常规合成方法在制备二硫化钼材料存在诸多局限。一方面,所得MoS2的尺寸一般在几百纳米~微米级别,这限制了其在馏分油加氢、电催化等方面的催化活性或使用性能。如能定向合成纳米级MoS2材料,可望在相关领域获得较好的应用效果。
另一方面,常规合成方法所得MoS2材料一般外形呈现为尺寸在几百纳米~微米区间的、花瓣状团簇物质,其实质组成为晶体学稳定的六边形颗粒的聚集体。如能调控MoS2材料颗粒的外形,不仅限于稳定状态的六边形,其意义是可望为加氢反应、电化学催化等领域提供新的活性中心或者活性位点,进而开发出新型的高活性催化剂。
发明内容
本发明针对现有技术存在的问题,提出了一种制备成为尺寸几纳米~几十纳米范围,形状由三角形-切角三角形-六边形变化,且有利于提高MoS2材料的各类性质或催化活性的异形纳米级MoS2材料的制备方法。
本发明的异形纳米二硫化钼材料的制备方法,包括:
(1)预先经过空气气氛焙烧的纳米级氧化物颗粒为载体,浸渍钼酸铵溶液;
(2)经过空气中的干燥、焙烧过程制得负载型氧化钼(MoO3)材料;
(3)在硫化条件下制得负载型二硫化钼材料;
(4)最后经过氢氟酸化学刻蚀去除氧化物载体,得到异形纳米级二硫化钼材料。
上述方案进一步包括:
步骤(1)中所述纳米级氧化物颗粒为载体包括纳米级的TiO2、ZrO2、SiO2或Al2O3载体,各载体材料使用前需经过空气气氛500-600℃焙烧1.5-2.5小时;
步骤(2)中以钼酸铵为钼前驱物种,以前述处理得到的纳米氧化物颗粒载体浸渍钼酸铵水溶液,在空气气氛中烘干后于500-600℃焙烧3.5-4.5小时,得到MoO3,氧化物载体复合材料,其中钼物种负载量以MoO3计的质量百分比为5~15%;
步骤(3)中将前述得到的负载型MoO3材料在硫化气氛为10%H2S-H2或10%H2S-N2,硫化温度为250~750℃,硫化时间为3.5-4.5小时。
步骤(4)中将步骤(3)得到的氧化物负载的MoS2复合材料,以氢氟酸化学刻蚀法去除氧化物载体,最终得到纳米级异形MoS2材料。
步骤(1)中所述焙烧是在550℃焙烧2小时;
步骤(2)中烘干和焙烧是在空气气氛中100℃烘干后于550℃焙烧4小时;
步骤(3)中的硫化时间为4小时。
步骤(4)中氢氟酸化学刻蚀法的工艺条件为:氢氟酸用量为相对复合材料中所含氧化物载体全部反应化学计量用量的5-30倍,搅拌并控制反应时间为2-12小时,反应后得到的混合物体系经过1~3次高速离心-洗涤过程,所得产物室温晾干即得。
按照本发明制备的异型纳米级MoS2具有特殊的催化活性,其合成与研发可望在相关领域获得后续应用。其特点是应用多种氧化物纳米颗粒为载体,以钼酸铵为钼前驱物种浸渍氧化物载体,焙烧后于特定的硫化条件(包括硫化气氛、硫化温度的选取)下制备得到负载型MoS2材料,而后经过氢氟酸化学刻蚀去除载体,最后可以得到尺寸在几纳米~几十纳米范围,形状由三角形-切角三角形-六边形变化的异形纳米级MoS2材料。该型MoS2的合成与研发可望在相关领域获得后续应用;特别是在石油馏分油加氢精制、电化学制氢、固体润滑剂等领域具有广泛的应用。
附图说明
图1为一组不同制备工艺所得异形MoS2纳米颗粒的透射电子显微镜照片;
图中:1、Al2O3载体,H2S-H2,750℃;2、Al2O3载体,H2S-N2,550℃;3、SiO2载体,H2S-N2,550℃;4、SiO2载体,H2S-N2,750℃;5、ZrO2载体,H2S-N2,450℃;6、ZrO2载体,H2S-N2,750℃;7、TiO2载体,H2S-H2,750℃;8、TiO2载体,H2S-N2,750℃。
具体实施方式
下面结合具体实施例对本发明作进一步说明:
实施例1:
以预先经过空气气氛焙烧的纳米级氧化物颗粒为载体,浸渍一定量的钼酸铵溶液,而后经过空气中的干燥、焙烧过程制得负载型氧化钼(MoO3)材料,而后在特定的硫化条件下(选取特定的硫化气氛、硫化温度)制得负载型二硫化钼材料,最后经过氢氟酸化学刻蚀去除氧化物载体,得到异形纳米级二硫化钼材料。
其中:氧化物颗粒载体的可选类型为纳米级的TiO2,ZrO2,SiO2以及Al2O3载体,各载体材料使用前需经过空气气氛550℃焙烧2小时。
以钼酸铵为钼前驱物种,以前述处理得到的纳米氧化物载体浸渍钼酸铵水溶液,在空气气氛中100℃烘干后于550℃焙烧4小时得到MoO3-氧化物载体复合材料,其中钼物种的负载量为5~15%(质量百分比,以MoO3计)。
将前述得到的负载型MoO3材料于一定的条件下硫化得到负载型MoS2材料,硫化气氛可选为10%H2S-H2或10%H2S-N2,硫化温度为250~750℃,硫化时间为4小时。
将前述得到的氧化物负载的MoS2复合材料,以氢氟酸化学刻蚀法去除氧化物载体,最终得到纳米级异形MoS2材料。该工艺方法可以参见申请人前述专利所述(ZL201410349250.6)。
对于本发明具体氢氟酸化学刻蚀法的工艺条件为:氢氟酸用量为相对催化剂所含氧化物载体全部反应化学计量用量的5-30倍,搅拌并控制反应时间为2-12小时,反应后得到的混合物体系经过1~3次高速离心-乙醇洗涤过程,所得产物室温晾干即得。
这里固定Mo物种的负载量为10%(质量百分比,以MoO3计),更换各种氧化物载体,在不同的硫化条件下可以得到特定形状与尺寸的MoS2。各制备条件所得MoS2材料的具体形貌和尺寸需经过氢氟酸化学刻蚀去除载体后,以高分辨透射电子显微镜观察统计获得。
系列实施例:
典型结果汇总如表1所示。
表1 部分制备条件获得MoS2纳米颗粒的形状与尺寸汇总
典型MoS2纳米颗粒的透射电镜照片见图1所示。
结合附图1,不同制备工艺所得异形MoS2纳米颗粒的透射电子显微镜照片:
1)Al2O3载体,H2S-H2,750℃;2)Al2O3载体,H2S-N2,550℃;
3)SiO2载体,H2S-N2,550℃;4)SiO2载体,H2S-N2,750℃;
5)ZrO2载体,H2S-N2,450℃;6)ZrO2载体,H2S-N2,750℃;
7)TiO2载体,H2S-H2,750℃;8)TiO2载体,H2S-N2,750℃。
图片表明,依照本发明制备的异形纳米二硫化钼材料确实是纳米级尺寸的异形硫化钼颗粒。
Claims (4)
1.一种异形纳米二硫化钼材料的制备方法,其特征是:
(1)预先经过空气气氛焙烧的纳米级氧化物颗粒为载体,浸渍钼酸铵溶液;
(2)经过空气中的干燥、焙烧过程制得负载型氧化钼(MoO3)材料;
(3)在硫化条件下制得负载型二硫化钼材料;
(4)最后经过氢氟酸化学刻蚀去除氧化物载体,得到异形纳米级二硫化钼材料。
2.根据权利要求1所述的异形纳米二硫化钼材料的制备方法,其特征是:
步骤(1)中所述纳米级氧化物颗粒为载体包括纳米级的TiO2、ZrO2、SiO2或Al2O3载体,各载体材料使用前需经过空气气氛500-600℃焙烧1.5-2.5小时;
步骤(2)中以钼酸铵为钼前驱物种,以前述处理得到的纳米氧化物颗粒载体浸渍钼酸铵水溶液,在空气气氛中烘干后于500-600℃焙烧3.5-4.5小时,得到MoO3,氧化物载体复合材料,其中钼物种负载量以MoO3计的质量百分比为5~15%;
步骤(3)中将前述得到的负载型MoO3材料,硫化气氛为10%H2S-H2或10%H2S-N2,硫化温度为250~750℃,硫化时间为3.5-4.5小时;
步骤(4)中将步骤(3)得到的氧化物负载的MoS2复合材料,以氢氟酸化学刻蚀法去除氧化物载体,最终得到纳米级异形MoS2材料。
3.根据权利要求2所述的异形纳米二硫化钼材料的制备方法,其特征是:
步骤(1)中所述焙烧是在550℃焙烧2小时;
步骤(2)中烘干和焙烧是在空气气氛中100℃烘干后于550℃焙烧4小时;
步骤(3)中的硫化时间为4小时。
4.根据权利要求2或3所述的异形纳米二硫化钼材料的制备方法,其特征是:
步骤(4)中氢氟酸化学刻蚀法的工艺条件为:氢氟酸用量为相对复合材料中所含氧化物载体全部反应化学计量用量的5-30倍,搅拌并控制反应时间为2-12小时,反应后得到的混合物体系经过1~3次高速离心-洗涤过程,所得产物室温晾干即得。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111530480A (zh) * | 2020-05-20 | 2020-08-14 | 杭州师范大学 | 一种多孔层状过渡金属硫族化合物及其制备方法和应用 |
CN114058353A (zh) * | 2021-12-02 | 2022-02-18 | 中国石油大学(北京) | 一种Janus改性二硫化钼纳米颗粒及其制备方法与驱油材料 |
CN114560502A (zh) * | 2020-11-27 | 2022-05-31 | 国电南瑞科技股份有限公司 | 一种三维纳米钼基锂离子电池负极材料及其制备方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3661508A (en) * | 1970-12-14 | 1972-05-09 | Sylvania Electric Prod | Process for producing molybdenum disulfide |
CN102583546A (zh) * | 2012-02-18 | 2012-07-18 | 长安大学 | 以介孔二氧化硅分子筛为硬模板合成介孔二硫化钼的方法 |
CN103910340A (zh) * | 2014-03-13 | 2014-07-09 | 杭州师范大学 | 一种金属硫族化合物纳米筛材料的制备方法 |
CN104122128A (zh) * | 2014-07-22 | 2014-10-29 | 中国石油大学(华东) | 一种氧化铝负载硫化态钼(钨)基加氢催化剂活性相的样品制备方法 |
-
2018
- 2018-05-30 CN CN201810534413.6A patent/CN108862387A/zh active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3661508A (en) * | 1970-12-14 | 1972-05-09 | Sylvania Electric Prod | Process for producing molybdenum disulfide |
CN102583546A (zh) * | 2012-02-18 | 2012-07-18 | 长安大学 | 以介孔二氧化硅分子筛为硬模板合成介孔二硫化钼的方法 |
CN103910340A (zh) * | 2014-03-13 | 2014-07-09 | 杭州师范大学 | 一种金属硫族化合物纳米筛材料的制备方法 |
CN104122128A (zh) * | 2014-07-22 | 2014-10-29 | 中国石油大学(华东) | 一种氧化铝负载硫化态钼(钨)基加氢催化剂活性相的样品制备方法 |
Non-Patent Citations (3)
Title |
---|
JOHN REARDON ET AL.: "Tailoring Alumina Surface Chemistry for Efficient Use of Supported MoS2", 《JOURNAL OF CATALYSIS》 * |
YANPENG LI ET AL.: "Application of HF etching in a HRTEM study of supported MoS2 catalysts", 《JOURNAL OF CATALYSIS》 * |
潘履让: "《固体催化剂的设计与制备》", 31 December 1993, 南开大学出版社 * |
Cited By (6)
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CN111530480B (zh) * | 2020-05-20 | 2022-11-25 | 杭州师范大学 | 一种多孔层状过渡金属硫族化合物及其制备方法和应用 |
US11577228B2 (en) * | 2020-05-20 | 2023-02-14 | Hangzhou Normal University | Porous layered transition metal dichalcogenide and preparation method and use thereof |
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