CN106179318B - 一种钒酸铋纳米线-石墨烯光催化剂的制备方法 - Google Patents
一种钒酸铋纳米线-石墨烯光催化剂的制备方法 Download PDFInfo
- Publication number
- CN106179318B CN106179318B CN201610852742.6A CN201610852742A CN106179318B CN 106179318 B CN106179318 B CN 106179318B CN 201610852742 A CN201610852742 A CN 201610852742A CN 106179318 B CN106179318 B CN 106179318B
- Authority
- CN
- China
- Prior art keywords
- graphene
- wire
- vanadic acid
- concentration
- acid bismuth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 30
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 30
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 title claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 13
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical class O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 239000004744 fabric Substances 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 8
- 206010013786 Dry skin Diseases 0.000 claims description 5
- 229920002873 Polyethylenimine Polymers 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- -1 oxygen Graphite alkene Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 25
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 150000001875 compounds Chemical class 0.000 abstract description 9
- 239000000758 substrate Substances 0.000 abstract description 8
- 150000001621 bismuth Chemical class 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000002070 nanowire Substances 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000012153 distilled water Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000006260 foam Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229920002401 polyacrylamide Polymers 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 229960003405 ciprofloxacin Drugs 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000000707 layer-by-layer assembly Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- XRRONFCBYFZWTM-UHFFFAOYSA-N octadecanoic acid;sodium Chemical compound [Na].CCCCCCCCCCCCCCCCCC(O)=O XRRONFCBYFZWTM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- 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
- B01J35/39—Photocatalytic properties
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
一种钒酸铋纳米线‑石墨烯复合光催化剂的制备方法,将铋盐、偏钒酸铵、二水合草酸按一定比例溶于蒸馏水中,超声混合,配成混合液,接着将氧化石墨烯加入到上述的混合液中,超声混合得到前驱体,最后将前驱体移入含有基底的高压反应釜中进行水热反应,反应结束后将负载有产物的基底洗净,干燥,即得所述的一种钒酸铋纳米线‑石墨烯复合光催化剂。本发明制备工艺简单,反应条件温和且反应时间短,制备出的钒酸铋纳米线与石墨烯能紧密接触和复合,有利于光生电子空穴的分离,从而提高光催化效率,提供了一种生产成本低且简单易行的高可见光活性光催化剂制备方法。
Description
技术领域
本发明涉及一种光催化剂的制备方法,特别涉及一种钒酸铋纳米线-石墨烯光催化剂的制备方法,属于光催化剂制备技术领域。
背景技术
近年来,随着全球不断加快发展的经济,工业废气、废水和废渣总量不断增长,生活废水的产生率也在不断增加,污水净化成为全球关注的焦点,传统的废水处理方法多采用物理吸附、化学气化法等,但这些方法工作效率太低,还要消耗大量能源,随着环境问题越来越严重,能源危机也日渐突出,利用免费太阳能进行光催化降解有机污染物和分解水产氧越来越受到人们的重视,利用光催化降解环境污染物具有在室温条件下反应、可直接利用太阳光作为光源来驱动氧化-还原反应等优点,是一种理想的环境污染治理技术。这个过程中必备的性能优良的光催化剂更是人们研究的热点。近些年来,钒酸铋BiVO4 作为一种具有可见光活性的新型光催化剂成为光催化的一个研究方向。钒酸铋是一种安全、环保的材料,没有毒性,具有独特的电磁性质、禁带宽度高、其带隙能为2.4eV、波长响应范围扩展到520nm左右、光催化活性高、对太阳光的利用率高,是最具有发展前景的光催化剂之一。但是单纯的钒酸铋作为光催化剂也面临着一些问题,例如:比表面积过小,吸附能力较差,而且光生载流子难以分离,电子空穴对容易复合等,这些缺陷都限制了钒酸铋的光催化性能。为了提高BiVO4 的催化效率,科学家做了一系列的努力。石墨烯是一种新型的二维碳材料,其带隙几乎为零,导电性高,比表面积极大等优点,其巨大的比表面积有效增加了催化材料对反应物的吸附量,并为催化反应提供反应位,而且氧化石墨烯上含氧基团中的羧基与传统半导体光催化剂的羟基形成键联,这使得在石墨烯上负载半导体光催化剂的可能性大大提高。石墨烯作为光催化剂的载体,利用其规整的二维平面结构可以提高催化剂的分散程度;借助石墨烯对载流子的较高迁移率及共轭π键分子的杂化作用,减少BiVO4中光生载流子的复合,进而提高BiVO4的光催化性能。如果将石墨烯与钡酸铋结合,利用石墨烯巨大的比表面积充份吸附溶液中的有机物,同时提供更多的反应活性位点,并且利用石墨烯优良的导电性能有效俘获光生电子,减小光生载流子的复合,可以使得光催化剂的量子效率得到提高,得到优良的光催化剂成品。目前已有许多研究致力于将钒酸铋与石墨烯复合来提高钒酸铋光催化效率。例如,Kudo等人 (Reducing Graphene Oxide on a Visible-Light BiVO4 Photocatalyst for an Enhanced Photoelectrochemical WaterSplitting,J. Phys. Chem. Lett.,2010,1,2607-2612)通过制备BiVO4/还原的氧化石墨烯(rGO)复合物(BiVO4/rGO),将BiVO4纳米颗粒均匀分散在rGO基体上,复合物中石墨烯和钒酸铋的紧密接触,有利于光生电子空穴的分离,从而提高了催化性能;Gong等人(ReducedGraphene Oxide (rGO)/BiVO4 Composites with Maximized Interfacial Coupling forVisible Lght Photocatalysis,ACS Sustainable Chem. Eng.,2014, 2, 2253−2258)通过界面相互作用制备了rGO/BiVO4复合光催化剂,这中方法制备出来的光催化剂的催化性能得到了很大的提高;Wang 等人(Electrostatic Self-Assembly of BiVO4−ReducedGraphene Oxide Nanocomposites for Highly Efficient Visible LightPhotocatalytic Activities,ACS Appl. Mater. Interfaces,2014, 6, 12698−12706)将用硅烷偶联剂改性后的纺锤状BiVO4与石墨烯通过静电作用复合在一起,改性后的BiVO4粒径更小,具有更高的比表面积,使BiVO4与石墨烯结合的更加紧密,提高了光响应范围和光生电子与空穴的分离效率,进而表现出极高的可见光光催性能。然而,这三种方法采用的都是水热法,他们的水热处理时间较长,温度较高。Yan 等人(Microwave-assisted in situsynthesis of reduced graphene oxide-BiVO4 composite photocatalysts and theirenhanced photocatalytic performance for the degradation of ciprofloxacin,Journal of Hazardous Materials 2013,250,106–114)采用微波辅助原位生长法制备了rGO/ BiVO4复合光催化剂,但微波法的微波发生器价格贵,而且现行的微波发生器的体积过小,限制了BiVO4产品的产量。中国专利公开号CN104383910A,公开日为2015年3月4日,发明名称为“一种颗粒大小可控的钒酸铋/石墨烯复合光催化剂的制法”,将石墨烯加入钒酸铋溶液中制得钒酸铋颗粒复合石墨烯复合物,虽然得到的光催化剂的催化性能良好,但需要经400~500℃的高温处理。
发明内容
针对现有技术中的以上问题,本发明旨在提供一种制备工艺简单,反应条件温和且反应时间短的钒酸铋纳米线的制备方法。
为实现以上目的,本发明采用的技术方案为:一种钒酸铋纳米线-石墨烯光催化剂的制备方法,制作步骤如下:
a :将铋盐、偏钒酸铵、二水合草酸、含氨基水溶性高分子共同溶于蒸馏水中,超声混合超声混合配成混合液;所述的铋盐为硝酸铋或碳酸铋或氯化铋或醋酸铋,所述的含氨基水溶性高分子为聚乙烯亚胺或聚丙烯酰胺或聚乙烯基吡咯烷酮;
b:将表面处理剂、氧化石墨烯加入到去离子水中,超声混合配成表面处理过的氧化石墨烯溶液;
c: 将步骤b中表面处理过的氧化石墨烯溶液加入到步骤a配制好的混合液中,超声混合得到前驱体溶液;
d:以碳布、棉布、钛片、不锈钢钢丝网或泡沫镍中的任意一种作为基底,将基底清洗后放入高压反应釜内衬中;
e :将经步骤c配制好的前驱体溶液转移至装有基底的高压反应釜内衬中后,在90~150℃反应40~120min,取出反应釜在室温自然冷却后,将反应后负载有钒酸铋纳米线-石墨烯复合光催化剂的基底取出,用去离子水冲洗,在烘箱中30~100℃干燥;
f :取将步骤e干燥后的负载有钒酸铋纳米线-石墨烯复合光催化剂的基底,在马弗炉中以0.5~2℃/min的升温速率,加热到200~300℃,保温2~5小时,即得钒酸铋纳米线-石墨烯复合光催化剂;
进一步的,所述偏钒酸铵的浓度为0.2~1mol/L, 偏钒酸铵和铋盐的浓度比为5:1~30:1,二水合草酸和铋盐的浓度比为10:1~60:1,含氨基水溶性高分子和铋盐的浓度比为1:1~6:1;
进一步的,所述步骤c中氧化石墨烯和铋盐的浓度比为5:1~20:1;
进一步的,所述的表面处理剂为十二烷基硫酸钠或十二烷基苯磺酸钠或硬脂酸钠。
本发明的积极有益技术效果在于:采用水热的方法,将氧化石墨烯与钒酸铋复合制成钒酸铋纳米线-石墨烯复合光催化剂,温度为90℃,40min就可以得到需要的产品,反应温度要求较低,时间较短,且制备出的产品长在棉布等成本较低的基底上,工艺简单,操作简便。其中石墨烯在室温下稳定存在,具有超凡的物理及电化学性质,比如高比表面积,高导电性,高机械强度,易于修饰,极易在其二维平面上修饰-COOH,-OH等含氧基团,因此非常适合用作纳米颗粒的载体材料,制备出的钒酸铋为纳米线,与石墨烯能紧密接触和复合,石墨烯作为优秀的电子接受体,可以提高光生电子和空穴的分离效率,提高材料的光催化性能。本发明制备工艺简单,反应条件温和且反应时间短,提供了一种生产成本低且简单易行的高可见光活性光催化剂制备方法。
附图说明
图1是本发明的催化剂的SEM图。
具体实施方式
为了更充分的解释本发明的实施,提供本发明的实施实例,这些实施实例仅仅是对本发明的阐述,不限制本发明的范围。
实施例1:
a :将硝酸铋、偏钒酸铵、二水合草酸、聚乙烯亚胺加入到去离子水中,超声混合配成混合液,其中偏钒酸铵的浓度为0.2mol/L,硝酸铋的浓度为0.04mol/L,二水合草酸的浓度为0.4mol/L,聚乙烯亚胺的浓度为0.04mol/L;
b:将十二烷基硫酸钠、氧化石墨烯加入到去离子水中,超声混合配成表面处理过的氧化石墨烯溶液;
c :将步骤b中表面处理过的氧化石墨烯溶液加入到步骤a配制好的混合液中,超声混合得到前驱体溶液,其中氧化石墨烯的浓度为0.2mol/L;
d:清洗碳布,将清洗后的碳布放入高压反应釜内衬中;
e :将经步骤c配制好的前驱体溶液转移至装有碳布的高压反应釜内衬中后,在90℃反应40min,取出反应釜在室温自然冷却后,将反应后负载有钒酸铋纳米线-石墨烯复合光催化剂的碳布取出,用去离子水冲洗,在烘箱中30℃干燥;
f :取经步骤e干燥后的负载有钒酸铋纳米线-石墨烯复合光催化剂的碳布,在马弗炉中以0.5℃/min的升温速率,加热到200℃,保温2h,即得钒酸铋纳米线-石墨烯复合光催化剂。
催化剂效果验证:向100 mL 20 mg/L的甲基橙溶液中加入钒酸铋纳米线-石墨烯复合光催化剂0.1g,在模拟太阳光下照射30min,甲基橙溶液完全被降解,溶液变为无色。
实施例2:
a: 将碳酸铋、偏钒酸铵、二水合草酸、聚丙烯酰胺加入到去离子水中,超声混合配成混合液,其中偏钒酸铵的浓度为1mol/L, 碳酸铋的浓度为0.03mol/L,二水合草酸的浓度为1.8mol/L,聚丙烯酰胺的浓度为0.18mol/L;
b:将十二烷基苯磺酸钠、氧化石墨烯加入到去离子水中,超声混合配成表面处理过的氧化石墨烯溶液;
c :将步骤b中表面处理过的氧化石墨烯溶液加入到a步骤配制好的混合液中,超声混合得到前驱体溶液,其中氧化石墨烯的浓度为0.8mol/L;
d:清洗不锈钢钢丝网,将清洗后的不锈钢钢丝网放入高压反应釜内衬中;
e :将经步骤c配制好的前驱体溶液转移至装有不锈钢钢丝网的高压反应釜内衬中后,在150℃反应120min,取出反应釜在室温自然冷却后,将反应后负载有钒酸铋纳米线-石墨烯复合光催化剂的不锈钢钢丝网取出,用去离子水冲洗,在烘箱中100℃干燥;
f :取经步骤e干燥后的负载有钒酸铋纳米线-石墨烯复合光催化剂的不锈钢钢丝网,在马弗炉中以2℃/min的升温速率,加热到300℃,保温5h,即得钒酸铋纳米线-石墨烯复合光催化剂。
催化剂效果验证:向100 mL 20 mg/L的甲基橙溶液中加入钒酸铋纳米线-石墨烯复合光催化剂0.1g,在模拟太阳光下照射30min,甲基橙溶液完全被降解,溶液变为无色。
实施例3:
a: 将醋酸铋、偏钒酸铵、二水合草酸、聚乙烯基吡咯烷酮加入到去离子水中,超声混合配成混合液,其中偏钒酸铵的浓度为0.5mol/L, 醋酸铋的浓度为0.05mol/L,二水合草酸的浓度为0.15mol/L,聚乙烯基吡咯烷酮的浓度为0.15mol/L;
b: 将硬脂酸钠、氧化石墨烯加入到去离子水中,超声混合配成表面处理过的氧化石墨烯溶液;
c :将步骤b中表面处理过的氧化石墨烯溶液加入到a步骤配制好的混合液中,超声混合得到前驱体溶液,其中氧化石墨烯的浓度为0.4mol/L;
d:清洗泡沫镍,将清洗后的泡沫镍放入高压反应釜内衬中;
e: 将经b步骤配制好的前驱体溶液转移至装有泡沫镍的高压反应釜内衬中后,在120℃反应60min,取出反应釜在室温自然冷却后,将反应后负载有钒酸铋纳米线-石墨烯复合光催化剂的泡沫镍取出,用去离子水冲洗,在烘箱中60℃干燥;
f: 取经步骤e干燥后的负载有钒酸铋纳米线-石墨烯复合光催化剂的泡沫镍,在马弗炉中以1℃/min的升温速率,加热到250℃,保温3h,即得钒酸铋纳米线-石墨烯复合光催化剂。
催化剂效果验证:向100 mL 20 mg/L的甲基橙溶液中加入钒酸铋纳米线-石墨烯复合光催化剂0.1g,在模拟太阳光下照射30min,甲基橙溶液完全被降解,溶液变为无色。
图1是本发明的催化剂的SEM图,从图中可以看出:纳米结构具有大的比表面积,具有更高的光催化活性点位,提高单位质量的催化活性。
在详细说明本发明的实施方式之后,熟悉该项技术的人士可清楚地了解,在不脱离上述申请专利范围与精神下可进行各种变化与修改,凡依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均属于本发明技术方案的范围,且本发明亦不受限于说明书中所举实例的实施方式。
Claims (1)
1.一种钒酸铋纳米线-石墨烯光催化剂的制备方法,其特征在于制作步骤如下:
a :将硝酸铋、偏钒酸铵、二水合草酸、聚乙烯亚胺加入到去离子水中,超声混合配成混合液,其中偏钒酸铵的浓度为0.2mol/L,硝酸铋的浓度为0.04mol/L,二水合草酸的浓度为0.4mol/L,聚乙烯亚胺的浓度为0.04mol/L;
b:将十二烷基硫酸钠、氧化石墨烯加入到去离子水中,超声混合配成表面处理过的氧化石墨烯溶液;
c :将步骤b中表面处理过的氧化石墨烯溶液加入到步骤a配制好的混合液中,超声混合得到前驱体溶液,其中氧化石墨烯的浓度为0.2mol/L;
d:清洗碳布,将清洗后的碳布放入高压反应釜内衬中;
e :将经步骤c配制好的前驱体溶液转移至装有碳布的高压反应釜内衬中后,在90℃反应40min,取出反应釜在室温自然冷却后,将反应后负载有钒酸铋纳米线-石墨烯复合光催化剂的碳布取出,用去离子水冲洗,在烘箱中30℃干燥;
f :取经步骤e干燥后的负载有钒酸铋纳米线-石墨烯复合光催化剂的碳布,在马弗炉中以0.5℃/min的升温速率,加热到200℃,保温2h,即得钒酸铋纳米线-石墨烯复合光催化剂。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610852742.6A CN106179318B (zh) | 2016-09-27 | 2016-09-27 | 一种钒酸铋纳米线-石墨烯光催化剂的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610852742.6A CN106179318B (zh) | 2016-09-27 | 2016-09-27 | 一种钒酸铋纳米线-石墨烯光催化剂的制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106179318A CN106179318A (zh) | 2016-12-07 |
CN106179318B true CN106179318B (zh) | 2019-03-08 |
Family
ID=57521098
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610852742.6A Expired - Fee Related CN106179318B (zh) | 2016-09-27 | 2016-09-27 | 一种钒酸铋纳米线-石墨烯光催化剂的制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106179318B (zh) |
Families Citing this family (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106964389B (zh) * | 2017-04-06 | 2018-04-13 | 上海理工大学 | 钒酸铋与氮掺杂石墨烯量子点复合型可见光催化剂的制备方法 |
CN107262104A (zh) * | 2017-07-27 | 2017-10-20 | 哈尔滨工业大学 | 一种微波快速合成铅、氧化石墨掺杂铁酸铋与泡沫镍复合材料的方法及应用 |
CN108479749A (zh) * | 2018-01-30 | 2018-09-04 | 昆明理工大学 | 一种金属离子掺杂钒酸盐纳米催化剂的合成方法 |
CN109092343B (zh) * | 2018-09-06 | 2023-02-07 | 滨州学院 | 一种可见光响应型g-C3N4/BiVO4异质结材料的制备方法及其应用 |
CN110639556A (zh) * | 2019-10-17 | 2020-01-03 | 扬州大学 | 一种复合光催化剂及其制备工艺 |
CN110801826A (zh) * | 2019-11-12 | 2020-02-18 | 广东工业大学 | 一种光电催化石墨毡材料及其制备方法和应用 |
CN112452348A (zh) * | 2020-11-03 | 2021-03-09 | 扬州大学 | 一种钒酸铋掺杂石墨相氮化碳纳米片光催化剂的制备方法 |
CN112973756A (zh) * | 2021-03-08 | 2021-06-18 | 合肥工业大学 | 一种棒状钒酸铋/rgo/石墨相氮化碳光催化材料及其制备方法 |
CN113877631B (zh) * | 2021-11-16 | 2023-08-11 | 江西省科学院应用化学研究所 | 一种高效降解重金属离子的石墨烯量子点负载钒酸铋纳米复合材料制备方法 |
CN115254192B (zh) * | 2022-08-08 | 2023-10-17 | 宁波(北仑)中科海西产业技术创新中心 | 一种石墨烯/UiO-66-NH2改性的Z-型钒酸铋可见光光催化剂及制备方法与应用 |
CN115709059B (zh) * | 2022-12-26 | 2024-03-08 | 开封大学 | 一种桑葚状钒酸铋-碳纳米管复合光催化剂及其制备方法和应用 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102513091A (zh) * | 2011-12-09 | 2012-06-27 | 东华大学 | 一种石墨烯自组装纳米钒酸铋光催化剂的制备方法 |
CN104383910A (zh) * | 2014-11-05 | 2015-03-04 | 上海交通大学 | 一种颗粒大小可控的钒酸铋/石墨烯复合光催化剂的制法 |
-
2016
- 2016-09-27 CN CN201610852742.6A patent/CN106179318B/zh not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102513091A (zh) * | 2011-12-09 | 2012-06-27 | 东华大学 | 一种石墨烯自组装纳米钒酸铋光催化剂的制备方法 |
CN104383910A (zh) * | 2014-11-05 | 2015-03-04 | 上海交通大学 | 一种颗粒大小可控的钒酸铋/石墨烯复合光催化剂的制法 |
Non-Patent Citations (1)
Title |
---|
钒酸铋/石墨烯复合光催化剂的制备及性能研究;覃涛;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20150215(第2期);第27页最后一段,第28页第一段,第30页,图3-8,第31页,第1段,第37页,引言第二段,第38-39页,图4-1 |
Also Published As
Publication number | Publication date |
---|---|
CN106179318A (zh) | 2016-12-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106179318B (zh) | 一种钒酸铋纳米线-石墨烯光催化剂的制备方法 | |
Li et al. | Recent advances in 3D g-C3N4 composite photocatalysts for photocatalytic water splitting, degradation of pollutants and CO2 reduction | |
Chen et al. | Bi‐based photocatalysts for light‐driven environmental and energy applications: Structural tuning, reaction mechanisms, and challenges | |
Chen et al. | Sulfur and potassium co-doped graphitic carbon nitride for highly enhanced photocatalytic hydrogen evolution | |
Yang et al. | BiOX (X= Cl, Br, I) photocatalytic nanomaterials: applications for fuels and environmental management | |
Fang et al. | Facile synthesis of anatase/rutile TiO2/g-C3N4 multi-heterostructure for efficient photocatalytic overall water splitting | |
Su et al. | Recent advances in the photocatalytic reduction of carbon dioxide | |
CN103990485B (zh) | 氮化碳纳米粒子修饰钒酸铋复合光催化剂及其制备方法 | |
Yin et al. | Bi2MoO6/TiO2 heterojunction modified with Ag quantum dots: a novel photocatalyst for the efficient degradation of tetracycline hydrochloride | |
CN102671683B (zh) | 一种纳米片自组装C掺杂(BiO)2CO3微球可见光催化剂的制备方法 | |
Vinesh et al. | rGO supported self-assembly of 2D nano sheet of (g-C3N4) into rod-like nano structure and its application in sonophotocatalytic degradation of an antibiotic | |
Zhao et al. | Salt templated synthesis of NiO/TiO2 supported carbon nanosheets for photocatalytic hydrogen production | |
CN110252346B (zh) | 一种MoS2/SnS2/r-GO复合光催化剂的制备方法与用途 | |
Luo et al. | Facile synthesis of PVDF photocatalytic membrane based on NCQDs/BiOBr/TiO2 heterojunction for effective removal of tetracycline | |
CN105645459B (zh) | 一种表面修饰海胆状ZnO/TiO2复合材料及其制备方法 | |
Liu et al. | Vacancy-engineered bismuth-based semiconductor with enhanced photocatalytic activity: A review | |
CN106268902B (zh) | 一种g-C3N4量子点、Ag量子点敏化BiVO4光催化剂的制备方法 | |
CN108043436A (zh) | 碳化钼/硫铟锌复合光催化剂的制备方法及其应用 | |
CN109876810A (zh) | 一种磁性微藻基生物炭的制备方法及其应用 | |
CN106622293A (zh) | 一种H‑TiO2/CdS/Cu2‑xS纳米带的制备方法 | |
CN110624564A (zh) | In2O3@ZnIn2S4纳米片材料、制备方法及其应用 | |
CN106622202A (zh) | 石墨烯‑TiO2纳米管/FTO双层复合膜的制备方法 | |
CN112619647A (zh) | Co-MOF衍生的四氧化三钴复合二氧化钛异质结的制备方法及电解水应用 | |
Liu et al. | Greatly improved photocatalytic performance of BiVO4/MoS2 heterojunction with enhanced hole transfer and attack capability by ultrasonic agitation and in-situ hydrothermal method | |
CN106914268A (zh) | 一种石墨烯复合纳米材料及其制备方法和应用 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190308 Termination date: 20200927 |