CN106311256B - 一种石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法 - Google Patents
一种石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法 Download PDFInfo
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 38
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
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- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
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- B01J35/33—
-
- B01J35/39—
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
一种石墨烯/β‑Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法,属于催化剂的技术领域。本发明以石墨烯、硝酸铋和SrFe12O19为原料,采用溶液浸渍一步热还原法制得产品。本发明工艺步骤简单,所用设备少,制备周期短,生产安全且成本低;采用本发明方法制备出的产品光催化性能优异,在可见光下50min内对罗丹明B的降解率达到99.5%以上;此外该产品磁学性能良好,矫顽力为4142.6G,抗退磁能力较强,磁回收重复使用4次后对罗丹明B的降解率依然可以达到90.2%,有利于催化剂的回收和重复使用,因此可节约工业生产成本。采用本发明制备得到的产品可广泛用于光催化降解水体有机污染物。
Description
技术领域
本发明属于催化剂技术领域,具体涉及石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法。
背景技术
石墨烯具有大的比表面积和优异的导电性能,可以将光生电子转移到其片层中,从而阻止光生电子在半导体表面发生积累,避免光生电子空穴对的复合,从而提高光催化效率,在光催化分解水制氢、光催化降解有机污染物和光化学电池等光催化领域得到了广泛的应用。
在光催化反应中,石墨烯复合氧化铋(Bi2O3)可以增强催化剂催化活性,同时进行赋磁可解决反应后难以回收和回收不彻底引起的二次污染问题。目前,许多研究者已成功制备出纳米Bi2O3催化剂并进行了相关改性方面的工作,但普遍存在合成产率低、污染大、成本高和工序复杂等问题。因此,在环境友好、降低成本的条件下,制备出便于回收的高效Bi2O3催化剂有十分重要的意义。
现有石墨烯复合Bi2O3光催化剂的制备方法,如《Journal of Alloys andCompounds》2015 年649卷872-877页中的“Visible light photocatalytic degradationof dyes byβ-Bi2O3/grapheme nanocomposites”(对比文件1)一文,公开的方法是:采用溶胶-凝胶法,以石墨烯、硝酸铋、柠檬酸、乙醇和丙烯酰胺为原料,首先将硝酸铋分散于硝酸溶液中;然后加入柠檬酸和丙烯酰胺单体,在磁力搅拌下加热至80℃形成凝胶;随后在120℃干燥并于600℃加热两小时得到β-Bi2O3;最后将所得的β-Bi2O3和石墨烯分散于乙醇中,并超声10min,再在60℃空气中干燥10h得到最终的产品。该方法的主要缺点是:(1)该复合光催化剂需要首先制备出β -Bi2O3,然后与石墨烯进行无机混合,此处使用的是简单的超声法,该方法不宜于无机物的有效复合,从而降低光催化剂的催化效能;(2)该复合光催化剂的性能较低,在可见光下, 240min内对亚甲基蓝的降解率仅为65%,且未考察对较难降解的染料如罗丹明B的作用效能; (3)该实验未考察光催化剂的回收和重复使用性能,这不利于催化剂的使用经济性,而且该催化剂属于纳米级材料,不易于回收使用,因此有可能造成二次污染。
此外,对Bi2O3磁性光催化剂改性的研究主要集中在二元复合基础上,如专利号为CN 1034470224 A的专利“一种铋基锶磁性光催化剂的制备方法及其铋基锶磁性光催化剂”(对比文件2)一文中以硝酸铋和铁酸锶(SrFe12O19)为原料,用十二烷基苯磺酸钠为分散剂,先制备铋基锶磁性光催化剂的前驱体,再经烘干焙烧得三氧化二铋/锶铁氧体 (Bi2O3/SrFe12O19)二元复合光催化剂。此法的不足之处在于:(1)制备过程中需要用到大量的十二烷基苯磺酸钠,高纯度的十二烷基苯磺酸钠价格昂贵,因此不适用于规模化生产;(2) 该工艺制备过程繁琐,耗时较长,另外在制备过程中需要在500-600℃的高温下进行3-5h的焙烧,因此会造成最终产品烧结严重,颗粒较大,影响催化效能,并且长时间高温焙烧对仪器设备要求较高同时也造成耗能较多,难以达到工业化节能要求;(3)该二元复合磁性光催化剂的活性组分为α型的Bi2O3,相对于β型Bi2O3催化性能较低,在可见光下对10mg/L的亚甲基蓝溶液降解率达98%时需要4h之久。
发明内容
本发明的目的是针对现有二元Bi2O3复合光催化剂制备方法复杂以及光催化效率低的问题,提出一种石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法,制备的石墨烯/ β-Bi2O3/SrFe12O19三元复合磁性光催化剂在可见光下具有较高的光催化效率,且该催化剂制备方法简单,可有效降解废水中芳香杂环类染料有机污染物。本发明方法具有原料安全,工艺流程对环境友好,生产成本低,所制得催化剂回收方便且可重复利用等特点。
本发明石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法如下:
(1)石墨烯/β-Bi2O3/SrFe12O19前驱体的制备
称取8mmol的Bi(NO3)3.5H2O于1mol/L的硝酸中,搅拌0.5h至硝酸铋完全溶解,然后加入质量分数为15%的SrFe12O19,搅拌2h,再将上述溶液逐滴加入至80ml、0.6mol/L碳酸钠溶液中,之后按氧化石墨烯和β-Bi2O3/SrFe12O19质量比为0.5~5∶100逐滴加入适量的氧化石墨烯(GO),继续搅拌12h至溶液呈棕色,静置后,溶液产生分层现象,过滤,滤饼经水洗、醇洗数次后,在80℃中干燥10h。
(2)石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备
取(1)中干燥后的样品置于研钵中研磨,然后移至马弗炉中,抽真空,在氮气保护下,控制升温速度为4℃/min,保温温度为380℃,焙烧10min后取出样品,自然冷却至室温,即得石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂。
本发明采用上述技术方案,主要有以下效果:
(1)本发明制备的三元复合磁性光催化剂,在可见光下对10mg/l的罗丹明B溶液进行照射,50min后紫外可见分光光度计未能检测出罗丹明B,说明降解率达到99.5%以上,此降解效率明显高于对比文件1、2中对亚甲基蓝的降解效率。
(2)本发明方法选用的原料安全易得,工艺流程简单,所用设备少,因而生产安全,成本低;加之不需要长时间高温焙烧,节能环保,因此本发明方法非常适宜于大规模生产。
(3)本发明方法制备的三元复合磁性光催化剂,磁学性能度良好,矫顽力为4142.6G,抗退磁能力较强,重复使用4次后,在可见光下50min内对罗丹明B的降解率仍达90.2%,这有利于催化剂的回收和重复利用,因此可节约工业生产成本。
(4)本发明方法制备出的三元复合磁性光催化剂,属于多功能复合材料,丰富了磁性催化剂的范畴。
附图说明
图1为实施例1制备得到的石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的X射线衍射图谱;
图2为实施例1制备得到的石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的扫描电子显微镜图;
图3为实施例1制备得到的石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的磁滞回线,为了便于比较,同时附上了β-Bi2O3/SrFe12O19二元磁性光催化剂的磁滞回线。
具体实施方式
下面结合具体实施方式,进一步说明本发明。
实施例1
一种石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法,其具体步骤如下:
(1)石墨烯/β-Bi2O3/SrFe12O19前驱体的制备
称取8mmol的Bi(NO3)3·5H2O于1mol/L的硝酸中,搅拌0.5h至硝酸铋完全溶解,然后加入质量分数为15%的SrFe12O19,搅拌2h,再将上述溶液逐滴加入至80ml、0.6mol/L碳酸钠溶液中,按氧化石墨烯和β-Bi2O3/SrFe12O19质量比为2∶100逐滴加入氧化石墨烯(GO),继续搅拌12h至溶液呈棕色,静置后,溶液产生分层现象,过滤,滤饼经水洗、醇洗数次后,在80℃中干燥10h。
(2)石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备
取(1)中干燥后的样品置于研钵中研磨,然后后移至马弗炉中,抽真空,在氮气保护下,控制升温速度为4℃/min,保温时间为380℃,焙烧10min后取出样品,自然冷却至室温,即得石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂。
实施例2
一种石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法,其具体步骤如下:
(1)石墨烯/β-Bi2O3/SrFe12O19前驱体的制备
称取8mmol的Bi(NO3)3·5H2O溶于1mol/L的硝酸中,搅拌0.5h至硝酸铋完全溶解,然后加入质量分数为15%的SrFe12O19,搅拌2h,再将上述溶液逐滴加入至80ml、0.6mol/L碳酸钠溶液中,按氧化石墨烯和β-Bi2O3/SrFe12O19质量比为0.5∶100逐滴加入氧化石墨烯(GO),继续搅拌12h至溶液呈棕色,静置后,溶液产生分层现象,过滤,滤饼经水洗、醇洗数次后,在80℃中干燥10h。
(2)同实施例1第(2)步。
实施例3
一种石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法,其具体步骤如下:
(1)石墨烯/β-Bi2O3/SrFe12O19前驱体的制备
称取8mmol的Bi(NO3)3·5H2O于1mol/L的硝酸中,搅拌0.5h至硝酸铋完全溶解,然后加入质量分数为15%的SrFe12O19、搅拌2h,再将上述溶液逐滴加入至80ml、0.6mol/L碳酸钠溶液中,按氧化石墨烯和β-Bi2O3/SrFe12O19质量比为5∶100逐滴加入氧化石墨烯(GO),继续搅拌12h至溶液呈棕色,静置后,溶液产生分层现象,过滤,滤饼经水洗、醇洗数次后,在80℃中干燥10h。
(2)同实施例1第(2)步。
实验结果
用实施例1制备得到的三元复合磁性光催化剂进行X射线衍射测试,其X射线衍射图谱如图1所示;实施例1制备得到的三元复合磁性光催化剂表面形貌分析如图2所示;用实施例1制备得到的三元复合磁性光催化剂,进行磁学性能测试,其磁滞回线如图3所示;用实施例1制备出的三元复合磁性光催化剂,进行光催化活性测试和重复利用。
从图1可知,石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的X射线衍射图谱中25.71°,27.95°,31.76°,32.69°和46.22°分别对应正方晶系β-Bi2O3的(210)(201)(002)(220)和(200)晶面衍射,说明石墨烯和SrFe12O19并不会改变β-Bi2O3的晶型,从而保证了三元复合磁性光催化剂中有效活性组分的结晶完整。此外,在谱图中没有发现石墨烯的峰,原因是由于石墨烯的负载量太低(仅2%)。为了进一步验证石墨烯的有效复合,进行了扫面电子显微镜表征,结果如图2所示,在高倍视野下可以清晰的观察到二维层状结构的石墨烯存在。实施例1制备出的三元复合磁性光催化剂,在可见光下对罗丹明B溶液进行照射,50min后紫外可见分光光度计未能检测出罗丹明B,说明降解率达到99.5%以上;磁滞回线显示三元复合磁性光催化剂的矫顽力为4142.6G,相比于二元磁性光催化剂的矫顽力并没有发生改变,说明石墨烯的引入不会影响其磁学性能,而矫顽力的大小在一定程度上反映了抗退磁能力,这说明该催化剂抗退磁能力较强,有利于该催化剂进行磁性回收再利用。通过重复回收利用4次后,发现在相同条件下该三元复合磁性光催化剂对罗丹明B的降解率仍然达到90.2%,说明采用本发明制备的三元复合磁性光催化剂具有较高的光催化活性和稳定性。综上所述,本发明技术方案的工艺条件简单,易于操作,可以制得磁学性能较好、催化活性高、性能稳定优异的石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂。
Claims (1)
1.一种石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备方法,其特征在于所述方法的具体步骤如下:
(1)石墨烯/β-Bi2O3/SrFe12O19前驱体的制备
称取8mmol的Bi(NO3)3·5H2O于1mol/L的硝酸中,搅拌0.5h至硝酸铋完全溶解,然后加入质量分数为15%的SrFe12O19,搅拌2h,再将上述溶液逐滴加入至80mL、0.6mol/L的碳酸钠溶液中,按氧化石墨烯和β-Bi2O3/SrFe12O19质量比为0.5~5∶100逐滴加入氧化石墨烯,继续搅拌12h至溶液呈棕色,静置后,溶液产生分层现象,过滤,滤饼经水洗、醇洗数次后,在80℃中干燥10h;
(2)石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂的制备
取(1)中干燥后的样品置于研钵中研磨,然后移至马弗炉中,抽真空,在氮气保护下,控制升温速度为4℃/min,保温温度为380℃,焙烧10min后取出样品,自然冷却至室温,即得石墨烯/β-Bi2O3/SrFe12O19三元复合磁性光催化剂。
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