CN107029751A - 高活性铂铜催化剂的制备方法 - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 55
- WBLJAACUUGHPMU-UHFFFAOYSA-N copper platinum Chemical compound [Cu].[Pt] WBLJAACUUGHPMU-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010792 warming Methods 0.000 claims abstract description 19
- 239000006229 carbon black Substances 0.000 claims abstract description 14
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 12
- 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 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 10
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 7
- 229960003280 cupric chloride Drugs 0.000 claims abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000001805 chlorine compounds Chemical class 0.000 claims 2
- 229910052697 platinum Inorganic materials 0.000 abstract description 9
- 238000006722 reduction reaction Methods 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- -1 Fig. 1 Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- Organic Chemistry (AREA)
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Abstract
本发明涉及铂铜催化剂生产领域,具体涉及一种高活性铂铜催化剂的制备方法。分别称取硝酸铂153mg、43mg无水氯化铜,加入50mL蒸馏水溶解,将其置于超声剪切机中剪切分散30min,备用。再分别称取碳黑(XC‑72)1.0g、水合肼20ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌10h,再升温至90℃,反应1h,经过滤、洗涤、干燥后得到高活性铂铜催化剂。优点是成本低、反应时间短、适合规模化制备的化学还原方法,所制备的催化剂铂颗粒较小且分布均匀。
Description
技术领域
本发明涉及铂铜催化剂生产领域,具体涉及一种高活性铂铜催化剂的制备方法。
背景技术
铂碳催化剂是将贵金属铂负载在活性炭上制备得到的一种电化学催化剂。铂碳催化剂主要用于燃料电池的氢气氧化、甲醇氧化、甲酸氧化以及氧气的还原。
铂碳催化剂的优劣主要由催化剂活性、稳定性和成本来评价。影响催化剂活性的因素有很多,如载体的性能(比表面积、孔结构、表面化学性质等)、催化剂中活性金属的含量和颗粒大小、活性金属在载体上的宏观和微观分布等。为了降低成本,减少贵金属铂的用量,引入非贵金属制备双金属或多金属催化剂是一种有效途径。本发明主要是一种成本低、适合规模化制备的化学还原方法,制备出铂铜双金属催化剂,所制备的催化剂铂颗粒较小且分布均匀。
发明内容
为了解决上述问题,本发明提出了高活性铂铜催化剂的制备方法,主要是一种成本低、反应时间短、适合规模化制备的化学还原方法,所制备的催化剂铂颗粒较小且分布均匀。
本发明的技术方案:
高活性铂铜催化剂的制备方法,具体步骤如下:分别称取硝酸铂153 mg、43mg无水氯化铜,加入50 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散30min,备用。再分别称取碳黑1.0 g、水合肼20 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌10 h,再升温至90℃,反应1h,经过滤、洗涤、干燥后得到高活性铂铜催化剂。所述的高活性铂铜催化剂中的Pt铜颗粒为4nm,以此催化剂制备的膜电极。
高活性铂铜催化剂的制备方法,其步骤如下:分别称取硝酸铂230mg、64.5mg无水氯化铜,加入100 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散30min,备用。再分别称取碳黑1.0 g、水合肼50 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌10 h,再升温至90℃,反应1h,经过滤、洗涤、干燥后得到高活性铂铜催化剂,高活性铂铜催化剂是15%铂铜催化剂。
高活性铂铜催化剂的制备方法,其步骤如下:分别称取硝酸铂765 mg、215mg无水氯化铜,加入300 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散50min,备用。再分别称取碳黑1.0 g、水合肼100 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌15 h,再升温至95℃,反应2h,经过滤、洗涤、干燥后得到高活性铂铜催化剂,高活性铂铜催化剂是50%铂铜催化剂。
所述的碳黑是碳黑XC-72。
铂铜催化剂中铂的质量含量可以从0-99%,但是铂的含量越高越不好做。我们能做到低载量的(10-40%),也能做高载量的(50-70%)。
本发明的优点是成本低、反应时间短、适合规模化制备的化学还原方法,所制备的催化剂铂颗粒较小且分布均匀。
附图说明
图1是催化剂的TEM图。
图2是膜电极极化曲线示意图。
具体实施方式
实施例1
高活性铂铜催化剂的制备方法,分别称取硝酸铂153 mg、43mg无水氯化铜,加入50 mL蒸馏水溶解,将其置于超声剪切机中剪切分散30min,备用。再分别称取碳黑(XC-72)1.0 g、水合肼20 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌10 h,再升温至90℃,反应1h,经过滤、洗涤、干燥后得到高活性铂铜催化剂。所得催化剂如图1,Pt铜颗粒为4nm左右,以此催化剂制备的膜电极性能如图2。电池温度:55℃,空气:常压、2000ml/min、30%湿度,H2:背压0.04MPa 不加湿。
实施例2
15 %铂铜催化剂的制备方法,其步骤如下:
分别称取硝酸铂230mg、64.5mg无水氯化铜,加入100 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散30min,备用。再分别称取碳黑(XC-72)1.0 g、水合肼50 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌10 h,再升温至90℃,反应1h,经过滤、洗涤、干燥后得到高活性铂铜催化剂。
实施例3
50%铂铜催化剂的制备方法,其步骤如下:
分别称取硝酸铂765 mg、215mg无水氯化铜,加入300 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散50min,备用。再分别称取碳黑(XC-72)1.0 g、水合肼100 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌15 h,再升温至95℃,反应2h,经过滤、洗涤、干燥后得到高活性铂铜催化剂。
Claims (5)
1.高活性铂铜催化剂的制备方法,其特征在于,具体步骤如下:分别称取硝酸铂153mg、43mg无水氯化铜,加入50 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散30min,备用;再分别称取碳黑1.0 g、水合肼20 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌10 h,再升温至90℃,反应1h,经过滤、洗涤、干燥后得到高活性铂铜催化剂。
2.高活性铂铜催化剂的制备方法,其特征在于,其步骤如下:分别称取硝酸铂230mg、64.5mg无水氯化铜,加入100 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散30min,备用;再分别称取碳黑1.0 g、水合肼50 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌10 h,再升温至90℃,反应1h,经过滤、洗涤、干燥后得到高活性铂铜催化剂,高活性铂铜催化剂是15%铂铜催化剂。
3.高活性铂铜催化剂的制备方法,其特征在于,其步骤如下:分别称取硝酸铂765 mg、215mg无水氯化铜,加入300 mL 蒸馏水溶解,将其置于超声剪切机中剪切分散50min,备用;再分别称取碳黑1.0 g、水合肼100 ml加入上述溶液中,混合均匀后,升温至70℃,低速搅拌15 h,再升温至95℃,反应2h,经过滤、洗涤、干燥后得到高活性铂铜催化剂,高活性铂铜催化剂是50%铂铜催化剂。
4.根据权利要求1所述的高活性铂铜催化剂的制备方法,其特征是所述的高活性铂铜催化剂中的Pt铜颗粒为4nm,以此催化剂制备的膜电极。
5.根据权利要求1或2或3所述的高活性铂铜催化剂的制备方法,其特征是所述的碳黑是碳黑XC-72。
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CN111505030A (zh) * | 2020-05-11 | 2020-08-07 | 北京工业大学 | 一种铂铜合金纳米催化剂形貌及三维结构的原位分析方法 |
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