CN110252355B - 一种处理有机废水的光催化剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种处理有机废水的光催化剂及其制备方法。所述的光催化剂的通式为Li0.1NiCoPSi4O12.6。该方法是将原料硝酸锂、硫酸镍、硝酸钴和磷酸氢二铵在常温常压下完全溶解在水中,在搅拌下滴加硅酸四乙酯,滴加完毕后,继续搅拌直至生成凝胶,然后将烘干凝胶并研磨成粉末,经煅烧后获得通式Li0.1NiCoPSi4O12.6的催化剂粉体,所制得的催化剂在光照射下能有效地降解废水中的亚甲基蓝染料。本发明光催化剂的制备方法简单,在常温常压下具有催化降解效率高,工艺流程简单,无二次污染产生,并且运行费用低等特点,有很高的实际应用价值。
Description
技术领域
本发明涉及到无机功能材料制备技术领域,特别涉及到一种处理有机废水的光催化剂及其制备方法。
背景技术
目前有机染料废水已经成为主要的水体污染源之一。该废水具有水量大、浓度高、成分复杂、色度深和难降解等特点。大多数染料具有毒性、致癌性、致畸和致突变的作用。亚甲基蓝是一种重要的有机化学合成阳离子染料,工业应用非常广泛。例如,可应用于麻、蚕丝织物、纸张的染色及竹、木的着色,应用于生物、细菌组织的染色以及应用于制造墨水和色淀等。亚甲基蓝在工业上的广泛应用导致含亚甲基蓝染料废水对水体的严重污染。目前有机染料废水的处理方法主要有生物法、混凝法、高级氧化技术、光催化法、吸附法及膜分离法等。生物法受pH值、温度、盐份和染料种类等因素的影响,使得生物法处理的效果不够理想。混凝法的运行费用较高,泥渣量大而且脱水困难,适用的pH值范围窄。高级氧化技术成本高,常用氧化剂也会表现出氧化能力不强、存在选择性氧化等缺点,而且处理过程中容易引入杂质造成二次污染。膜分离法的成本较高,操作压力较大,造成膜法的能耗偏高。
近年来,利用半导体材料光催化降解有毒有害的污染物已成为重要的研究方向。光催化技术不仅能耗低、操作简便、反应条件温和、无二次污染,而且可有效地将有机污染物转化为无机小分子,达到完全无机化的目的。目前使用较多光催化剂是白色的TiO2,其具有光催化活性高、稳定性好的优点。然而TiO2的带隙较宽,只能吸收λ≤387nm的紫外光,太阳能的利用率低。因此,开发一种代替TiO2并且能简单高效处理亚甲基蓝染料废水的光催化剂具有重要的意义。
发明内容
本发明的目的在于解决现有技术中存在的上述技术问题,从而提供一种简单有效降解亚甲基蓝废水的光催化剂及其制备方法和应用。
为了实现上述目的,本发明的技术方案为:
一种处理有机废水的光催化剂,所述的光催化剂的通式为Li0.1NiCoPSi4O12.6。
一种处理有机废水的光催化剂的制备方法,所述方法按如下步骤进行:
1、制备凝胶:将原料硝酸锂、硫酸镍、硝酸钴和磷酸氢二铵在常温常压下完全溶解在水中,在搅拌下滴加硅酸四乙酯,滴加完毕后,继续搅拌直至生成凝胶;
2、制备催化剂粉体:将步骤1所获得的凝胶,在100℃−140℃温度下烘干并研磨成粉末,烘干的凝胶粉末放入马弗炉中,经煅烧后获得通式为Li0.1NiCoPSi4O12.6的催化剂粉体,所制得的催化剂在模拟阳光的氙灯照射下能有效地降解废水中的亚甲基蓝染料。
所述催化剂粉体中的锂元素、镍元素、钴元素、磷元素和硅元素的摩尔比为0.1:1:1:1:4。
所述方法中的煅烧是将凝胶粉末放入马弗炉中,在400℃− 900℃温度下煅烧5−15小时。
一种处理有机废水的光催化剂的使用方法,该方法将所制备的光催化剂粉体悬浮于亚甲基蓝染料废水中,在模拟阳光的氙灯光照射30-60 分钟进行处理。
一种处理有机废水的光催化剂的使用方法,按0.5-2.5g/L废水的比例加入所制备的光催化剂粉体,在搅拌下处理。
本发明的具体使用方法为:将亚甲基蓝染料有机废水引入圆柱形石英光催化反应器中,根据亚甲基蓝染料有机废水的浓度加入0.5−2g/L所制备的光催化剂粉体,再开启磁力搅拌器进行搅拌,使催化剂呈悬浮状态,然后接通氙灯光源,照射30-60分钟,利用光催化降解废水中的有机成分。所述氙灯置于石英冷阱内,该冷阱固定在圆柱形石英反应器中央,冷阱内的夹层中通有冷却水,通过调节冷却水的流量来消除氙灯的热效应。所述光源采用模拟太阳光谱的氙灯,在本发明中也可以用太阳光照射。
基于以上应用效果,本发明还提供了一种利用上述光催化剂处理亚甲基蓝染料有机废水的方法,其中该方法包括将所制备的光催化剂粉体悬浮于亚甲基蓝染料废水中氙灯光照射30−60 分钟进行处理。
与现有技术相比,本发明具有如下显著的优点和显著的进步:
1、本发明光催化剂的制备方法简单,在常温常压下具有催化降解效率高,工艺流程简单,无二次污染产生,并且运行费用低等特点,有很高的实际应用价值;
2、本发明制备的光催化剂粉体活性高,去除污染物效果显著,能在较短的时间内快速而且高效降解污染物;
3、本发明采用的有机废水处理方法在常温常压下即可进行,工艺流程简单和成本低;
4、本发明采用的废水处理方法处理有机废水后,最终将有机废水中的污染物降解成无机小分子物质,从而避免了二次污染的产生。
具体实施方式
以下通过实施例进一步对本发明的技术方案进行清楚、完整的描述。
实施例1
1、制备催化剂粉体:称取0.069g硝酸锂(即1.0×10-3mol),称取2.910g六水硝酸镍(即1.0×10-2mol),称取2.910g六水硝酸钴(即1.0×10-2mol),称取1.320g磷酸氢二铵(即1.1×10-2mol),将硝酸锂、六水硝酸镍、六水硝酸钴和磷酸氢二铵在常温常压下完全溶解在50mL水中,在搅拌下滴加8.91mL硅酸四乙酯,滴加完毕后,继续搅拌直至生成凝胶。然后140℃温度下烘干凝胶并研磨成粉末,将获得的凝胶粉末放入马弗炉中,在400℃温度下煅烧15小时后,获得通式为Li0.1NiCoPSi4O12.6的黑色催化剂粉体。
2、催化剂粉体的使用:将40 mL浓度为10.0 mg/L的亚甲基蓝染料有机废水加入圆柱形石英光催化反应器中,加入制备得到的催化剂粉体40 mg,磁力搅拌使光催化剂粉体一直处于悬浮状态,然后用300 W 氙灯照射60 分钟后,亚甲基蓝的降解率为90.10%。
实施例2
1、制备催化剂粉体:称取0.069g硝酸锂(即1.0×10-3mol),称取2.910g六水硝酸镍(即1.0×10-2mol),称取2.910g六水硝酸钴(即1.0×10-2mol),称取1.320g磷酸氢二铵(即1.1×10-2mol),将硝酸锂、六水硝酸镍、六水硝酸钴和磷酸氢二铵在常温常压下完全溶解在50mL水中,在搅拌下滴加8.91mL硅酸四乙酯,滴加完毕后,继续搅拌直至生成凝胶。然后130℃温度下烘干凝胶并研磨成粉末,将获得的凝胶粉末放入马弗炉中,在550℃温度下煅烧15小时后,获得通式为Li0.1NiCoPSi4O12.6的黑色催化剂粉体。
2、催化剂粉体的使用:将40 mL浓度为10.0 mg/L的亚甲基蓝染料有机废水加入圆柱形石英光催化反应器中,加入制备得到的催化剂粉体40 mg,磁力搅拌使光催化剂粉体一直处于悬浮状态,然后用300 W 氙灯照射40 分钟后,亚甲基蓝的降解率为94.50%。
实施例3
1、制备催化剂粉体:称取0.069g硝酸锂(即1.0×10-3mol),称取2.910g六水硝酸镍(即1.0×10-2mol),称取2.910g六水硝酸钴(即1.0×10-2mol),称取1.320g磷酸氢二铵(即1.1×10-2mol),将硝酸锂、六水硝酸镍、六水硝酸钴和磷酸氢二铵在常温常压下完全溶解在50mL水中,在搅拌下滴加8.91mL硅酸四乙酯,滴加完毕后,继续搅拌直至生成凝胶。然后120℃温度下烘干凝胶并研磨成粉末,将获得的凝胶粉末放入马弗炉中,在750℃温度下煅烧10小时后,获得通式为Li0.1NiCoPSi4O12.6的黑色催化剂粉体。
2、催化剂粉体的使用:将40 mL浓度为10.0 mg/L的亚甲基蓝染料有机废水加入圆柱形石英光催化反应器中,加入制备得到的催化剂粉体40 mg,磁力搅拌使光催化剂粉体一直处于悬浮状态,然后用300 W 氙灯照射30 分钟后,亚甲基蓝的降解率为94.45%。
实施例4
1、制备催化剂粉体:称取0.069g硝酸锂(即1.0×10-3mol),称取2.910g六水硝酸镍(即1.0×10-2mol),称取2.910g六水硝酸钴(即1.0×10-2mol),称取1.320g磷酸氢二铵(即1.1×10-2mol),将硝酸锂、六水硝酸镍、六水硝酸钴和磷酸氢二铵在常温常压下完全溶解在50mL水中,在搅拌下滴加8.91mL硅酸四乙酯,滴加完毕后,继续搅拌直至生成凝胶。然后100℃温度下烘干凝胶并研磨成粉末,将获得的凝胶粉末放入马弗炉中,在900℃温度下煅烧5小时后,获得通式为Li0.1NiCoPSi4O12.6的黑色催化剂粉体。
2、催化剂粉体的使用:将40 mL浓度为10.0 mg/L的亚甲基蓝染料有机废水加入圆柱形石英光催化反应器中,加入制备得到的催化剂粉体40 mg,磁力搅拌使光催化剂粉体一直处于悬浮状态,然后用300 W 氙灯照射30 分钟后,亚甲基蓝的降解率为94.62%。
本说明书中公开的所有特征,或公开的所有制备方法和应用,除了互相排斥的特征和/或步骤、应用以外,均可以以任何方式组合。本说明书(包括权利要求、摘要)中公开的任一特征,除非特别叙述,均可被其他等效或具有类似目的的替代特征加以替换。即除非特别叙述,每个特征只是一系列等效或类似特征中的一个例子而已。
以上所述仅是发明的非限定实施方式,还可以衍生出大量的实施例,对于本领域的普通技术人员来说,在不脱离本发明创造构思和不作出创造性劳动的前提下,还可以做出若干变形和改进的实施例,这些都属于本发明的保护范围。
Claims (1)
1.一种处理有机废水的光催化剂,其特征在于:所述光催化剂的通式为Li0.1NiCoPSi4O12.6,所述处理有机废水的光催化剂的使用方法为将光催化剂粉体悬浮于亚甲基蓝染料有机废水中,在模拟阳光的氙灯光照射30−60分钟进行处理;按0.5-2.5g/L废水的比例加入所制备的光催化剂粉体,在搅拌下处理;
所述的处理有机废水的光催化剂的制备方法按如下步骤进行:
(1)制备凝胶:将原料硝酸锂、硫酸镍、硝酸钴和磷酸氢二铵在常温常压下完全溶解在水中,在搅拌下滴加硅酸四乙酯,滴加完毕后,继续搅拌直至生成凝胶;
(2)制备催化剂粉体:将步骤(1)所获得的凝胶,在100℃−140℃温度下烘干并研磨成粉末,烘干的凝胶粉末放入马弗炉中,经煅烧后获得通式为Li0.1NiCoPSi4O12.6的催化剂粉体,所制得的催化剂在模拟阳光的氙灯照射下能有效地降解废水中的亚甲基蓝染料;所述催化剂粉体中的锂元素、镍元素、钴元素、磷元素和硅元素的摩尔比为0.1:1:1:1:4;所述方法中的煅烧是将所获得的凝胶粉末放入马弗炉中,在400℃−900℃温度下煅烧5−15小时。
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