CN113769748A - 一种FeNi@玉米芯活性炭复合材料的制备 - Google Patents
一种FeNi@玉米芯活性炭复合材料的制备 Download PDFInfo
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- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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Abstract
本发明涉及一种FeNi@玉米芯活性炭复合材料的制备。本发明以废弃的玉米芯、铁盐、镍盐和对苯二甲酸为主要原料,经搅拌、溶剂热、冷却、离心、干燥和活化‑炭化过程制备得到FeNi@玉米芯活性炭复合材料(FeNi@CCAC)。本发明制备的FeNi@CCAC具有较大的比表面积(904.72m2/g)和丰富的孔结构,有利于FeNi纳米粒子的均匀负载、有机污染物的吸附与固定,且可加速Fe3+/Fe2+的转化和电子的传输与跃迁。基于此,FeNi@CCAC可降低光Fenton反应中载流子复合率,显著提高对有机污染物的光Fenton催化降解性能和循环稳定性。此外,FeNi@CCAC可广泛用于催化降解水环境中的多种有机污染物,具有较强的普适性且不产生二次污染,可重复多次使用,适合大规模生产。该材料易得、成本低、易回收和环境友好,既符合实际应用需求,同时也提高了农林废弃物的高附加值利用。
Description
技术领域
本发明涉及一种FeNi@玉米芯活性炭复合材料的制备。
背景技术
随着工农业的快速发展给生产和生活提供便利的同时对生态环境造成了严重的污染问题。一些具有高毒性、易富集和难降解的染料肆意排放,严重的威胁着人们与动物的生命安全。因此,水体污染已成为当今世界亟需解决的难题。目前,治理水污染的解决办法有:物理法、吸附法、生物降解法、化学氧化法、光催化法和光Fenton法等。物理法和化学法具有较高的经济成本,且会产生一些有毒、有害的产物排放到环境中,导致二次污染。生物法主要是依靠细菌和真菌等对染料进行脱色分解来完成,但该方法存在起效慢,脱色周期长,筛选菌种易被外来菌种入侵,难以长期维持等不足。因此,导致生物法无法大规模应用。吸附法对染料的去除有不错的效果,但是需要选择具有比表面积大、孔结构丰富、活性位点合适和吸附能力稳定的吸附剂,但仍存在不能完全去除污染物且会产生有害产物的问题。光Fenton法是通过Fenton反应从H2O2中产生反应性强的羟基自由基,是氧化降解有机污染物最有效的方法之一。此外,因其降解效果好、工艺简单和矿化完全而成为处理水污染的研究热点。但用于Fenton反应的样品的制备仍是当前的挑战。如以Fe2O3纳米粒子为光Fenton催化剂时,由于纳米粒子较高的表面能,使其易发生团聚,减少了催化剂表面活性位点,降低了对有机污染物的降解效果。另外,仍存在Fe3+/Fe2+转化率较低的问题。鉴于此,需要设计并制备具有高催化效率的光Fenton催化剂。本工作通过简单的水热和炭化活化相结合的方法,合成了具有高效光Fenton性能的FeNi@CCAC复合材料来解决目前光Fenton反应存在的难题。
活性炭由于比表面积大和孔结构丰富而被广泛用作催化剂的载体。尤其是生物质活性炭,不仅来源广泛和成本低,而且具有可持续和环境友好等优点。但不同原料制备的活性炭其表面积和孔结构也有较大的差别。为此,许多研究通过探究不同种类的生物质原料,将其与金属或金属氧化物复合或掺杂的方法来解决金属和金属氧化物纳米颗粒小和易团聚的问题。然而,金属或金属氧化物纳米颗粒会发生堵塞活性炭孔隙和产生二次污染等问题。近年来,由于金属有机框架(MOF)是将金属或金属簇与有机配体通过配位键进行周期性结合的三维框架结构,且具有可调控的孔结构、不饱和的金属配位键、多样的结构和超低的密度等特点。因此,金属有机框架被提出用于代替颗粒小和易团聚的金属或者金属氧化物在许多领域被广泛的研究,如超级电容器、析氢、储气、气体分离、化学传感、药物释放和催化等。而MOF在水和高温环境下框架结构不稳定、容易坍塌。因此,本发明以废弃的玉米芯为原料,采用溶剂热和炭化活化相结合的方法,构建了高度稳定的FeNi纳米颗粒均匀分散在玉米芯活性炭结构中的FeNi@CCAC复合材料。
发明内容
本发明的目的在于提供一种溶剂热和炭化活化相结合的方法,用于制备一种FeNi@玉米芯活性炭复合材料的制备。
本发明的具体步骤如下:
(1)将MOF前驱体(铁盐、镍盐和对苯二甲酸)和玉米芯粉末(CC)以1:0~1:9质量比在DMF溶液中进行混合,随后在磁力搅拌器上,以200~700rpm的转速下搅拌30~60min,得到均匀的混合溶液。
(2)将混合溶液转移至有聚四氟乙烯内置的高压反应釜中,放入均相反应器中,在80~180℃下,溶剂热处理12~64h。
(3)溶剂热反应后的溶液自然冷却至室温,在3500~8000rpm的转速下进行离心处理,随后用甲醇和水进行洗涤3~6次,在40~150℃下,过夜干燥,制备得到有机金属框架/玉米芯(MOF/CC)。
(4)将得到的MOF/CC放入瓷舟中,然后在管式炉中,在氮气气氛下,以5℃/min的升温速率,将其加热到450℃,并保持30~120min,得到MOF@CC-450。随后加入与MOF@CC-450与KOH的质量比为1:0~1:6,继续在管式炉中,以上述条件进行升温到600~1200℃,保持30~420min,冷却至室温后得到FeNi@CCAC。本发明通过一系列的物理化学表征,结果证实成功制备了FeNi@CCAC复合材料。
本发明对制备的FeNi@CCAC复合材料进行光Fenton催化降解实验条件的探究和性能测试。5mg FeNi@CCAC复合材料,在pH=3,60μL H2O2条件下,暗反应30min达到吸附平衡后,在可见光下,90min内对10mg/L,100mL的罗丹明B进行了光Fenton催化降解实验;在相同的光Fenton催化降解实验条件下,对不同的FeNi@CCAC复合材料对有机染料(罗丹明B、亚甲基蓝和孔雀石绿)降解效率进行了比较和分析,选出最佳性能的FeNi@CCACC复合材料,对其进行不同染料的光Fenton催化降解实验,均具有优异的性能。
附图说明
图1为FeNi@CCAC复合材料扫描电镜和透射电镜图;
图2为FeNi@CCAC复合材料降解罗丹明B的5次光Fenton循环图。
具体实施方式
这些实施例仅限于说明本发明,但本发明并不局限与这些实施例。
实施例1:
将MOF前驱体和CC以1:0的比例在DMF溶液中进行混合,将混合液置于磁力搅拌器上,在400rpm的转速下搅拌30min。将溶液混合均匀后,转移至高压反应釜中,在均相反应器中120℃的条件下,溶剂热处理24h。经过7000rpm离心,洗涤3次,在80℃下,过夜干燥,得到MOF。随后,将其在氮气气氛下以5℃/min的升温速率,加热到900℃并保持60min。冷却至室温后得到MOF-900。物化性能测试结果显示:制备的MOF材料的比表面积为257.82m2/g。光Fenton催化降解实验表明:90min内,MOF-900对10mg/L,100mL罗丹明B的降解率为29.25%。
实施例2:
将MOF前驱体和CC以1:1的比例在DMF溶液中进行混合,将混合液置于磁力搅拌器上,在700rpm的转速下,搅拌30min。将溶液混合均匀后,转移至高压反应釜中,在均相反应器中120℃的条件下,溶剂热处理24h。在8000rpm转速下离心,洗涤3次,80℃下,过夜干燥,制备得到MOF@CC-1复合材料,然后将其在氮气气氛下以5℃/min的升温速率,加热到450℃并保持30min。得到MOF/CC-450。随后加入与MOF/CC-450质量比为1:1的KOH,继续在管式炉中,以上述条件进行升温到900℃并保持60min。冷却至室温后得到FeNi@CCAC-1。物化性能测试结果显示:复合材料的比表面积为904.72m2/g。光Fenton催化降解实验表明:90min内,FeNi@CCAC-1对10mg/L,100mL罗丹明B的降解率为97%。
实施例3:
MOF前驱体和CC以1:5的比例在DMF中进行混合,将混合液置于磁力搅拌器上,在600rpm的转速下搅拌60min。将溶液混合均匀后,转移至高压反应釜中,在均相反应器中180℃的条件下,溶剂热处理12h。经过7000rpm离心,洗涤5次,150℃下,过夜干燥,制备得到MOF/CC-5复合材料,然后将其在氮气气氛下以5℃/min的升温速率,将其加热到450℃并保持60min。得到MOF/CC-450。随后加入与MOF/CC-450质量比为1:3的KOH,继续在管式炉中,以上述条件进行升温到700℃保持240min。冷却至室温后,得到FeNi@CCAC-5。结果显示:制备的MOF/CCAC-3复合材料的比表面积为762.45m2/g。光Fenton催化降解实验表明:90min内,FeNi@CCAC-5对10mg/L,100mL罗丹明B的降解率为78.15%。
实施例4:
MOF前驱体和CC以1:9的比例在DMF中进行混合,将混合液置于磁力搅拌器上在200rpm的转速下,搅拌30min。将溶液混合均匀后,转移至高压反应釜中,在均相反应器中120℃的条件下,溶剂热处理24h。经过7000rpm离心,洗涤3次,60℃下,过夜干燥,制备得到MOF/CC-9复合材料,然后将其在氮气气氛下,以5℃/min的升温速率,将其加热到450℃并保持90min。得到MOF/CC-450。随后加入与MOF/CC-450质量比为1:5的KOH,继续在管式炉中,以上述条件进行升温到800℃保持120min。冷却至室温后得到FeNi@CCAC-9。物化性能测试结果显示:制备的MOF/CCAC-5复合材料的比表面积为823.61m2/g。光Fenton催化降解实验表明:90min内,FeNi@CCAC-9对10mg/L,100mL罗丹明B的降解率为70%。
实施例5:
MOF前驱体和玉米芯粉末CC以0:1的比例在DMF中进行混合,将混合液置于磁力搅拌器上在500rpm的转速下,搅拌60min。混合均匀后转移至高压反应釜中,在均相反应器中120℃的条件下,溶剂热处理12h。经过7000rpm离心,洗涤3次,50℃下,过夜干燥,制备得到CC,然后将其在氮气气氛下以5℃/min的升温速率,将其加热到450℃并保持120min。得到CC-450。随后加入与CC-450质量比为1:1的KOH,继续在管式炉中,以上述条件进行升温到900℃保持60min。冷却至室温后,得到CCAC。光Fenton催化降解实验表明:90min内,CCAC对10mg/L,100mL罗丹明B的降解率为51.08%。
实施例6:
将MOF前驱体和CC以1:1的比例在DMF中进行混合,将混合液置于磁力搅拌器上在700rpm的转速下,搅拌30min。将溶液混合均匀后,转移至高压反应釜中,在均相反应器中120℃的条件下,溶剂热处理48h。经过8000rpm离心,洗涤5次,80℃下,过夜干燥,制备得到MOF@CC-1复合材料,然后将其在氮气气氛下,以5℃/min的升温速率,将其加热到450℃并保持30min。得到MOF/CC-450。随后加入与MOF/CC-450质量比为1:1的KOH,继续在管式炉中,以上述条件进行升温到900℃保持60min。冷却至室温后,得到FeNi@CCAC-1。物化性能测试结果显示:复合材料的比表面积为904.72m2/g。光-Fenton催化降解实验表明:90min内,FeNi@CCAC-1对10mg/L,100mL亚甲基蓝的降解率为95%。
实施例7:
将MOF前驱体和CC以1:1的比例在DMF中进行混合,将混合液置于磁力搅拌器上在700rpm的转速下,搅拌30min。将溶液混合均匀后,转移至高压反应釜中,在均相反应器中120℃的条件下,溶剂热处理48h。经过8000rpm离心,洗涤5次,80℃下过夜干燥,制备得到MOF@CC-1复合材料,然后将其在氮气气氛下,以5℃/min的升温速率,将其加热到450℃并保持30min。得到MOF/CC-450。随后加入与MOF/CC-450质量比为1:1的KOH,继续在管式炉中,以上述条件进行升温到900℃保持60min。冷却至室温后,得到FeNi@CCAC-1。物化性能测试结果显示:复合材料的比表面积为904.72m2/g。光-Fenton催化降解实验表明:90min内,FeNi@CCAC-1对10mg/L,100mL孔雀石绿的降解率为92%。
Claims (5)
1.一种FeNi@玉米芯活性炭复合材料的制备,其特征在于所述方法如下步骤进行:
(1)将MOF前驱体(铁、镍金属盐和有机配体)和玉米芯粉末(CC)以一定质量比在DMF溶液中进行混合,随后在磁力搅拌器上,以200~700rpm的转速下搅拌30~60min,得到均匀的混合溶液。
(2)将混合溶液转移至有聚四氟乙烯内置的高压反应釜中,放入均相反应器中,在一定温度下,溶剂热反应一定时间。
(3)溶剂热反应后的溶液自然冷却至室温,在3500~8000rpm的转速下进行离心处理,随后用甲醇和水进行洗涤3~6次,在40~150℃下过夜干燥,制备得到有机金属框架/玉米芯(MOF/CC)。
(4)将得到的MOF/CC放入瓷舟中,然后在氮气气氛下,以5℃/min的升温速率下,将其加热到一定温度,并保持30~120min,得到MOF@CC-T。随后加与MOF@CC-T不同质量比的KOH,继续在上述条件进行升温到一定温度,并保持一定时间。最后,冷却至室温后得到MOF衍生的核壳结构的FeNi@玉米芯活性炭复合材料(FeNi@CCAC)。
2.如权利要求1所述的一种FeNi@玉米芯活性炭复合材料的制备,其特征在于步骤(1)所述MOF前驱体(铁、镍金属盐和有机配体)和玉米芯粉末(CC)的质量比为1:0~1:9;其中铁、镍金属盐可为Fe(NO3)2·6H2O、Fe(NO3)3·9H2O、FeCl3·6H2O、FeCl2·4H2O和Ni(NO3)2·6H2O和NiCl2·6H2O中的一种,有机配体为对苯二甲酸、1,3,5-均苯三甲酸、卟啉、酞菁和对苯二甲酸二甲酯中的一种。
3.如权利要求1所述的一种FeNi@玉米芯活性炭复合材料的制备,其特征在于步骤(2)所述的溶剂热反应温度为80~180℃,处理时间为12~64h。
4.如权利要求1所述的一种FeNi@玉米芯活性炭复合材料的制备,其特征在于步骤(4)在氮气气氛下,以5℃/min的升温速率,将其加热到450℃,并保持30~120min,得到MOF@CC-450,MOF@CC-450与KOH的质量比为1:0~1:6,继续在上述条件,升温的温度为600~1200℃,保持时间为30~420min。
5.如权利要求1所述的一种FeNi@玉米芯活性炭复合材料的制备,其特征在于所述一种FeNi@CCAC用于光Fenton催化降解有机染料分子。
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