CN112642426B - 一种贵金属/石墨烯担载锰锌基弱光光触媒的制备方法 - Google Patents
一种贵金属/石墨烯担载锰锌基弱光光触媒的制备方法 Download PDFInfo
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- CN112642426B CN112642426B CN202011537395.0A CN202011537395A CN112642426B CN 112642426 B CN112642426 B CN 112642426B CN 202011537395 A CN202011537395 A CN 202011537395A CN 112642426 B CN112642426 B CN 112642426B
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- noble metal
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- zinc
- graphene
- manganese
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 65
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 53
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 title abstract description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000008139 complexing agent Substances 0.000 claims abstract description 29
- 239000011572 manganese Substances 0.000 claims abstract description 29
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 23
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- -1 Pt or Pd in water Chemical class 0.000 claims abstract description 19
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- 239000002002 slurry Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000011701 zinc Substances 0.000 claims abstract description 13
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000001408 amides Chemical class 0.000 claims abstract description 11
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 11
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 239000013008 thixotropic agent Substances 0.000 claims abstract description 9
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 7
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- 229910052697 platinum Inorganic materials 0.000 claims abstract description 6
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- 239000002243 precursor Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 8
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- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
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- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
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- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229960000892 attapulgite Drugs 0.000 claims description 2
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- 229920002678 cellulose Polymers 0.000 claims description 2
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- 229920002647 polyamide Polymers 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 241000894006 Bacteria Species 0.000 abstract description 7
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- 241000700605 Viruses Species 0.000 abstract description 5
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- 229910052763 palladium Inorganic materials 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 229910007612 Zn—La Inorganic materials 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 5
- 229910003120 Zn-Ce Inorganic materials 0.000 description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 4
- 229940071125 manganese acetate Drugs 0.000 description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 4
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052706 scandium Inorganic materials 0.000 description 4
- 239000004246 zinc acetate Substances 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- VZMHYPSCFWNPBO-UHFFFAOYSA-N [Zn].[Mn].[Ce] Chemical compound [Zn].[Mn].[Ce] VZMHYPSCFWNPBO-UHFFFAOYSA-N 0.000 description 3
- 238000010494 dissociation reaction Methods 0.000 description 3
- 230000005593 dissociations Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 3
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 229910052772 Samarium Inorganic materials 0.000 description 2
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
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- 238000005457 optimization Methods 0.000 description 2
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- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 description 2
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- 239000011149 active material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
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- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
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- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/656—Manganese, technetium or rhenium
- B01J23/6562—Manganese
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- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Environmental & Geological Engineering (AREA)
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- Biomedical Technology (AREA)
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Abstract
本发明提供了一种贵金属/石墨烯担载锰锌基弱光光触媒的制备方法,首先将Pt或Pd等贵金属氯化物溶于水中,然后加入足量的石墨烯微片粉末,酰胺类非离子表面活性剂,乳化,制备石墨烯表面均匀分布有贵金属氯化物的复合微片浆料;其次,将锰、锌和稀土化合物溶于水中,加入络合剂,搅拌,添加氨水调节pH值,超声震荡,加热,待凝胶态后马弗炉焙烧,制成弱光光触媒催化材料;最后,将弱光光触媒加入到复合微片浆料中,搅拌,高压均质处理,加入触变剂调节粘度,冷冻干燥,280℃处理,得到贵金属/石墨烯微包覆锰锌‑稀土基弱光光触媒粉末材料。该材料在弱光作用下可产生羟基自由基,可以无选择性地降解室内的污染物,杀死细菌、霉菌和病毒。
Description
技术领域
本发明属于光触媒催化剂制备技术领域,具体涉及一种贵金属/石墨烯担载锰锌基弱光光触媒的制备方法。
背景技术
光触媒也叫光催化剂,是一种以纳米级具有光催化功能的半导体材料的总称它能在光照射下产生强氧化性的物质(如羟基自由基、氧气等),并且可用于分解有机化合物、部分无机化合物、细菌及病毒等。日常生活中,光触媒能有效地降解空气中有毒有害气体如甲醛等,高效净化空气;同时,能够有效杀灭多种细菌,并能将细菌或真菌释放出的毒素分解及无害化处理,是未来清洁能源生产和环境污染治理的理想材料之一。
以TiO2和ZnO为代表的传统光催化剂,由于较窄的光响应范围和较低的光生电子-空穴对分离效率,限制了其实际应用。因此,对传统紫外光响应半导体材料和新型可见光响应半导体材料进行微结构的调控和优化,构筑制备过程相对简便、成本较低和光催化活性较好的复合光催化材料,以及研究其构效关系仍然是光催化领域的一个重要课题。
在材料学领域:石墨烯高的导电性可以加快光诱导电子传输,促进电子-空穴活性位点的表面吸附解离效率;锰-稀土掺杂的氧化锌纳米棒作为活性材料能够最大限度地发挥尺寸和界面优化性能。引入的贵金属与石墨烯层的协同作用,有效地扩展了体系的光吸收范围,增强了光吸收强度以及促进了光生电子-空穴的分离,协同增强了可见光捕获能力以及提高了光生电子-空穴对的分离率,同时石墨烯材料的复合也减少了贵金属的使用量。
因此,本发明制备的这种贵金属/石墨烯担载锰锌基弱光光触媒复合材料具有增强光电流产生的作用而且对光催化活性也有显著的改善,即在可见光下可以被激发,其加强的导电性加速了电子的转移,并提供更多的反应活性位,增强了污染物气体、细菌或病毒在光触媒表面的吸附和解离效率,三者的协同效应使得该复合材料成为一种在弱光条件下活性很高的的光催化材料,具有广阔的应用前景。
发明内容
本发明提供一种贵金属/石墨烯担载锰锌基弱光光触媒的制备方法,其具体步骤如下:
(1)将Pt或Pd等贵金属氯化物溶于水中,然后加入足量的石墨烯微片粉末,酰胺类非离子表面活性剂,乳化,制备石墨烯表面均匀分布有贵金属氯化物的复合微片浆料;
(2)将锰、锌和稀土的硝酸盐或醋酸盐溶于水中,加入络合剂,搅拌,添加氨水调节pH值,超声震荡,加热,使锰、锌和稀土等金属离子可以与络合剂完全络合,形成透明的溶胶;
(3)待步骤(2)中的溶胶在加热条件下形成粘稠凝胶态后,再放入烘箱预烘烤,碳化,制成锰锌-稀土基弱光光触媒前驱体;
(4)将步骤(3)制得的锰锌-稀土基弱光光触媒前驱体放入马弗炉中低温焙烧,制成锰锌-稀土基弱光光触媒催化材料;
(5)将步骤(4)制得的锰锌-稀土基弱光光触媒催化材料加入到复合微片浆料中,剪切,搅拌,高压均质处理,加入触变剂调节粘度,得到软团聚已经打开并表面微包覆有贵金属氯化物/石墨烯的锰锌-稀土基弱光光触媒混合液;
(6)将步骤(5)制得的贵金属氯化物/石墨烯的锰锌-稀土基弱光光触媒混合液进行冷冻干燥,在干燥出箱前再280℃热处理,得到贵金属/石墨烯微包覆锰锌-稀土基弱光光触媒粉末材料。
优选的,所述步骤(1)中酰胺类非离子表面活性剂为烷基葡萄糖酰胺类、烷醇酰胺类、聚氧乙烯酰胺类、三聚酰胺类中的一种或其组合;所述贵金属为Pt、Pd、Ru、Rh中的一种或其组合;所述贵金属氯化物、石墨烯微片、酰胺类非离子表面活性剂、去离子水的质量比为(1~3):15:10:1000。
优选的,所述步骤(2)中稀土元素为Ce、Sc、Y、La、Pr、Nd、Sm、Gd中的一种或其组合;所述络合剂为EDTA、CA、乙醇胺络合剂、氨基羧酸络合剂、羟氨基羧酸络合剂、甲叉膦酸酯络合剂中的一种或其组合;所述锰、锌、稀土和络合剂的摩尔比为(4~30):(60~95):(1~10):100。
优选的,所述步骤(2)中氨水调节pH值的范围为7.5~10;所述超声震荡频率为10~60HZ,时间为10~90min;所述加热温度为70~90℃,加热时间为2~8小时。
优选的,所述步骤(3)中烘箱预烘烤温度为200~300℃,时间为2~6小时。
优选的,所述步骤(4)中马弗炉焙烧温度为400~600℃,焙烧时间为4~10小时。
优选的,所述步骤(5)中锰锌-稀土基弱光光触媒催化材料和复合微片浆料的质量比为1:(2~5);所述触变剂为羟乙基纤维素等纤维素衍生物、聚乙烯醇、聚丙烯酸盐、凹凸棒土、膨润土、气相二氧化硅、聚酰胺中的一种或其组合,添加比例为0.1~2.0%。
优选的,所述步骤(6)中冷冻干燥温度为-80℃,干燥时间为24~72小时。
与现有技术相比,本发明所述的方法制备贵金属/石墨烯微包覆锰锌-稀土基弱光光触媒具有如下的有益效果:
(1)贵金属,石墨烯微包覆锰锌,稀土三者的协同效应使得该复合材料成为一种在弱光条件下活性很高的的光催化材料,在可见光下可以被激发,其加强的导电性加速了电子的转移,并提供更多的反应活性位。可极大增强污染物气体、细菌或病毒在光触媒表面的吸附和解离效率。
(2)该材料在弱光作用下可产生羟基自由基,可以无选择性地降解室内的污染物,杀死细菌、霉菌和病毒。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述,本发明的其它特征、目的和优点将会变得更明显:
图1为本发明实施例一中间产物氯化铂/石墨烯的SEM图
图2为本发明实施例二产物锰锌-稀土基弱光光触媒的晶体结构示意图
图3为本发明实施例三产物钌/石墨烯微包覆Zn0.85Mn0.1Sm0.05O1-δ弱光光触媒的SEM图
图4为本发明实施例四产物铑/石墨烯微包覆Zn0.95Mn0.04Sc0.01O1-δ弱光光触媒的TEM图
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例一:
制备贵金属氯化铂的复合微片浆料:将1g氯化铂溶于1kg去离子水中,然后加15g石墨烯微片粉末,10g烷基葡萄糖酰胺类非离子表面活性剂,乳化2小时即可。
制成锰锌-镧基弱光光触媒催化材料:将硝酸锌、硝酸锰和硝酸镧溶于1kg水中,加入EDTA络合剂,硝酸锌、硝酸锰、硝酸镧和络合剂的摩尔比为60:30:10:100,搅拌,加氨水调节pH值到7.5,10HZ超声震荡10min,70℃加热2小时,使锌、锰和镧金属离子可以与络合剂完全络合,形成透明的溶胶;继续加热条件下形成粘稠凝胶态后,再放入烘箱200℃预烘烤2小时,碳化,制成锰锌-稀土基弱光光触媒前驱体,放入马弗炉中400℃焙烧4小时,制成锰锌-镧基弱光光触媒催化材料。
制备贵金属铂/石墨烯微包覆锰锌-稀土基弱光光触媒粉末:将100g制得的锰锌-镧基弱光光触媒催化材料加入到200g复合微片浆料中,剪切,搅拌,高压均质处理,加入0.3g羟乙基纤维素触变剂调节粘度,得到软团聚已经打开并表面微包覆有贵金属氯化镧/石墨烯的锰锌-镧基弱光光触媒混合液,然后-80℃下冷冻干燥24小时,在干燥出箱前再280℃热处理,得到贵金属铂/石墨烯微包覆锰锌-镧基弱光光触媒粉末材料。
实施例二:
制备贵金属氯化钯的复合微片浆料:将1.5g氯化钯溶于1kg去离子水中,然后加15g石墨烯微片粉末,10g烷醇酰胺类非离子表面活性剂,乳化2小时即可。
制成锰锌-铈基弱光光触媒催化材料:将醋酸锌、醋酸锰和醋酸铈溶于1kg水中,加入乙醇胺络合剂,醋酸锌、醋酸锰、醋酸铈和络合剂的摩尔比为75:20:5:100,搅拌,加氨水调节pH值到8,25HZ超声震荡30min,75℃加热4小时,使锌、锰和铈金属离子可以与络合剂完全络合,形成透明的溶胶;继续加热条件下形成粘稠凝胶态后,再放入烘箱240℃预烘烤4小时,碳化,制成锰锌-铈基弱光光触媒前驱体,放入马弗炉中500℃焙烧6小时,制成锰锌-铈基弱光光触媒催化材料。
制备贵金属钯/石墨烯微包覆锰锌-铈基弱光光触媒粉末:将100g制得的锰锌-铈基弱光光触媒催化材料加入到300g复合微片浆料中,剪切,搅拌,高压均质处理,加入1.2g聚乙烯醇触变剂调节粘度,得到软团聚已经打开并表面微包覆有贵金属氯化钯/石墨烯的锰锌-铈基弱光光触媒混合液,然后-80℃下冷冻干燥36小时,在干燥出箱前再280℃热处理,得到贵金属钯/石墨烯微包覆锰锌-铈基弱光光触媒粉末材料。
实施例三:
制备贵金属氯化钌的复合微片浆料:将2g氯化钌溶于1kg去离子水中,然后加15g石墨烯微片粉末,10g聚氧乙烯酰胺类非离子表面活性剂,乳化2小时即可。
制成锰锌-钐基弱光光触媒催化材料:将硝酸锌、硝酸锰和硝酸钐溶于1kg水中,加入氨基羧酸络合剂,硝酸锌、硝酸锰、硝酸钐和络合剂的摩尔比为85:10:5:100,搅拌,加氨水调节pH值到9,45HZ超声震荡60min,80℃加热6小时,使锌、锰和钐金属离子可以与络合剂完全络合,形成透明的溶胶;继续加热条件下形成粘稠凝胶态后,再放入烘箱280℃预烘烤6小时,碳化,制成锰锌-钐基弱光光触媒前驱体,放入马弗炉中500℃焙烧6小时,制成锰锌-钐基弱光光触媒催化材料。
制备贵金属钌/石墨烯微包覆锰锌-钐基弱光光触媒粉末:将100g制得的锰锌-钐基弱光光触媒催化材料加入到400g复合微片浆料中,剪切,搅拌,高压均质处理,加入3g聚丙烯酸盐触变剂调节粘度,得到软团聚已经打开并表面微包覆有贵金属氯化钌/石墨烯的锰锌-钐基弱光光触媒混合液,然后-80℃下冷冻干燥48小时,在干燥出箱前再280℃热处理,得到贵金属钌/石墨烯微包覆锰锌-钐基弱光光触媒粉末材料。
实施例四:
制备贵金属氯化铑的复合微片浆料:将3g氯化铑溶于1kg去离子水中,然后加15g石墨烯微片粉末,10g三聚酰胺类非离子表面活性剂,乳化2小时即可。
制成锰锌-钪基弱光光触媒催化材料:将醋酸锌、醋酸锰和醋酸钪溶于1kg水中,加入羟氨基羧酸络合剂,醋酸锌、醋酸锰、醋酸钪和络合剂的摩尔比为95:4:1:100,搅拌,加氨水调节pH值到10,60HZ超声震荡90min,90℃加热8小时,使锌、锰和钪金属离子可以与络合剂完全络合,形成透明的溶胶;继续加热条件下形成粘稠凝胶态后,再放入烘箱300℃预烘烤6小时,碳化,制成锰锌-钪基弱光光触媒前驱体,放入马弗炉中600℃焙烧10小时,制成锰锌-钪基弱光光触媒催化材料。
制备贵金属铑/石墨烯微包覆锰锌-钪基弱光光触媒粉末:将100g制得的锰锌-钪基弱光光触媒催化材料加入到500g复合微片浆料中,剪切,搅拌,高压均质处理,加入6g膨润土触变剂调节粘度,得到软团聚已经打开并表面微包覆有贵金属氯化铑/石墨烯的锰锌-钪基弱光光触媒混合液,然后-80℃下冷冻干燥72小时,在干燥出箱前再280℃热处理,得到贵金属铑/石墨烯微包覆锰锌-钪基弱光光触媒粉末材料。
表1实施例一、二、三、四的产物跟纯氧化锌60分钟日光灯照射下光催化降解甲醛效率对比
样品编号 | 甲醛去除率% |
纯氧化锌 | 63.6 |
实施例一粉体 | 98.7 |
实施例二粉体 | 99.3 |
实施例三粉体 | 95.4 |
实施例四粉体 | 92.8 |
Claims (8)
1.一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于具体步骤如下:
(1)将Pt、Pd、Ru、Rh中的一种或其组合贵金属氯化物溶于水中,然后加入足量的石墨烯微片粉末,酰胺类非离子表面活性剂,乳化,制备石墨烯表面均匀分布有贵金属氯化物的复合微片浆料;
(2)将锰、锌和稀土的硝酸盐或醋酸盐溶于水中,加入络合剂,搅拌,添加氨水调节pH值,超声震荡,加热,使锰、锌和稀土Ce、Sc、Y、La、Pr、Nd、Sm、Gd中的一种或其组合金属离子与络合剂完全络合,形成透明的溶胶;
(3)待步骤(2)中的溶胶在加热条件下形成粘稠凝胶态后,再放入烘箱预烘烤,碳化,制成锰锌-稀土基弱光光触媒前驱体;
(4)将步骤(3)制得的锰锌-稀土基弱光光触媒前驱体放入马弗炉中低温焙烧,制成锰锌-稀土基弱光光触媒催化材料;
(5)将步骤(4)制得的锰锌-稀土基弱光光触媒催化材料加入到复合微片浆料中,剪切,搅拌,高压均质处理,加入触变剂调节粘度,得到软团聚已经打开并表面微包覆有贵金属氯化物@石墨烯的锰锌-稀土基弱光光触媒混合液;
(6)将步骤(5)制得的贵金属氯化物@石墨烯的锰锌-稀土基弱光光触媒混合液进行冷冻干燥,在干燥出箱前再280℃热处理,得到贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒粉末材料。
2.根据权利要求1所述一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于,所述步骤(1)中酰胺类非离子表面活性剂为烷基葡萄糖酰胺类、烷醇酰胺类、聚氧乙烯酰胺类、三聚酰胺类中的一种或其组合;所述贵金属氯化物、石墨烯微片、酰胺类非离子表面活性剂、去离子水的质量比为(1~3):15:10:1000。
3.根据权利要求1所述一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于,所述步骤(2)中络合剂为EDTA、CA、乙醇胺络合剂、氨基羧酸络合剂、羟氨基羧酸络合剂、甲叉膦酸酯络合剂中的一种或其组合;所述锰、锌、稀土和络合剂的摩尔比为(4~30):(60~95):(1~10):100。
4.根据权利要求1所述一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于,所述步骤(2)中氨水调节pH值的范围为7.5~10;所述超声震荡频率为10~60HZ,时间为10~90min;所述加热温度为70~90℃,加热时间为2~8小时。
5.根据权利要求1所述一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于,所述步骤(3)中烘箱预烘烤温度为200~300℃,时间为2~6小时。
6.根据权利要求1所述一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于,所述步骤(4)中马弗炉焙烧温度为400~600℃,焙烧时间为4~10小时。
7.根据权利要求1所述一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于,所述步骤(5)中锰锌-稀土基弱光光触媒催化材料和复合微片浆料的质量比为1:(2~5);所述触变剂为羟乙基纤维素等纤维素衍生物、聚乙烯醇、聚丙烯酸盐、凹凸棒土、膨润土、气相二氧化硅、聚酰胺中的一种或其组合,添加比例为0.1~2.0%。
8.根据权利要求1所述一种贵金属@石墨烯微包覆锰锌-稀土基弱光光触媒的制备方法,其特征在于,所述步骤(6)中冷冻干燥温度为-80℃,干燥时间为24~72小时。
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