CN107234246B - 一种超薄Rh纳米片组成的纳米花的制备方法 - Google Patents
一种超薄Rh纳米片组成的纳米花的制备方法 Download PDFInfo
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 2
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 abstract description 2
- 229910001630 radium chloride Inorganic materials 0.000 abstract description 2
- LGRDAQPMSDIUQJ-UHFFFAOYSA-N tripotassium;cobalt(3+);hexacyanide Chemical compound [K+].[K+].[K+].[Co+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] LGRDAQPMSDIUQJ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000010948 rhodium Substances 0.000 description 29
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- 229910052700 potassium Inorganic materials 0.000 description 3
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- RKBAPHPQTADBIK-UHFFFAOYSA-N cobalt;hexacyanide Chemical compound [Co].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] RKBAPHPQTADBIK-UHFFFAOYSA-N 0.000 description 1
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- 229910052703 rhodium Inorganic materials 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/464—Rhodium
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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Abstract
本发明公开了一种超薄Rh纳米片组成的纳米花的制备方法,该方法以氯化铑和钴氰化钾为原料合成RhCl3‑K3Co(CN)6氰胶前驱体,再以甲醛做还原剂,采用氰胶还原法还原RhCl3‑K3Co(CN)6氰胶前驱体,即可得到形状规则、尺寸均一、分散性及稳定性良好的Rh纳米片组成的纳米花。本发明制备方法简单、经济,制得的Rh纳米花对合成氨催化反应展现出优异的电催化活性和稳定性,在电化学合成氨方面有广泛的应用前景。
Description
技术领域
本发明涉及一种Rh纳米花的制备方法,尤其涉及一种超薄Rh纳米片组成的纳米花的制备方法,该Rh纳米花作为催化剂对合成氨展现出较高的催化活性和稳定性。
背景技术
近些年,贵金属催化剂一直深受广大科研者的关注,由于其在各个领域(例如电化学催化、化学催化、生物制药等)都有着优异的催化活性。然而由于其价格昂贵,全球储量低的缺点,严重的限制了它的商业化发展。
近几年的研究表明,二维材料可以大大提升催化剂的原子利用率,从而大大提升了催化剂的催化活性,因此受到了越来越多的关注。二维材料具有超大的比表面积,更多的活性位点等优点。因此,寻找制备超薄的二维贵金属纳米材料的方法,成为了当前材料领域的热点问题。然而,二维贵金属材料由于动力学难以控制而难被合成出来。
发明内容
本发明所要解决的技术问题在于提供一种简单有效的氰胶还原方法制备超薄Rh纳米片组成的纳米花的方法。
解决上述技术问题所采用的技术方案由下述步骤组成:
1、制备RhCl3-K3Co(CN)6氰胶
将RhCl3水溶液和K3Co(CN)6水溶液混合均匀,在75~100℃下加热反应20~36小时,得到RhCl3-K3Co(CN)6氰胶。
2、制备超薄Rh纳米片组成的纳米花
将RhCl3-K3Co(CN)6氰胶与甲醛水溶液混合,在160~190℃下还原反应10~16小时,反应结束后冷却、离心、洗涤、干燥,得到超薄Rh纳米片组成的纳米花。
上述步骤1中,所述RhCl3水溶液中RhCl3的浓度为0.025~0.3mol/L,K3Co(CN)6水溶液中K3Co(CN)6的浓度为0.05~0.3mol/L,RhCl3与K3Co(CN)6的摩尔比为1:0.25~2;优选RhCl3水溶液中RhCl3的浓度为0.05~0.15mol/L,K3Co(CN)6水溶液中K3Co(CN)6的浓度为0.05~0.15mol/L,RhCl3与K3Co(CN)6的摩尔比为1:0.5~1。
上述步骤1中,进一步优选在90~95℃下还原反应24小时。
上述步骤2中,所述RhCl3-K3Co(CN)6氰胶与甲醛水溶液的体积比为1.5~5:1,优选RhCl3-K3Co(CN)6氰胶与甲醛水溶液的体积比为2~4:1,所述甲醛水溶液中甲醛的质量浓度为20%~40%。
上述步骤2中,进一步优选在180℃下还原反应12小时。
本发明的有益效果如下:
1、本发明采用氯化铑和钴氰化钾为原料合成RhCl3-K3Co(CN)6氰胶,以RhCl3-K3Co(CN)6氰胶为前驱体,再以甲醛做还原剂,采用简单的氰胶还原法将RhCl3-K3Co(CN)6氰胶前驱体还原,即可得到形状规则、尺寸均一、分散性及稳定性良好的Rh纳米片组成的纳米花。
2、本发明不需要较长的反应时间,不需要复杂的pH调控过程,操作简单,产品产量高且均一性好,适合大规模生产。
3、本发明制备的Rh纳米片组成的纳米花与商业化铑相比,对合成氨催化反应展现出优异的电催化活性和稳定性,在合成氨领域具有潜在的应用前景。
附图说明
图1是实施例1制备的Rh纳米片组成的纳米花的TEM图。
图2是实施例1制备的Rh纳米片组成的纳米花的SEM图。
图3是实施例2制备的Rh纳米片组成的纳米花的SEM图。
图4是实施例3制备的Rh纳米片组成的纳米花的SEM图。
图5是实施例4制备的Rh纳米片组成的纳米花的SEM图。
图6是实施例5制备的Rh纳米片组成的纳米花的SEM图。
图7是实施例6制备的Rh纳米片组成的纳米花的SEM图。
图8是Rh黑和实施例1制备的Rh纳米片组成的纳米花分别电催化合成氨测试图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
1、制备RhCl3-K3Co(CN)6氰胶
将1mL 0.05mol/L三氯化铑水溶液和0.5mL 0.05mol/L六氰合钴酸钾水溶液超声混合均匀,在95℃下加热反应24小时,得到RhCl3-K3Co(CN)6氰胶。
2、制备超薄Rh纳米片组成的纳米花
向1.5mL RhCl3-K3Co(CN)6氰胶中加入0.5mL质量浓度为37%~40%的甲醛水溶液,在180℃下加热反应12小时,反应结束后冷却至常温,离心分离、用去离子水洗涤、60℃干燥,得到超薄Rh纳米片组成的纳米花(见图1和图2),纳米片的厚度为1.0~1.1nm。
实施例2
本实施例的步骤1中,将1mL 0.05mol/L三氯化铑水溶液和1mL 0.05mol/L六氰合钴酸钾水溶液超声混合均匀,在95℃下加热反应24小时,得到RhCl3-K3Co(CN)6氰胶。其他步骤与实施例1相同,得到超薄Rh纳米片组成的纳米花(见图3)。
实施例3
本实施例的步骤1中,将1mL 0.05mol/L三氯化铑水溶液和0.5mL 0.05mol/L六氰合钴酸钾水溶液超声混合均匀,在80℃下加热反应24小时,得到RhCl3-K3Co(CN)6氰胶。其他步骤与实施例1相同,得到超薄Rh纳米片组成的纳米花(见图4)。
实施例4
本实施例的步骤2中,向1.5mL RhCl3-K3Co(CN)6氰胶中加入1mL质量浓度为37%~40%的甲醛水溶液,在180℃下加热反应12小时,其他步骤与实施例1相同,得到超薄Rh纳米片组成的纳米花(见图5)。
实施例5
本实施例的步骤2中,向1.5mL RhCl3-K3Co(CN)6氰胶中加入0.5mL质量浓度为37%~40%的甲醛水溶液,在200℃下加热反应12小时,其他步骤与实施例1相同,得到超薄Rh纳米片组成的纳米花(见图6)。
实施例6
本实施例的步骤1中,将1mL 0.15mol/L三氯化铑水溶液和1mL 0.15mol/L六氰合钴酸钾水溶液超声混合均匀,在75℃下加热反应36小时,得到RhCl3-K3Co(CN)6氰胶。其他步骤与实施例1相同,得到超薄Rh纳米片组成的纳米花(见图7)。
发明人采用实施例1得到的超薄Rh纳米片组成的纳米花电催化合成氨,具体方法为:将4mg超薄Rh纳米片组成的纳米花加入1mL由乙醇、水、萘酚按体积比为3:7:0.33混合的混合液中,混合均匀,取所得混合液20μL滴加0.5×0.5cm2碳布上,待干燥后即可用于电化学测试,测试结果见图8。由图8可见,与商业化Rh黑相比,本发明制备的Rh纳米片组成的纳米花对电化学合成氨具有超高的电催化活性。
Claims (6)
1.一种超薄Rh纳米片组成的纳米花的制备方法,其特征在于它由下述步骤组成:
(1)制备RhCl3-K3Co(CN)6氰胶
将RhCl3水溶液和K3Co(CN)6水溶液混合均匀,在75~100℃下加热反应20~36小时,得到RhCl3-K3Co(CN)6氰胶;所述RhCl3水溶液中RhCl3的浓度为0.025~0.3mol/L,K3Co(CN)6水溶液中K3Co(CN)6的浓度为0.025~0.3mol/L,RhCl3与K3Co(CN)6的摩尔比为1:0.25~2;
(2)制备超薄Rh纳米片组成的纳米花
将RhCl3-K3Co(CN)6氰胶与甲醛水溶液按体积比为1.5~5:1混合,在160~190℃下还原反应10~16小时,反应结束后冷却、离心、洗涤、干燥,得到超薄Rh纳米片组成的纳米花。
2.根据权利要求1所述的超薄Rh纳米片组成的纳米花的制备方法,其特征在于:步骤(1)中,所述RhCl3水溶液中RhCl3的浓度为0.05~0.15mol/L,K3Co(CN)6水溶液中K3Co(CN)6的浓度为0.05~0.15mol/L,RhCl3与K3Co(CN)6的摩尔比为1:0.5~1。
3.根据权利要求1或2所述的超薄Rh纳米片组成的纳米花的制备方法,其特征在于:步骤(1)中,在90~95℃下还原反应24小时。
4.根据权利要求1所述的超薄Rh纳米片组成的纳米花的制备方法,其特征在于:步骤(2)中,所述RhCl3-K3Co(CN)6氰胶与甲醛水溶液的体积比为2~4:1。
5.根据权利要求1或4所述的超薄Rh纳米片组成的纳米花的制备方法,其特征在于:所述甲醛水溶液中甲醛的质量浓度为20%~40%。
6.根据权利要求5所述的超薄Rh纳米片组成的纳米花的制备方法,其特征在于:步骤(2)中,在180℃下还原反应12小时。
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