CN109317184A - 双功能β-FeOOH/eg-C3N4复合纳米材料及其制备方法和应用 - Google Patents
双功能β-FeOOH/eg-C3N4复合纳米材料及其制备方法和应用 Download PDFInfo
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- 229910003153 β-FeOOH Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 17
- 238000002604 ultrasonography Methods 0.000 claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 7
- 238000006731 degradation reaction Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 6
- 229910002588 FeOOH Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 230000005622 photoelectricity Effects 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229940075397 calomel Drugs 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L sodium sulphate Substances [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- -1 potassium ferricyanide Chemical compound 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B01J27/24—Nitrogen compounds
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Abstract
本发明涉及一种双功能β‑FeOOH/eg‑C3N4复合纳米材料的制备方法,以水为溶剂,加入适量eg‑C3N4,调节溶液pH,再加入适量铁盐,超声,洗涤,干燥,得到β‑FeOOH/eg‑C3N4复合纳米材料。本发明的优点是:操作简单易行,反应条件温和,整个过程避免了除原料外其他化学试剂和溶剂的使用,无副产物的生成,实现了复合与纳米晶生长的同步化,成本低廉,绿色环保,可满足产业化应用的要求。通过本发明所述的方法制备的β‑FeOOH/eg‑C3N4纳米棒状复合物催化剂,具有在可见光下光催化降解染性能,同时还有着电催化分解水产氢的能力。
Description
技术领域
本发明涉及一种双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,属于无机/有机复合纳米材料的绿色制备技术领域。
背景技术
纳米级的铁氧化物由于具有超强的吸附能力、极好的流动稳定性和较低廉价格等优点,已经成为国际水处理剂的研究热点,其中针状β-FeOOH是一类集吸附与光催化于一体的半导体材料,其晶体结构中层与层之间以氢键相结合,并且由于纳米材料独特的自组现象,使其不仅在环境保护、催化剂、生物医学等方面得到了广泛应用,而且是一类极具开发前途的纳米结构材料。但将β-FeOOH用于处理环境污染物降解,存在以下主要缺点:(1)在pH值2.5-3.5范围内进行,需消耗大量酸,且酸性水环境中铁浸出严重;(2)有机复杂因素下芬顿活动价低。近年来,异质光催化和芬顿催化作为降解水体和土壤中有机物的环保型方法得到了广泛的研究,然而,非均相铁基芬顿催化剂由于暴露铁活性位点少,且在非均相芬顿反应过程中Fe(III)/Fe(II)循环缓慢,效率较低,阻碍了其在水环境处理领域的广泛应用。因此,构建稳相、高活性的β-FeOOH复合材料非常有必要。石墨相氮化碳(g-C3N4)由于其廉价、易得的优点,广泛应用于光催化分解水制氢以及光催化降解污染物等领域,但由于其比表面积小、光生载流子易于复合等缺陷,限制了其光电催化活性进一步的提升,因此,将g-C3N4与β-FeOOH复合是提高其稳定性及光电催化活性的有效策略之一。
目前,在制备β-FeOOH通常是采用FeSO4为原料,加入NaOH或Na2CO3或尿素等沉淀剂在碱性条件下制备,步骤比较复杂繁琐,且未见β-FeOOH与g-C3N4复合的制备方法。
发明内容
本发明的目的是提供一种稳态、高活性的β-FeOOH/eg-C3N4具有双功能的纳米复合物催化剂的制备方法,即拥有较高的光电催化析氢(HER)以及优良的光催化降解染料性能。
本发明解决上述技术问题所采用的技术方案是:双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,包括以下步骤:以水为溶剂,加入适量eg-C3N4,调节溶液pH,再加入适量铁盐,超声,洗涤,干燥,得到β-FeOOH/eg-C3N4复合纳米材料。
按上述方案,所述干燥温度为50~80℃,干燥时间10~12h。
按上述方案,所述铁盐为FeCl3·6H2O,Fe2(SO4)3或Fe(NO3)3·9H2O。
按上述方案,调节pH采用盐酸,盐酸浓度为4~8mol/L,调节溶液pH 0.5~3。
按上述方案,所述铁盐与eg-C3N4的质量配比为0.5:1~2:1。
按上述方案,所述的eg-C3N4的制备方法包括有以下步骤:称取适量三聚氰胺第一次煅烧,得到bulk g-C3N4;然后加适量水超声一段时间后干燥,再进行二次煅烧,得到超薄的eg-C3N4。
按上述方案,所述的第一次煅烧是以5℃/min速率升温至500~600℃煅烧4~6h,所述的第二次煅烧是快速升温至550℃煅烧4~6h。
按上述方案,所述的超声时间0.5~1h,所述的干燥温度是105~120℃,所述的干燥时间是2h。
上述方案所得的双功能β-FeOOH/eg-C3N4复合纳米材料。
所述的双功能β-FeOOH/eg-C3N4复合纳米材料作为高光电催化析氢(HER)(塔菲尔斜率可达87.2mV/decade)以及优良的光催化降解染料(光照20min,10mg/mL RhB的降解率为100.0%)材料的应用。
本发明仅使用水为溶剂,加入铁盐和eg-C3N4,经过超声波和界面水分子的剧烈反应,制备稳态、高活性的β-FeOOH/eg-C3N4复合纳米材料,所得材料不仅具有良好的处理染料污染水的性能,同时还具有电催化分解水析氢的能力。其中以FeCl3·6H2O为原料制备的β-FeOOH/eg-C3N4的结晶性最高和光吸收能力最强,且FeCl3·6H2O:eg-C3N4的比例为0.5:1、1.0:1、1.5:1、2.0:1,当比例为1.5:1的β-FeOOH/eg-C3N4的塔菲尔斜率最小为87.2mV/decade,10mg/mL RhB溶液光照20min后降解率为100%,具有较好的HER的性能和光催化降解染料的性能。
本发明的优点是:操作简单易行,反应条件温和,整个过程避免了除原料外其他化学试剂和溶剂的使用,无副产物的生成,实现了复合与纳米晶生长的同步化,成本低廉,绿色环保,可满足产业化应用的要求。通过本发明所述的方法制备的β-FeOOH/eg-C3N4纳米棒状复合物催化剂,具有在可见光下光催化降解染性能,同时还有着电催化分解水产氢的能力。
附图说明
图1为实施例1中得到β-FeOOH/eg-C3N4复合材料:(a)TEM图,(b)HRTEM图,(c)电子衍射图;
图2为不同铁源所制备的β-FeOOH/eg-C3N4复合材料的XRD图;
图3为实施例1中得到β-FeOOH/eg-C3N4复合材料:(a)交流阻抗图,(b)光电流图;
图4为不同铁盐和不同比例制备所得到的β-FeOOH/eg-C3N4复合材料的Tafel斜率曲线:(a)不同铁盐,(b)不同比例;
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。
实施例1
(1)eg-C3N4的制备
取18g三聚氰胺于坩埚中,置于马弗炉中以5℃/min的升温速度加热到550℃,煅烧4h,得到黄色Bulk g-C3N4。取6g g-C3N4于坩埚中,加适量水超声1h后置于120℃烘箱中干燥2h,冷却后再置于马弗炉中加热到550℃,继续煅烧4h,冷却后得到eg-C3N4。
(2)β-FeOOH/eg-C3N4的制备
取100mg的eg-C3N4粉末放入100ml的烧杯中,随后加入50ml的去离子水,再用6mol/L的盐酸调节pH=2。再加入142mg的FeCl3·6H2O后超声6h,离心分离,产物分别用乙醇和纯水洗涤3次,放入60℃烘箱中干燥12h。
所得产物形貌、结构和成分经透射电镜图(TEM)、高分辨透射电镜图(HRTEM)、选区电子衍射图(SADE)和X射线衍射图(XRD)进行表征。图1a是棒状形貌β-FeOOH掺杂在超薄eg-C3N4片上的TEM图。图1b是棒状β-FeOOH的HRTEM图,图1c是棒状β-FeOOH的SADE图。由图1b得出棒状β-FeOOH的晶格间距分别为0.331nm和0.252nm;从图1c可以看出β-FeOOH为单晶结构,(211)晶面晶格间距为0.255nm,(310)晶面晶格间距为0.333nm;均与四方相β-FeOOHJCPDS No.34-1266标准卡片相吻合,证实已制备出β-FeOOH。
从图2可以看出,在27.4°处有一个明显的衍射峰,层间距d=0.325nm,对应g-C3N4的(002)晶面,为芳香物层间堆积峰,其余的衍射峰均为四方相β-FeOOH的衍射峰,且与JCPDS No.34-1266标准卡片相吻合,进一步证实成功的制备了β-FeOOH/g-C3N4复合物。
实施例2
(1)eg-C3N4的制备
取6g三聚氰胺于坩埚中,置于马弗炉中以5℃/min的升温速度加热到550℃,煅烧4h,得到黄色的eg-C3N4。取3g-C3N4于坩埚中,加适量水超声1h后置于120℃烘箱中干燥2h,冷却后再置于马弗炉中加热到550℃,继续煅烧5h,冷却后得到eg-C3N4。
(2)β-FeOOH/eg-C3N4的制备
取50mg eg-C3N4粉末放入100ml的烧杯中,加入50ml的去离子水,再用6mol/L的盐酸调节溶液pH=1,超声1h后,加入94mg的FeCl3·6H2O,继续超声4h,离心分离,产物分别用乙醇和纯水洗涤3次,放入60℃烘箱中干燥12h。
实施例3
(1)eg-C3N4的制备
取9g三聚氰胺于坩埚中,置于马弗炉中以5℃/min的升温速度加热到550℃,煅烧4h,得到黄色Bulk g-C3N4。取3g-C3N4于坩埚中,加适量水超声1h后置于120℃烘箱中干燥2h,冷却后再置于马弗炉中加热到550℃,继续煅烧4h,冷却后得到eg-C3N4。
(2)β-FeOOH/eg-C3N4的制备
取200mg的eg-C3N4粉末放入100ml的烧杯中,加入100ml的去离子水,再用6mol/L的盐酸调节溶液pH=0.5,超声1h后,加入378mg FeCl3·6H2O,超声6h,离心分离,产物分别用乙醇和纯水洗涤3次,放入60℃烘箱中干燥12h。
实施例4
(1)eg-C3N4的制备
取3g三聚氰胺于坩埚中,置于马弗炉中以5℃/min的升温速度加热到550℃,煅烧4h,得到黄色Bulk g-C3N4。取3g g-C3N4于坩埚中,加适量水超声0.5~1h后置于120℃烘箱中干燥2h,冷却后再置于马弗炉中加热到550℃,继续煅烧4h,得到淡黄色的产物,记为eg-C3N4。
(2)β-FeOOH/eg-C3N4的制备
取25mg的eg-C3N4粉末放入100ml的烧杯中,加入25ml的去离子水,再用6mol/L的盐酸调节溶液pH=0.5,超声0.5h后,加入47mg的FeCl3·6H2O,继续超声2h,离心分离,产物分别用乙醇和纯水洗涤3次,放入60℃烘箱中干燥10h。
实施例5电化学性能测试
(1)β-FeOOH/eg-C3N4/GCE制备:准确称取实施例1中所制备且已研磨好的β-FeOOH/eg-C3N4粉末4mg,将其分散于1mL超纯水中,超声30min使其分散均匀,制成4mg·mL-1的分散液。用微量进样器取5μL上述分散液滴涂在处理好的GCE表面,干燥后即可得到β-FeOOH/eg-C3N4/GCE。
(2)阻抗测试:将处理好的β-FeOOH/eg-C3N4/GCE电极置于5mmoL铁氰化钾+亚铁氰化钾和0.1moL KCl的混合溶液中,用甘汞电极为参比电极,铂丝为对电极,测得复合材料的阻抗如图3a所示,由图可见β-FeOOH/eg-C3N4复合材料的在高频区的能奎斯特半圆弧比eg-C3N4的半圆弧小,纯β-FeOOH和eg-C3N4的阻抗分别是β-FeOOH/eg-C3N4复合材料的2.56倍和1.47倍,表明复合材料具有更小的阻抗值和更强的电子传输能力,表面暴露活性位点的增加,加速了电极表面电子传递速率。
(3)光电流测试:Pt为对电极,Ag/AgCl为参比电极,β-FeOOH/eg-C3N4/GCE电极为工作电极,1mol·L-1硫酸钠为电解液,300w氙灯为光源,测得复合材料的光电流图如图3b所示。eg-C3N4样品产生的光电流值为1.52μA·cm-2,而β-FeOOH与eg-C3N4的复合增强了电极的光电流密度,使其光电流密度增加到2.53μA·cm-2,约为eg-C3N4样品光电流密度的1.6倍,增加了光生e-和h+的分离效率,具有更高的光电催化活性。
(4)Tafel斜率曲线测试:不同条件制备的β-FeOOH/eg-C3N4修饰GCE获得不同的工作电极,分别置于5mL 0.5mol·L-1的硫酸溶液中活化30min,然后以甘汞电极为参比电极,碳棒为对电极,氙灯为光源,测得到复合材料Tafel斜率曲线如图4所示。不同铁盐(FeCl3·6H2O,Fe2(SO4)3,Fe(NO3)3·9H2O)制备的β-FeOOH/eg-C3N4/GCE复合材料Tafel斜率曲线中,以FeCl3·6H2O为原料制备的β-FeOOH/eg-C3N4Tafel斜率最小(图4a),且FeCl3·6H2O:eg-C3N4的比例为1.5:1的β-FeOOH/eg-C3N4的塔菲尔斜率最小为87.2mV/decade(图4b),具有较好的HER的性能。
实施例6光催化性能测试
将25mg的光催化剂(实施例1制备)加入到50mL浓度为10mg/mL的RhB溶液中,暗处搅拌30min,加入2mL 10mmol/L的H2O2,PLS-SXE 300W氙灯光照20min,RhB的降解率为100.0%。
Claims (10)
1.双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,包括以下步骤:以水为溶剂,加入适量eg-C3N4,调节溶液pH,再加入适量铁盐,超声,洗涤,干燥,得到β-FeOOH/eg-C3N4复合纳米材料。
2.根据权利要求1所述的双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,其特征在于所述干燥温度为50~80℃,干燥时间10~12h。
3.根据权利要求1所述的双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,其特征在于所述铁盐为FeCl3·6H2O,Fe2(SO4)3或Fe(NO3)3·9H2O。
4.根据权利要求1所述的双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,其特征在于调节pH采用盐酸,盐酸浓度为4~8mol/L,调节溶液pH 0.5~3。
5.根据权利要求1所述的双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,其特征在于所述铁盐与eg-C3N4的质量配比为0.5:1~2:1。
6.根据权利要求1所述的双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,其特征在于所述的eg-C3N4的制备方法包括有以下步骤:称取适量三聚氰胺第一次煅烧,得到bulkg-C3N4;然后加适量水超声一段时间后干燥,再进行二次煅烧,得到超薄的eg-C3N4。
7.根据权利要求6所述的双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,其特征在于所述的第一次煅烧是以5℃/min速率升温至500~600℃煅烧4~6h,所述的第二次煅烧是快速升温至550℃煅烧4~6h。
8.根据权利要求1所述的双功能β-FeOOH/eg-C3N4复合纳米材料的制备方法,其特征在于所述的超声时间0.5~1h,所述的干燥温度是105~120℃,所述的干燥时间是2h。
9.权利要求1-8任一项权利要求所得的双功能β-FeOOH/eg-C3N4复合纳米材料。
10.权利要求9所述的双功能β-FeOOH/eg-C3N4复合纳米材料作为高光电催化析氢或光催化降解染料材料的应用。
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