CN110064346A - 一种二氧化钛/硫化锌镉石墨烯气凝胶及其制备方法与应用 - Google Patents
一种二氧化钛/硫化锌镉石墨烯气凝胶及其制备方法与应用 Download PDFInfo
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- CN110064346A CN110064346A CN201910426062.1A CN201910426062A CN110064346A CN 110064346 A CN110064346 A CN 110064346A CN 201910426062 A CN201910426062 A CN 201910426062A CN 110064346 A CN110064346 A CN 110064346A
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Abstract
一种二氧化钛/硫化锌镉石墨烯气凝胶及其制备方法与应用。该制备方法为:将氧化石墨烯超声分散于乙醇水溶液中,将二氧化钛和硫化锌镉分别分散到无水乙醇后加入上述石墨烯分散液,充分搅拌得到均匀的悬浮液;向该悬浮液中分别加入丙烯酰胺、N,N‑亚甲基双丙烯酰胺和过硫酸铵,继续搅拌使其分散均匀;将该混合物转移到水热釜中,经高温反应后得到二氧化钛/硫化锌镉石墨烯水凝胶,经多次洗涤后冷冻干燥得到三维异质结构二氧化钛/硫化锌镉石墨烯气凝胶。本发明的异质结构石墨烯气凝胶可作为吸附剂和光催化剂用于水污染控制领域,特别是废水中六价铬的去除,具有制备方法简单,去除效率高,并且可将六价铬还原为低毒性的三价铬的优点。
Description
技术领域
本发明涉及水污染控制技术领域,具体涉及一种二氧化钛/硫化锌镉石墨烯气凝胶及其制备方法与应用。
背景技术
随着经济的高速发展,在工农业领域化学试剂被大量使用,我国大部分地表水和地下水受到了以重金属和有机物为主的污染物不同程度的污染,其中,六价铬是主要的重金属污染物之一,其毒性是三价铬的几十倍甚至百倍。六价铬为吞入性毒物/吸入性极毒物,皮肤接触可能导致过敏;更可能造成遗传性基因缺陷,吸入可能致癌,对环境有持久危险性,因此,对六价铬毒性的降低及有效去除一直是各国研究者的探讨热点。
目前,分离与去除水介质中的六价铬离子的方法有多种,如化学还原法、离子交换法、反渗透法、膜分离法、生物处理法、光催化还原法以及吸附法等。吸附法和光催化还原法由于其成本低、操作运行简便、去除效率较高并且吸附剂和催化剂可再生循环使用而受到广泛关注,但是,一般的吸附剂存在吸附容量有限和吸附速率低的问题;常见的光催化剂也存在光生电子和空穴对复合率高,量子利用效率低等缺陷,从而限制了其广泛应用。若将吸附和光催化结合起来就能够解决各自存在的缺点,提高处理效率,扩大其应用范围。常见的粉末状吸附剂和催化剂存在分离困难的问题,为了解决该问题,气凝胶是一种很好的选择。石墨烯作为一种新兴材料,由于其具备较大的比表面积,具有丰富的含氧官能团,导电性能良好等优良性质而备受关注。石墨烯气凝胶材料具有三维网络结构,既具备石墨烯材料本身具有的良好属性,又可以根据需要进行改性修饰,也受到了广泛关注。
发明内容
本发明的目的之一在于为废水中六价铬离子的去除提供一种高效、经济、环保、易于制备的二氧化钛/硫化锌镉石墨烯气凝胶材料。
本发明的目的之二在于提供上述二氧化钛/硫化锌镉石墨烯气凝胶的制备方法,该方法工艺简单、便于操作。
本发明的目的之三在于提供上述二氧化钛/硫化锌镉石墨烯气凝胶作为吸附剂和光催化剂协同去除废水中六价铬的应用方法。
本发明所采取的技术方案如下:
一种二氧化钛/硫化锌镉石墨烯气凝胶的制备方法,包括以下步骤:
(1)将氧化石墨烯溶液加入到乙醇水溶液中进行超声处理,得氧化石墨烯分散液;
(2)将二氧化钛和硫化锌镉纳米颗粒分别在超声条件下分散到无水乙醇中,再将两种分散液在搅拌条件下加入步骤(1)所得氧化石墨烯分散液中,继续搅拌得到均匀悬浮液;
(3)在搅拌条件下向步骤(2)所得的悬浮液中分别加入丙烯酰胺、N,N-亚甲基双丙烯酰胺和过硫酸铵,继续搅拌得到分散均匀的混合物;
(4)将步骤(3)所得混合物转移到水热反应釜中,经高温反应后,得到二氧化钛/硫化锌镉石墨烯水凝胶;
(5)将步骤(4)所得二氧化钛/硫化锌镉石墨烯水凝胶多次洗涤后进行冷冻干燥,得到二氧化钛/硫化锌镉石墨烯气凝胶。
上述方法中,步骤(1)中,所述氧化石墨烯溶液的浓度0.5~1.0g/L,所述乙醇水溶液中乙醇与水的体积比为1:1~1:4,所得氧化石墨烯分散液浓度为0.3~0.5g/L,所述超声处理的时间为45~60min。
上述方法中,步骤(2)中,所述二氧化钛的加入量为0.5~2.0mmol;所述硫化锌镉的加入量为0.5~2.0mmol,所述超声处理时间为20~30min,所述搅拌时间为30~45min。
上述方法中,所述硫化锌镉纳米颗粒的制备方法为:将2.5~5mmol的醋酸锌和2.5~5mmol的醋酸镉同时溶入5~10mL去离子水中得溶液A;将5~10mmol硫脲溶于30~40mL乙醇水溶液中得溶液B,将溶液A加入溶液B中,将混合溶液超声处理30~60min使其完全混匀,将其转移到50mL的水热釜中,在160~200℃下反应10~18h,待冷却至室温,用去离子水和乙醇多次洗涤后在60~80℃烘箱中干燥12h~24h得到硫化锌镉纳米颗粒;所述乙醇水溶液中乙醇与水的体积比为1:1~1:4。
上述方法中,步骤(3)中,所述丙烯酰胺的投加量为20~50mg,N,N-亚甲基双丙烯酰胺的投加量为20~50mg,过硫酸铵的投加量为3~8mg,所述搅拌时间为1~2h;步骤(4)中,反应温度为120~180℃,反应时间为3~5h。
上述方法中,步骤(5)中,所述冷冻干燥温度为-50~-80℃,时间为36~48h。
一种二氧化钛/硫化锌镉石墨烯气凝胶,所述二氧化钛/硫化锌镉石墨烯气凝胶具有三维网络结构,二氧化钛和硫化锌镉颗粒分布于被还原的氧化石墨烯片层上,形成了异质结构。
一种二氧化钛/硫化锌镉石墨烯气凝胶作为吸附剂和光催化剂应用于含六价铬废水的处理中。
上述应用,包括以下步骤:
将二氧化钛/硫化锌镉石墨烯气凝胶加入含六价铬的水溶液中,在暗环境中震荡至吸附平衡后,取溶液经滤膜进行固液分离,测定分离后所得溶液的中剩余六价铬离子含量;再将该反应体系在可见光照射下进行光催化反应,反应结束后测定溶液中剩余六价铬离子含量。
上述应用中,二氧化钛/硫化锌镉石墨烯气凝胶的投加量为0.1~1.0g/L;所述的吸附时间为40~60min,光催化时间为30~60min;所述光催化反应的反应温度为25±2℃,反应的pH为1.5~8.0。
与现有技术相比,本发明的优点在于:
(1)本发明充分利用石墨烯、二氧化钛和硫化锌镉的理化性质,通过简单的水热过程制得二氧化钛/硫化锌镉石墨烯气凝胶,形成了具有三维网络结构的异质结构系统,既提高了材料的吸附性能,同时也提高了其光催化效果。
(2)本发明制备工艺简单,设备要求低,操作便捷,易于大规模批量生产;
(3)本发明制备的二氧化钛/硫化锌镉石墨烯气凝胶能够协同吸附和光催化作用高效去除六价铬,并将其还原为毒性较低的三价铬,达到对六价铬的解毒目的;
(4)本发明制备的二氧化钛/硫化锌镉石墨烯气凝胶对六价铬进行去除后,材料通过简单过滤后即可进行重复利用,便于从液体中分离,不会对环境造成二次污染。
附图说明
图1本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶扫描电镜图。
图2本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶XRD谱图。
图3本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶XPS光谱图。
图4本发明实施例1-5制备的二氧化钛/硫化锌镉石墨烯气凝胶对六价铬去除效果对比。
图5本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶去除六价铬前后XRD谱图对比。
图6本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶去除六价铬前后XPS光谱图对比。
图7本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶不同pH条件下对六价铬去除效果对比。
图8本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶不同投加量条件下对六价铬去除效果对比。
图9本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶对不同浓度六价铬去除效果对比。
图10本发明实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶循环利用效果对比。
具体实施方式
下面结合实施例,对本发明作进一步的详细说明,但本发明的实施方式不限于此,对于未特别注明的工艺参数,可参照常规技术进行。
实施例1
(1)氧化石墨烯的制备:在1000mL的烧杯中,加入120mL的98%浓硫酸,置于冰水浴。然后,在搅拌的条件下,加入5g石墨粉和2.5g硝酸钠。在强烈的搅拌下,缓慢加入15g高锰酸钾,过程中保持温度不高于20℃,持续反应90min;然后移除冰水浴,将温度升高到35℃,持续搅拌反应30min。在搅拌条件下,缓慢加入230mL去离子水,并升温至98℃,溶液呈现棕色,反应15min;然后加入30mL30%的过氧化氢,待溶液呈亮黄色后,继续搅拌至没有气泡产生。将得到的产物先用5%的盐酸洗至无硫酸根,再用去离子水多次离心洗涤至中性,最后超声处理2h使其分散均匀,得到氧化石墨烯悬浮液保存备用。
(2)硫化锌镉(Zn0.5Cd0.5S)纳米颗粒的制备:将2.5mmol的醋酸锌和2.5mmol的醋酸镉同时溶入5mL去离子水中得溶液A;将5mmol硫脲溶于30mL乙醇水溶液(乙醇与水的体积比为1:2)中得溶液B,将溶液A加入溶液B中,将混合溶液超声处理30min使其完全混匀,将其转移到50mL的水热釜中,在180℃下反应12h,待冷却至室温,用去离子水和乙醇多次洗涤后在60℃烘箱中干燥12h得到硫化锌镉纳米颗粒。
(3)取步骤(1)所得氧化石墨烯悬浮液加入乙醇水溶液(乙醇与水的体积比为1:2)配成10mL浓度为0.3g/L的石墨烯悬浮液,超声处理60min形成均匀的石墨烯分散液。
(4)将0.5mmol的二氧化钛(从德固赛购得)和硫化锌镉粉末(即二氧化钛和硫化锌镉的摩尔比为1:1)分别在超声条件下分散到1mL无水乙醇中,再将两种分散液在搅拌条件下加入步骤(3)所得氧化石墨烯分散液中,继续搅拌得到均匀悬浮液;
(5)在搅拌条件下向步骤(4)所得的悬浮液中分别加入30mg丙烯酰胺、30mgN,N-亚甲基双丙烯酰胺和5mg过硫酸铵,继续搅拌得到分散均匀的混合物;
(6)将步骤(5)所得混合物转移到水热反应釜中,在120℃反应3h后,得到二氧化钛/硫化锌镉石墨烯水凝胶;
(7)将步骤(6)所得二氧化钛/硫化锌镉石墨烯水凝胶多次洗涤后在-50℃下冷冻干燥48h,得到二氧化钛/硫化锌镉石墨烯气凝胶。
本实施例得到的二氧化钛/硫化锌镉石墨烯气凝胶(TSGA)得扫描电镜图如图1所示,可以看出该气凝胶材料呈现出三维网络多孔结构,二氧化钛和硫化锌镉颗粒均匀分布在被还原的氧化石墨烯片层表面。图2所示是二氧化钛(TiO2),硫化锌镉(Zn0.5Cd0.5S)和二氧化钛和硫化锌镉气凝胶(TSGA)的XRD图谱,可以看出二氧化钛和硫化锌镉的衍射峰均出现在二氧化钛/硫化锌镉气凝胶的XRD图谱中,并且在15°附近出现一个宽峰,说明氧化石墨烯被还原,并且二氧化钛和硫化锌镉被成功负载到被还原得氧化石墨烯片层上。图3是三种材料的XPS图谱,也证明了二氧化钛/硫化锌镉气凝胶被成功合成。
将本实施例制备的二氧化钛/硫化锌镉气凝胶应用于溶液中六价铬的去除,具体步骤为:
(1)称取二氧化钛/硫化锌镉石墨烯气凝胶40mg加入50mL50mg/LpH 2.0的六价铬溶液中;
(2)在暗环境中震荡40min,吸附平衡时取一定量溶液经滤膜进行固液分离,测定分离后所得溶液的中剩余六价铬离子含量;
(3)再将该反应体系在氙灯(λ>420nm)照射下进行光催化反应,光照60min反应结束后测定溶液中剩余六价铬离子含量。
去除效果如图4所示,可以看出本实施例制备的二氧化钛/硫化锌镉气凝胶在吸附和光催化协同作用下对六价铬有良好的去除效果。
吸附及光催化后材料的XRD图谱对比如图5所示,可以看出,在吸附及光催化反应之后,材料的晶型并未发生变化。吸附及光催化后材料的XPS图谱对比如图6所示,可以看出在吸附及光催化反应之后材料的基本组成成分并未发生变化,所制备的二氧化钛/硫化锌镉气凝胶具有良好的稳定性。
实施例2
将实施例1中的二氧化钛与硫化锌镉的比例变成1:4,其他条件不变。
实施例3
将实施例1中的二氧化钛与硫化锌镉的比例变成1:2,其他条件不变。
实施例4
将实施例1中的二氧化钛与硫化锌镉的比例变成2:1,其他条件不变。
实施例5
将实施例1中的二氧化钛与硫化锌镉的比例变成4:1,其他条件不变。
实施例6
测试1
对不同溶液初始pH条件下二氧化钛/硫化锌镉石墨烯气凝胶对六价铬的去除效果进行对比,具体步骤为:
(1)分别配制pH为1.5,2.0,3.0,4.0,5.0,6.0,7.0,8.0的六价铬溶液,其浓度均为50mg/L;
(2)称取实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶40mg分别加入50mL步骤(1)配制的六价铬溶液中;
(3)在暗环境中震荡40min,每隔10min取一定量溶液经滤膜进行固液分离,测定分离后所得溶液的中剩余六价铬离子含量;
(4)再将该反应体系在氙灯(λ>420nm)照射下进行光催化反应,分别在10,20,30,40,60,80和100min测定溶液中剩余六价铬离子含量。
测试结果如图7所示,随着pH的增大,二氧化钛/硫化锌镉石墨烯气凝胶材料对六价铬的吸附能力逐渐减弱,表明在酸性条件下有利于吸附过程,光催化能力也随着pH的增大而减弱,为了使材料保持部分活性位点,2.0是较为理想的pH条件。
测试2
对不同二氧化钛/硫化锌镉石墨烯气凝胶投加量条件下溶液中六价铬去除效果进行对比,具体步骤为:
(1)分别称取实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶10,20,30,40和50mg加入50mL的pH为2.0的六价铬溶液中;
(2)在暗环境中震荡40min,每隔10min取一定量溶液经滤膜进行固液分离,测定分离后所得溶液的中剩余六价铬离子含量;
(3)再将该反应体系在氙灯(λ>420nm)照射下进行光催化反应,分别在10,20,30,40,60,80和100min测定溶液中剩余六价铬离子含量。
测试结果如图8所示,随着材料投加量的增加,其对六价铬的吸附和光催化性能均有所提升,当投加量增加50mg时去除六价铬的效率比40mg增加并不明显,因此该测试中二氧化钛/硫化锌镉石墨烯气凝胶的投加量以40mg(即0.8g/L)为宜。
测试3
对二氧化钛/硫化锌镉石墨烯气凝胶对不同初始浓度溶液中六价铬去除效果进行对比,具体步骤为:
(1)分别配制浓度为25,50,75和100mg/L的六价铬溶液;
(2)称取实施例1制备的二氧化钛/硫化锌镉石墨烯气凝胶40mg分别加入50mL步骤(1)配制的pH为2.0的六价铬溶液中;
(3)在暗环境中震荡40min,每隔10min取一定量溶液经滤膜进行固液分离,测定分离后所得溶液的中剩余六价铬离子含量;
(4)再将该反应体系在氙灯(λ>420nm)照射下进行光催化反应,分别在10,20,30,40,60,80和100min测定溶液中剩余六价铬离子含量。
测试结果如图9所示,二氧化钛/硫化锌镉石墨烯气凝胶对高浓度和低浓度的六价铬均有较好的去除效果。
测试4
对二氧化钛/硫化锌镉石墨烯气凝胶循环利用效果的测试,具体步骤如下:
(1)将测试(1)中pH为2.0体系中的材料通过过滤分离,在60℃真空干燥箱中烘干2h得到再生的材料;
(2)称取40mg步骤(1)的材料加入到50mL 50mg/L,pH为2.0的六价铬溶液中,按照测试(1)中步骤(3)(4)进行操作;
(3)共重复以上操作4次。
测试结果如图10所示,可以看出经过5次循环之后,二氧化钛/硫化锌镉石墨烯气凝胶已然对六价铬有较高的去除能力,说明该材料具有良好的循环利用性能。
以上所致,仅是本发明较佳实施例,并非对本发明作任何形式上的限制。任何熟悉本领域的技术人员,在不脱离本发明的精神实质和技术方案的情况之下,可利用所述发放和技术内容对本发明的技术方案做出合理的变动和修饰,或修改为等同变化的等效实施例。因此,凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所做的简单修改或等效替换,均仍属于本发明技术方案保护的范围之内。
Claims (10)
1.一种二氧化钛/硫化锌镉石墨烯气凝胶的制备方法,其特征在于,包括以下步骤:
(1)将氧化石墨烯溶液加入到乙醇水溶液中进行超声处理,得氧化石墨烯分散液;
(2)将二氧化钛和硫化锌镉纳米颗粒分别在超声条件下分散到无水乙醇中,再将两种分散液在搅拌条件下加入步骤(1)所得氧化石墨烯分散液中,继续搅拌得到均匀悬浮液;
(3)在搅拌条件下向步骤(2)所得的悬浮液中分别加入丙烯酰胺、N,N-亚甲基双丙烯酰胺和过硫酸铵,继续搅拌得到分散均匀的混合物;
(4)将步骤(3)所得混合物转移到水热反应釜中,经高温反应后,得到二氧化钛/硫化锌镉石墨烯水凝胶;
(5)将步骤(4)所得二氧化钛/硫化锌镉石墨烯水凝胶多次洗涤后进行冷冻干燥,得到二氧化钛/硫化锌镉石墨烯气凝胶。
2.根据权利要求1所述二氧化钛/硫化锌镉石墨烯气凝胶的制备方法,其特征在于,步骤(1)中,所述氧化石墨烯溶液的浓度0.5~1.0g/L,所述乙醇水溶液中乙醇与水的体积比为1:1~1:4,所得氧化石墨烯分散液浓度为0.3~0.5 g/L,所述超声处理的时间为45~60 min。
3.根据权利要求1所述二氧化钛/硫化锌镉石墨烯气凝胶的制备方法,其特征在于,步骤(2)中,所述二氧化钛的加入量为0.5~2.0 mmol;所述硫化锌镉的加入量为0.5~2.0mmol,所述超声处理时间为20~30 min,所述搅拌时间为30~45 min。
4.根据权利要求1所述的制备方法,其特征在于,所述硫化锌镉纳米颗粒的制备方法为:将2.5~5mmol的醋酸锌和2.5~5mmol的醋酸镉同时溶入5~10 mL去离子水中得溶液A;将5~10 mmol硫脲溶于30~40mL乙醇水溶液中得溶液B,将溶液A加入溶液B中,将混合溶液超声处理30~60min使其完全混匀,将其转移到50 mL的水热釜中,在160~200℃下反应10~18h,待冷却至室温,用去离子水和乙醇多次洗涤后在60~80℃烘箱中干燥12 h~24 h得到硫化锌镉纳米颗粒;所述乙醇水溶液中乙醇与水的体积比为1:1~1:4。
5.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,所述丙烯酰胺的投加量为20~50 mg,N,N-亚甲基双丙烯酰胺的投加量为20~50 mg,过硫酸铵的投加量为3~8 mg,所述搅拌时间为1~2 h;步骤(4)中,反应温度为120~180℃,反应时间为3~5h。
6.根据权利要求1所述的制备方法,其特征在于,步骤(5)中,所述冷冻干燥温度为-50~-80℃,时间为36~48 h。
7.由权利要求1~6任一项所述的制备方法制得的一种二氧化钛/硫化锌镉石墨烯气凝胶,其特征在于,所述二氧化钛/硫化锌镉石墨烯气凝胶具有三维网络结构,二氧化钛和硫化锌镉颗粒分布于被还原的氧化石墨烯片层上,形成了异质结构。
8.权利要求7所述的一种二氧化钛/硫化锌镉石墨烯气凝胶作为吸附剂和光催化剂应用于含六价铬废水的处理中。
9.根据权利要求8所述的应用,其特征在于,包括以下步骤:
将二氧化钛/硫化锌镉石墨烯气凝胶加入含六价铬的水溶液中,在暗环境中震荡至吸附平衡后,取溶液经滤膜进行固液分离,测定分离后所得溶液的中剩余六价铬离子含量;再将该反应体系在可见光照射下进行光催化反应,反应结束后测定溶液中剩余六价铬离子含量。
10.根据权利要求9所述的应用,其特征在于,二氧化钛/硫化锌镉石墨烯气凝胶的投加量为0.1~1.0g/L; 所述的吸附时间为40~60 min,光催化时间为30~60 min;所述光催化反应的反应温度为25±2℃,反应的pH为1.5~8.0。
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