CN111229239B - 一种氧化锌/锗酸锌-铜纳米复合材料光催化剂及其制备方法和应用 - Google Patents
一种氧化锌/锗酸锌-铜纳米复合材料光催化剂及其制备方法和应用 Download PDFInfo
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- 239000011701 zinc Substances 0.000 title claims abstract description 31
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 28
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010949 copper Substances 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 title claims abstract description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims description 52
- 239000011787 zinc oxide Substances 0.000 title claims description 27
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims description 25
- 229910052725 zinc Inorganic materials 0.000 title claims description 22
- 229910052802 copper Inorganic materials 0.000 title claims description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 230000001699 photocatalysis Effects 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 11
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 10
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004246 zinc acetate Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
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- 239000002904 solvent Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
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- 238000005303 weighing Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 2
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- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001431 copper ion Inorganic materials 0.000 abstract description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 abstract 1
- 229910005833 GeO4 Inorganic materials 0.000 description 8
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- 239000010953 base metal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 150000003751 zinc Chemical class 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/835—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B01J35/39—
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
本发明涉及一种纳米复合材料光催化剂的制备方法及其在催化分解水产氢方面的应用。该催化剂以一定浓度的氢氧化钠做溶剂,采用一步水热法通过调控乙酸锌和氧化锗的摩尔比得到不同比例的光催化剂,选取催化活性最好比例的光催化复合材料通过湿化学方法浸渍不同浓度的铜离子,最终得到ZnO/Zn2GeO4‑Cu纳米复合材料光催化剂。该方法简单、可控、反应条件温和,且获得的催化剂形貌好、成本低、光响应范围广。将所述催化剂进行光催化分解水产氢研究具有高效的催化活性,在光催化领域具有较高的应用前景。
Description
技术领域
本发明属于纳米复合材料制备技术及光催化领域,具体涉及一种氧化锌/锗酸锌-铜光催化产氢功能的光催化剂;还涉及所述催化剂的制备及在光催化制氢方面的应用。
背景技术
环境污染与能源短缺是当前制约人类社会发展的主要问题,开发新能源代替化石燃料的燃烧迫在眉睫。而氢气是最一种燃烧热值高、清洁环保的可再生能源,利用光催化技术分解制水氢已经受到了广泛的研究。而这项技术的关键就是开发研究新型、高效且价格低廉的光催化剂。
Zn2GeO4是一种重要的n型金属氧化物半导体光催化剂,晶体由GeO4四面体和ZnO4四面体组成,由于结构中存在严重扭曲的GeO4四面体,即Ge原子的中心偏离四周O原子的中心,此GeO4四面体偶极矩产生的电场有利于光生电子和空穴的分离,提高了其光催化性能。然而,较宽的带隙导致了Zn2GeO4只能吸收紫外光,光电子利用率低,为解决这一问题,通常利用离子掺杂,复合金属修饰等方法调控带隙值,拓宽光响应范围,降低电子和空穴的复合率,从而提高产氢活性。而ZnO具有氧化还原位高、激子结合能大,化学稳定性好等特点,是极具潜力的光催化材料,也是研究和应用较广的光催化材料之一。
为了制备兼具成本低,光吸收范围广且稳定高效的光催化剂,本发明首先以乙酸锌为锌盐,将不同比例的锌盐和氧化锗溶于配制好的氢氧化钠溶液,混匀溶解后转入反应釜中,通过一步水热法制得氧化锌/锗酸锌复合光催化剂,最后通过以乙酸铜为铜源,采用湿化学方法得到氧化锌/锗酸锌-铜锌基金属氧化物纳米光催化剂。目前采用此方法制备氧化锌/锗酸锌-铜锌基金属氧化物纳米光催化剂、以及该催化剂用于光催化分解水析氢的研究还未见报道。
本发明首先采用水热法,通过控制锌和锗的比例,在溶剂热条件下温和反应,从而得到氧化锌/锗酸锌催化剂,最后通过湿化学方法,引入铜原子从而得到氧化锌/锗酸锌-铜锌基金属氧化物光催化剂。该方法制备的所述光催化剂不仅拓宽了光吸收范围,而且有效抑制了光生电子和空穴的复合,在光催化过程中表现出显著提高的光催化分解水产氢活性。对解决能源危机的问题具有很重要的理论指导和实际意义。
发明内容
针对现有技术光催化分解水析氢性能不理想及本领域应用需要,本发明提供一种锌基金属氧化物纳米光催化剂的制备方法及其在光催化分解水制氢方面的应用。即该催化剂以一定浓度的氢氧化钠做溶剂,采用一步水热法通过调控乙酸锌和氧化锗的摩尔比得到不同比例的光催化复合材料,选取催化活性最好比例的光催化复合材料通过湿化学方法浸渍不同浓度的铜离子,最终得到所述ZnO/Zn2GeO4-Cu纳米复合材料光催化剂。
具体来说,本发明步骤如下:
1.氧化锌/锗酸锌纳米复合材料光催化剂的制备
(1) 称取1~6 mmol 乙酸锌分散到20 mL 0.5 M 氢氧化钠溶液中,磁力搅拌至充分溶解,得到无色透明溶液;
(2) 称取1~6 mmol 氧化锗分散溶液到(1)中,磁力搅拌至完全溶解后继续磁力搅拌1~60 min得乳白色溶液;
(3) 将(2)中搅拌好的溶液转入50 mL高压反应釜中100~200℃下反应10~12 h,产物用无水乙醇离心洗涤数次,50℃干燥8 h,得到白色粉末,备用;
2.氧化锌/锗酸锌-铜纳米复合材料光催化剂的制备
(1) 0~0.347 g 氧化锌/锗酸锌与0~0.009 g 乙酸铜分散到一定量无水乙醇中,超声1~10 min,然后室温搅拌1~12 h;
(2) 将上述混合溶液离心洗涤数次,50℃干燥6~8 h,将所得淡蓝色粉末收集备用。
具体实施方式:
为进一步理解本发明,下面以实施例对本发明作进一步说明,但并不以任何方式限制本发明。
实施例1
(a) 氧化锌/锗酸锌纳米复合材料光催化剂的制备
(1) 称取3 mmol 乙酸锌分散到20 mL 0.5 M 氢氧化钠溶液中,磁力搅拌至充分溶解,得到无色透明溶液;
(2) 称取1 mmol 氧化锗分散溶液到(1)中,磁力搅拌至完全溶解后继续磁力搅拌60 min得乳白色溶液;
(3) 将(2)中搅拌好的溶液转入50 mL高压反应釜中200℃下反应12 h,产物用无水乙醇离心洗涤数次,50℃干燥8 h,得到白色粉末,备用;
(b) 氧化锌/锗酸锌-铜纳米复合材料光催化剂的制备
(1) 0.347 g 氧化锌/锗酸锌与0.009 g 乙酸铜分散到一定量无水乙醇中,超声10 min然后室温搅拌12 h;
(2) 将上述混合溶液离心洗涤数次,50℃干燥8 h,得到淡蓝色粉末,备用;
实施例2
(a) ZnO/Zn2GeO4纳米复合材料光催化剂的制备
按照实施例1中步骤(a)的方法和条件制备;
(b) ZnO/Zn2GeO4-Cu纳米复合材料光催化剂的制备
按照实施例1中步骤(b)的方法和条件制备;
(c) 光催化分解水制氢
复合材料制氢性能测试用光催化活性评价***测试,具体实验步骤如下所述:
在石英反应器皿加入10%的甲醇水溶液100 mL,50 mg ZnO/Zn2GeO4复合材料并加入一定量氯亚铂酸钾(Pt含量为0.5%)作为助催化剂→反应器皿接入***继续抽真空至溶液没有气泡冒出关闭真空泵后开灯(灯源为300W氙灯)→反应产生的氢气接入气相色谱开始分析并记录峰面积(保留时间大约在1min左右)。根据峰面积和产氢时间计算氢气析出量和氢气析出速率。
在石英反应器皿加入10%的甲醇水溶液100 mL,50 mg ZnO/Zn2GeO4/Cu复合材料并加入一定量氯亚铂酸钾(Pt含量为0.5%)作为助催化剂→反应器皿接入***继续抽真空至溶液没有气泡冒出关闭真空泵后开灯(灯源为300W氙灯)→反应产生的氢气接入气相色谱开始分析并记录峰面积(保留时间大约在1min左右)。根据峰面积和产氢时间计算氢气析出量和氢气析出速率。
Claims (5)
1.一种氧化锌/锗酸锌-铜纳米复合材料光催化剂的制备方法,其特征在于该催化剂以一定浓度的氢氧化钠做溶剂,采用一步水热法通过调控乙酸锌和氧化锗的摩尔比得到不同比例的光催化剂,最后通过以乙酸铜为铜源,采用湿化学方法得到氧化锌/锗酸锌-铜纳米复合材料光催化剂;
所述的纳米复合材料光催化剂的制备方法,其特征在于:步骤如下:
(a) 氧化锌/锗酸锌纳米复合材料光催化剂的制备
(1) 称取1~6mmol 乙酸锌分散到20 mL 0.5M 氢氧化钠溶液中,磁力搅拌至充分溶解,得到无色透明溶液;
(2) 称取1~6mmol 氧化锗分散溶液到(1)中,磁力搅拌至完全溶解后继续磁力搅拌1~60 min得乳白色溶液;
(3) 将(2)中搅拌好的溶液转入50 mL高压反应釜中200℃下反应12 h,产物用无水乙醇离心洗涤数次,50℃干燥8 h,得到白色粉末,备用;
(b) 氧化锌/锗酸锌-铜纳米复合材料光催化剂的制备
(1) 0~0.347 g 氧化锌/锗酸锌与0~0.009 g 乙酸铜分散到一定量无水乙醇中,超声1~10 min,然后室温搅拌1~12 h;
(2) 将上述混合溶液离心洗涤数次,50℃干燥8 h,将所得淡蓝色粉末收集备用。
2.根据权利要求1所述的制备方法,其特征在于步骤(a)中Zn(ac)2·2H2O的用量为3mmol;GeO2为1 mmol。
3.根据权利要求1所述的制备方法,其特征在于步骤(b)中氧化锌/锗酸锌的量为0.347g;乙酸铜的量为0.009 g;超声分散时间为10 min;室温下搅拌时间为12 h;离心使用无水乙醇洗涤三次。
4.根据权利要求1所述的制备方法制得的纳米复合材料光催化剂在光催化分解水制氢领域的应用。
5.根据权利要求4所述的应用,其特征在于:测试条件光源为300 W氙灯;催化剂的量为0.05 g;牺牲剂甲醇的浓度为10%。
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