CN113353932A - 火龙果皮制备的分级孔生物炭电催化剂及制备方法和应用 - Google Patents
火龙果皮制备的分级孔生物炭电催化剂及制备方法和应用 Download PDFInfo
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Abstract
本发明公开了火龙果皮制备的分级孔生物炭电催化剂及制备方法和应用;用火龙果皮制备分级孔生物炭电催化剂的方法,其特征在于:该方法包括如下步骤:1)将火龙果皮洗净后在烘箱中干燥;2)在惰性气氛下,将干燥后的火龙果皮在高温炉中碳化,并将碳化后的火龙果皮研磨成碳粉;3)将碳粉与KOH按照一定的质量比混合,并加入适量醇水溶液,超声震荡形成均匀的悬浮液;4)将悬浮液烘干后,收集固体碳材料,在惰性气氛下,将固体碳材料放入管式炉中进行退火;5)取出退火后的固体碳材料用去离子水洗至中性,然后用适量酸性溶液清洗,再用去离子水洗至中性,烘干后得到分级孔生物炭电催化剂;本发明可广泛应用于纺织、化工、食品、环保等领域。
Description
技术领域
本发明涉及分级孔生物炭电催化剂领域,具体地涉及火龙果皮制备的分级孔生物炭电催化剂及制备方法和应用。
背景技术
随着我国国民经济的快速发展,高浓度的有机废水对我国宝贵的水资源造成了极大威胁。然而利用现有的生物处理方法,对可生化性差、相对分子质量从几千到几万的物质处理较困难,采用混凝、电混凝和吸附等物理分离方法,虽然分离污染物的效果较好,但是存在吸附剂再生困难,污染物仍需进一步处理等问题,因此研究者们一直在寻求一种能高效降解水中大分子污染物的方法。近年来,利用羟基自由基(·OH)强氧化性快速降解大分子污染物的特点而发展起来的高级氧化法(AOPs)受到人们越来越多的关注,其能够使绝大部分有机物完全矿化或分解为低毒或无毒的小分子物质,具有非常广阔的应用前景。
AOPs根据产生自由基的方式和反应条件的不同,可将其分为光化学氧化、催化湿式氧化、声化学氧化、臭氧氧化、电化学氧化、芬顿氧化等。其中,芬顿氧化法相对于其他几种方法,其原理是利用Fe2+与H2O2反应生成·OH,所受局限最小,特别适用于生物难降解或一般化学氧化难以奏效的有机废水如垃圾渗滤液的氧化处理。芬顿氧化法处理污染物的影响因素主要就是H2O2和亚铁盐的投加量。但是亚铁离子的不稳定性会影响其降解效率,同时对于污染物处理量大的场景所需的H2O2的量也很大。基于芬顿法而演化出来的电芬顿法,其结合电化学原理,不仅可以实现原位H2O2合成,还可以实现亚铁离子的再生,发展潜力更大。
对于电芬顿过程,H2O2产率是影响其降解效率最关键的因素。H2O2电化学合成也是目前的研究热点,其涉及到氧气的两电子选择性还原,核心点在于找到一种具有高选择性,高电化学活性的两电子氧还原催化剂。从目前已有文献的报道来看,活性和选择性极佳的贵金属(如Pt,Au和Pd)及其合金(如Pt-Hg和Au-Pd)的稀缺性和高成本限制了其大规模应用。与贵金属相比,纯的非贵金属(如Fe,Cu和Ni)性能又较差,因此需要成本低、性能优的新型材料。
发明内容
本发明所需要解决的技术问题在于火龙果皮制备的分级孔生物炭电催化剂及制备方法和应用。
本发明的技术方案是,用火龙果皮制备分级孔生物炭电催化剂的方法,其特征在于:该方法包括如下步骤:
1)将火龙果皮洗净后在烘箱中干燥;
2)在惰性气氛下,将干燥后的火龙果皮在高温炉中碳化,并将碳化后的火龙果皮研磨成碳粉;
3)将碳粉与KOH按照一定的质量比混合,并加入适量醇水溶液,超声震荡形成均匀的悬浮液;
4)将悬浮液烘干后,收集固体碳材料,在惰性气氛下,将固体碳材料放入管式炉中进行退火;
5)取出退火后的固体碳材料用去离子水洗至中性,然后用适量酸性溶液清洗退火后的固体碳材料孔隙中的盐类及金属离子,再用去离子水洗至中性,烘干后得到分级孔生物炭电催化剂。
本发明将火龙果皮碳化为炭质材料,将炭质材料经过一定处理后,在中性或碱性环境下对两电子氧还原电化学生产H2O2展现出了优异的活性、选择性和稳定性,并且由于火龙果皮来源广泛、成本低廉,炭质材料导电性好,因此具有巨大的应用前景。并且生物炭材料还具有储量丰富、比表面积高、结构多样、环保、物理/化学性质可调控等一系列优势,是研制纳米炭质催化剂的理想原料,本发明对火龙果皮改性,以增强其对电化学合成H2O2的选择性。
本发明活化机理为:KOH和碳反应生成含钾化合物如K2CO3,K2O等,从而对炭材料进行刻蚀,得到孔结构;中间产物H2O和CO2能和碳进一步反应,获得孔结构;生成的钾能够在活化过程中有效地插入炭基体的炭晶格中,导致炭晶格的膨胀,得到孔。最后,再通过酸洗除掉材料表面及孔隙中的盐和碱,就能够得到具有发达孔隙的分级孔生物炭电催化剂,
本发明利用KOH活化机理,提出了一种简易且低成本的火龙果皮制备的分级孔生物炭电催化剂及制备方法,采用火龙果皮这种常见生活废弃物为原料,以KOH为活化剂,通过简单的管式炉退火制备得到一种用于高效电芬顿的分级孔生物炭电催化剂。
本发明所述的用火龙果皮制备的分级孔生物炭电催化剂。
本发明所述的用火龙果皮制备的分级孔生物炭电催化剂的应用。
本发明所述的火龙果皮制备的分级孔生物炭电催化剂及制备方法和应用的有益效果是:
所制备的分级孔生物炭电催化剂具有优异的电芬顿性能,原材料来源广泛、成本低廉、环保、可利用电芬顿原理处理废水,可广泛应用于纺织、化工、食品、环保等领域。
附图说明
图1是分级孔生物炭电催化剂的SEM图。
图2是分级孔生物炭电催化剂的TEM图。
图3是分级孔生物炭电催化剂在70mA/cm2电流密度下的H2O2产量及电流效率。
图4污染物经过不同降解时间的含量及去除率。
图5经过不同降解时间的污染物溶液中有机碳(TOC)含量及去除率。
具体实施方式
下面结合试验例及具体实施方式对本发明作进一步的详细描述。
实施例1,用火龙果皮制备分级孔生物炭电催化剂的方法,该方法包括如下步骤:
1)将火龙果皮洗净后在烘箱中干燥。
2)在惰性气氛如氮气、氩气等气氛下,将干燥后的火龙果皮在400℃左右的高温管式炉中碳化,管式炉碳化过程中,管式炉的升温速率为5℃/min,N2气流速率为40~60sccm,保温时间为2h。并将碳化后的火龙果皮研磨成碳粉。
3)将碳粉与KOH按照一定的质量比混合,并加入适量甲醇、乙醇或异丙醇等水溶液,超声震荡形成均匀的悬浮液。
4)将悬浮液烘干后,收集固体碳材料,在惰性气氛下,将固体碳材料放入管式炉中进行退火;
5)取出退火后的固体碳材料用去离子水洗至中性,然后用适量酸性溶液如HCl、H2SO4等清洗退火后的固体碳材料孔隙中的盐类及金属离子,再用去离子水洗至中性,烘干后得到分级孔生物炭电催化剂。
分级孔生物炭电催化剂扫描电镜图和场发射透射电镜图分别如图1、图2所示,从图中明显看出其具有高度多孔结构,而且大孔、介孔、微孔都存在,具有明显的分级多孔特性。
实施例2:
将实施例1制备的分级孔生物炭电催化剂、乙醇和全氟磺酸膜溶液配制成均相催化剂浆料,将该催化剂浆料喷涂至具有气体扩散层的碳基底材料上作为电解池阴极;以涂覆有氧化铱的商业钛板作为电解池阳极,搭建单室反应器。电解液为Na2SO4与FeSO4的混合溶液。阴阳极间距为2cm。用直流稳压电源控制电流密度为70mA/cm2,测量H2O2 60min产量为623.29mg/L,60min电流效率为70.17%,如图3所示。从图3可以看出,即使在70mA/cm2的高电流密度下,其电流效率依旧维持在一个较高的水平,说明本发明制备的分级孔生物炭质催化剂具有非常优异的产H2O2性能。其中,电解时的H2O2产量是利用草酸钛钾与H2O2生成橙色络合物在400nm紫外分光光度计中的吸光度换算得到。
实施例3:
将实施例2中的电解液分别换成100mg/L的罗丹明B(RhB)、亚甲基蓝(MB)和酸性橙7(AO7)等污染物溶液,其中电解液中FeSO4浓度均为0.5mmol/L,Na2SO4浓度仍为0.05mol/L。将开始通电的时刻记为0min,分别在5、10、15、20、30、40min测量污染物的降解情况,经过40min的降解,罗丹明B,亚甲基蓝和酸性橙7的含量分别为0.26mg/L,4.13mg/L,0.82mg/L,去除率分别为99.74%,95.87%,99.18%,如图4所示。说明本发明制备的分级孔生物炭电催化剂的H2O2产量可满足不同的高浓度污染物的快速降解需求。
实施例4:
将实施例2中的电解液分别换成100mg/L的罗丹明B(RhB),亚甲基蓝(MB)和酸性橙7(AO7)等污染物溶液,其中电解液中FeSO4浓度均为0.5mmol/L,Na2SO4浓度仍为0.05mol/L,将开始通电的时刻记为0min,经过40min降解,分别在降解了0min、40min的时候取6mL溶液,进行总有机碳(TOC)测量,罗丹明B,亚甲基蓝和酸性橙7在0min的TOC为49.9mg/L,56.49mg/L,43.19mg/L,在40min的TOC为13.2mg/L,19.51mg/L,11.8mg/L。其去除率为73.55%,65.46%,72.68%,如图5所示,说明本发明制备的分级孔生物炭电催化剂的H2O2产量可满足有机物快速降解的需求。
从实施例2-4可以看出,本发明用火龙果皮制备的分级孔生物炭电催化剂不仅具有高的H2O2产量,还有优异的电芬顿性能。H2O2产量可满足有机物快速降解的需求。并且通过实验发现,只需在由其所组成的单室反应器中加入极少量的亚铁盐就可以实现对多种高浓度污染物的快速降解。用火龙果皮制备的分级孔生物炭电催化剂具有极大的应用前景,特别是利用电芬顿电芬顿原理处理废水。
以上所述仅为本发明的优选实施例,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.用火龙果皮制备分级孔生物炭电催化剂的方法,其特征在于:该方法包括如下步骤:
1)将火龙果皮洗净后在烘箱中干燥;
2)在惰性气氛下,将干燥后的火龙果皮在高温炉中碳化,并将碳化后的火龙果皮研磨成碳粉;
3)将碳粉与KOH按照一定的质量比混合,并加入适量醇水溶液,超声震荡形成均匀的悬浮液;
4)将悬浮液烘干后,收集固体碳材料,在惰性气氛下,将固体碳材料放入管式炉中进行退火;
5)取出退火后的固体碳材料用去离子水洗至中性,然后用适量酸性溶液清洗退火后的固体碳材料孔隙中的盐类及金属离子,再用去离子水洗至中性,烘干后得到分级孔生物炭电催化剂。
2.根据权利要求1所述的用火龙果皮制备的分级孔生物炭电催化剂。
3.根据权利要求1所述的用火龙果皮制备的分级孔生物炭电催化剂的应用。
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CN114293206A (zh) * | 2022-01-05 | 2022-04-08 | 哈尔滨工业大学 | 一种脉冲电合成h2o2的方法 |
CN115312326A (zh) * | 2022-04-20 | 2022-11-08 | 湖南和广生物科技有限公司 | 一种基于山茶果皮制备超级电容器电极材料的方法 |
CN115124036A (zh) * | 2022-06-24 | 2022-09-30 | 闽西职业技术学院 | 用于废水中苯酚吸附的火龙果皮活性炭的制备方法 |
CN115920913A (zh) * | 2022-10-18 | 2023-04-07 | 江苏爱柯道环保工程科技有限公司 | 一种脂改性微疏水电催化材料及其制备方法和应用 |
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