CN114014411B - 一种用于处理喷涂废水的高活性三维粒子电极材料及其制备方法 - Google Patents
一种用于处理喷涂废水的高活性三维粒子电极材料及其制备方法 Download PDFInfo
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Abstract
本发明提供一种用于处理喷涂废水的高活性三维粒子电极材料,包括铁精粉(45~65wt.%)、活性炭(20~40wt.%)、配方催化剂(5~15wt.%)、辅料成分(5~10wt.%),所述高活性三维粒子电极材料为球形蜂窝多微孔结构的圆球,直径为8‑18mm,在20℃时电阻率在20~200mΩ·cm之间;将废旧压电陶瓷压制成200~400目的细微粉末,更小的粒径,基本上处于无定形态因而具有更高的表面活性,纳米至微米级催化剂具有更大的比表面积,有效提高了电化学效率,处理效果得到显著改善,更好的分散性,更易于在最终产品中均匀分布。
Description
技术领域
本发明涉及废水处理材料技术领域,具体涉及为一种用于处理喷涂废水的高活性三维粒子电极材料及其制备方法。
背景技术
喷涂废水是在制造业喷漆处理工序中产生的一种工业废水,其中含有大量的悬浮物和难以生物降解有机物污染物。喷涂废水一旦直接排到环境中,很难被分解,在水体、土壤等环境介质中长期滞留。另外,废水中含有难降解性有机物,一般具有低水溶性、高脂溶性的特征,能够在多数生物脂肪中发生生物蓄积,而且有的难降解性有机物具有半挥发性,可以在大气环境中远距离迁移,它们对人和动物一般具有毒性作用,有的可以导致生物体内分泌紊乱生殖及免疫机能失调,有的甚至引起癌症等严重疾病。因此,我们必须对废水进行处理达标后排放。
三维电极催化氧化技术是处理高浓度有机废水的一种工艺,通过三维电极和电芬顿方法的复合,组成催化粒子氧化***,也称粒子电极法。粒子电极法是针对传统的双电极法进行的改进方法,具体是指在传统的二维电解电极间填充粒状电极材料,使之带电,并在材料表面发生电化学反应的电化学处理方法。采用粒子电极法,使用高频脉冲电源,在反应器中的电极上施加脉冲电压,实现三维电极、电催化氧化和微电解三种作用体系的联合。反应过程集氧化还原、絮凝吸附、催化氧化及沉积等作用为一体。外加电场提供高频脉冲电压0-15V,电极产生OH,利用其强氧化性氧化有机物及络合物,降解废水中的有机物。
传统三维粒子材料采用高温烧结,在烧制的原料中加入催化剂的方法或者产品相对较少。而在其中加入催化剂时,大部分是直接使用商品金属氧化物。这种商品金属氧化物的结晶较好,粒径相对较大,其比表面积相对较低,因而催化活性低。
发明内容
为解决上述技术问题,本发明提供一种用于处理喷涂废水的高活性三维粒子电极材料及其制备方法,具体的技术方案为:
一种用于处理喷涂废水的高活性三维粒子电极材料,包括铁精粉(45~65wt.%)、活性炭(20~40wt.%)、配方催化剂(5~15wt.%)、辅料成分(5~10wt.%),所述高活性三维粒子电极材料为球形蜂窝多微孔结构的圆球,直径为8-18mm,在20℃时电阻率在20~200mΩ·cm之间。
进一步地,所述配方催化剂使用纳米级或微米级材料。
进一步地,所述配方催化剂为含有氧化锆、二氧化钛过渡金属的压电陶瓷提取物。
进一步地,所述配方催化剂是以废旧的压电陶瓷为主要成分的复合物且压制成200~400目的细微粉末。
进一步地,所述铁精粉与活性炭摩尔比为1:1。
一种用于处理喷涂废水的高活性三维粒子电极材料的制备方法,包括如下步骤:
S1、将铁精粉、活性炭、配方催化剂、辅料成分分别磨碎,过200-400目筛;
S2、按配方称取各组分,经过球磨混合均匀后造粒成直径为8-18mm的圆球,并将其在120℃干燥2h,制得球形料;
S3、将步骤S2制得的球形料进行装罐,并在还原气氛中加热至1000-1100℃,加热烧结成型,制得罐装三维粒子电极材料材料;
S4、将步骤S3制得的罐装铁碳材料冷却出罐,去除罐体,即得三维粒子电极材料。
进一步地,所述配方催化剂的制备方法包括如下步骤:
S01、选用废旧压电陶瓷,经过多级磨碎,过200-400目筛;再采用压电陶瓷粉末质量5倍的硝酸溶解提纯,提取的溶液制成硝酸盐M;
S02、将步骤S01制得的硝酸盐M溶于水,为提高其稳定性,再加入固体有机酸配置成溶液N;
S03、将步骤S02制得的溶液N在80-120℃蒸发干燥,得到干态物质O;
S04、将步骤S03制得的干态物质O在400-800℃煅烧100-150min,得到物质P;
S05、将步骤S04制得的物质P研磨至纳米级粉末,即得物质Q,即配方催化剂。
本发明地有益效果
1、更小的粒径,制成的高活性三维粒子电极材料材料为直径8-18mm的圆球,基本上处于无定形态因而具有更高的表面活性。纳米至微米级催化剂具有更大的比表面积,有效提高了电化学效率,处理效果得到显著改善,更好的分散性,更易于在最终产品中均匀分布。纳米至微米级材料可以被三维粒子电极材料材料中的活性炭吸附,使材料中的活性炭作为催化剂的吸附载体,因而可以进一步提高催化剂的活性;
2、变废为宝,综合利用。添加有废旧压电陶瓷粉末提取物的催化剂材料,含有大量氧化锆、二氧化钛等过渡金属,同时在辅料成分中适量加入压电陶瓷粉末调节导电的电阻,且电阻率在20℃时约在20~200mΩ·cm之间,提高增加了催化剂的反应活性点,提升了反应效率,最终制得的三维粒子电极材料产品具有更好的污水处理效果。
附图说明
图1为本发明制备的工艺流程图。
图2为本发明的应用效果示意图。
图中:1、高活性三维粒子电极材料;2、曝气。
具体实施方式
下面将结合本发明中的图1与图2,其中图1为本发明制备的工艺流程图;图2为本发明的应用效果示意图。对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
一种用于处理喷涂废水的高活性三维粒子电极材料,由铁精粉(45~65wt.%)、活性炭(20~40wt.%)、配方催化剂(5~15wt.%)、辅料成分(5~10wt.%)组成,所述高活性三维粒子电极材料1为球形蜂窝多微孔结构,有利于使用过程中提高布水和布气的均匀性,从而提高材料表面积,提高多相反应传质效率,从而提高反应速度和处理效率;采用等摩尔技术来控制复合材料组分比例,使得所述铁精粉与活性炭摩尔比为1:1时,三维电极微粒形成的电极对数量最大,反应速度最快,所述配方催化剂使用的是纳米级或者微米级材料,所述配方催化剂原料为含有氧化锆和二氧化钛等过渡金属氧化物的废旧压电陶瓷且压制成200~400目的细微粉末的提取物,利用过渡元素的活性,同时在辅料成分中适量加入压电陶瓷粉末用以调节导电的电阻,增强催化反应活性,提升废水处理效率,让废旧压电陶瓷变废为宝。
如图1所示,一种用于处理喷涂废水的高活性三维粒子电极材料的制备方法,包括如下步骤:
S1:将铁精粉、活性炭、配方催化剂、辅料成分分别磨碎,过200-400目筛;
S2、按配方称取各组分,经过球磨混合均匀后造粒成直径为8-18mm的圆球,并将其在120℃干燥2h,制得球形料;
S3、将步骤S2制得的球形料进行装罐,并在还原气氛中加热至1000-1100℃,加热烧结成型,制得罐装三维粒子电极材料材料;
S4、将步骤S3制得的罐装铁碳材料冷却出罐,去除罐体,即得。
所述配方催化剂的制备方法包括如下步骤:
S01选用废旧压电陶瓷,经过多级磨碎,过200-400目筛;再采用压电陶瓷粉末质量5倍的硝酸溶解提纯,提取的溶液制成硝酸盐M;
S02将步骤S01制得的硝酸盐M溶于水,为提高其稳定性,再加入固体有机酸配置成溶液N;
S03将步骤S02制得的溶液N在80-120℃蒸发干燥,得到干态物质O;
S04将步骤S03制得的干态物质O在400-800℃煅烧100-150min,得到物质P;
S05将步骤S04制得的物质P研磨至纳米级粉末,即得物质Q。
本发明通过相关实施例进一步说明了本发明的创造性,具体实施效果图如图2所示。
实施例1:
实验例1:
(1)取调节池中废水试验,测定COD,计算COD去除率。
(2)采用三维电极催化氧化技术,使用新型的高活性三维粒子电极材料1作为催化剂,调节ph值5-6进水,反应2h后中和延时曝气2,混凝沉淀取上层清夜,观察其颜色及气味,测定其COD,并计算COD去除率。
实验结果见表1:
表1
结果表明:喷涂废水原水经过使用新型高活性粒子电极1作为催化剂的三维电极催化氧化技术,COD可从7930降至3090,去除率可达61%,颜色气味呈无色轻微刺鼻状态。
实验例2:
(1)取调节池中废水试验,测定COD,计算COD去除率。
(2)采用三维电极催化氧化技术,使用我司旧粒子电极1材料,调节ph值5-6进水,反应2h后中和延时曝气2,混凝沉淀取上层清夜,观察其颜色及气味,测定其COD,并计算COD去除率。
实验结果见表2
表2
结果表明:喷涂废水原水经过使用我司旧型粒子电极1作为催化剂的三维电极催化氧化技术,COD从7930降至4520,去除率为43%,与实验例1进行对比,相同条件下,新型粒子电极1去除COD的效率比旧型粒子电极1更高,脱色效果也更好。
实验例3:
(1)取调节池中废水试验,测定COD,计算COD去除率。
(2)采用传统二维电解技术,不使用粒子电极1材料,调节ph值5-6进水,反应2h后中和延时曝气2,混凝沉淀取上层清夜,观察其颜色及气味,测定其COD,并计算COD去除率。
实验结果见表3
表3
结果表明:喷涂废水原水经过无催化剂的二维电解技术,COD从7930降至5700,去除率为28.1%,与实验例1和实验例2进行对比,相同条件下,采用无粒子电极1的二维电解技术COD去除效率较低,脱色脱味效果较差。
通过实验例1,实验例2和实验例3的对比实验,总结出采用实验1的新型高活性三维粒子电极材料1作为催化剂的三维电极催化氧化技术,对喷涂废水的COD,颜色,气味的去除效率最高。
对比例1:
在实验例1中,将高活性球形三维粒子电极材料材料由粒径8-18mm换成4-8mm的圆球颗粒,其它条件不变。测定其COD,并计算COD去除率。
对比例2:
在实验例1中,将高活性球形三维粒子电极材料材料由粒径8-18mm换成18-22mm的圆球颗粒,其它条件不变。测定其COD,并计算COD去除率。
对比例3:
在实验例1中,将高活性球形三维粒子电极材料材料由电阻率在20~200mΩ·cm之间材料换成电阻率在200~500mΩ·cm的材料,其它条件不变。测定其COD,并计算COD去除率。
对比例4:
在实验例1中,将高活性球形三维粒子电极材料材料由电阻率在20~200mΩ·cm之间材料换成电阻率在1~20mΩ·cm的材料,其它条件不变。测定其COD,并计算COD去除率。
检测结果见表4
表4
通过对比例1,对比例2、对比例3和对比例4的对比实验,总结出本发明的新型高活性三维粒子采用粒径8-18mm以及电阻率在20~200mΩ·cm的材料,对喷涂废水的COD,颜色,气味的去除效率最高
本发明通过添加以废旧压电陶瓷粉末的催化剂材料,利用过渡的性质,调节导电的电阻,提升反应效率,同时将废旧压电陶瓷有效利用,因而将电力行业发展所产生的废旧压电陶瓷变废为宝,为把国家早日建设成环保型社会出一份力量。以上所述仅是本发明的优选实施方式,其描述较为具体和详细,但并不能因此理解为对发明专利范围的限制,应当指出的是,在不脱离本发明构思的前提下,还可以做出若干改进以及变形,这些都属于本发明的保护范围。
Claims (4)
1.一种用于处理喷涂废水的高活性三维粒子电极材料,其特征在于,包括45~65wt%铁精粉、20~40wt%活性炭、5~15wt%配方催化剂、5~10wt%辅料成分,所述高活性三维粒子电极材料为球形蜂窝多微孔结构的圆球,直径为8-18mm,在20℃时电阻率在20~200mΩ·cm之间,所述配方催化剂使用纳米级或微米级材料,所述配方催化剂为含有氧化锆、二氧化钛过渡金属的压电陶瓷提取物。
2.根据权利要求1所述的一种用于处理喷涂废水的高活性三维粒子电极材料,其特征在于:所述配方催化剂是以废旧的压电陶瓷为主要成分的复合物且制成200~400目的细微粉末。
3.根据权利要求1所述的一种用于处理喷涂废水的高活性三维粒子电极材料,其特征在于:所述铁精粉与活性炭摩尔比为1:1。
4.一种如权利要求1所述的用于处理喷涂废水的高活性三维粒子电极材料的制备方法,其特征在于,包括如下步骤:
S1、将铁精粉、活性炭、配方催化剂、辅料成分分别磨碎,过200-400目筛;所述配方催化剂的制备方法包括如下步骤:
S01、选用废旧压电陶瓷,经过多级磨碎,过200-400目筛;再采用压电陶瓷粉末质量5倍的硝酸溶解提纯,提取的溶液制成硝酸盐M;
S02、将步骤S01制得的硝酸盐M溶于水,为提高其稳定性,再加入固体有机酸配置成溶液N;
S03、将步骤S02制得的溶液N在80-120℃蒸发干燥,得到干态物质O;
S04、将步骤S03制得的干态物质O在400-800℃煅烧100-150min,得到物质P;
S05、将步骤S04制得的物质P研磨至纳米级粉末,即得物质Q,即配方催化剂;
S2、按配方称取各组分,经过球磨混合均匀后造粒成直径为8-18mm的圆球,并将其在120℃干燥2h,制得球形料;
S3、将步骤S2制得的球形料进行装罐,并在还原气氛中加热至1000-1100℃,加热烧结成型,制得罐装三维粒子电极材料;
S4、将步骤S3制得的罐装三维粒子电极材料冷却出罐,去除罐体,即得三维粒子电极材料。
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