CN112121808A - 一种Fe掺杂改性的Fe-Bi2O4压电催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种Fe掺杂改性的Fe‑Bi2O4压电催化剂的制备方法，包括以下步骤：(1)在内村有聚四氟乙烯的反应釜中，在超纯水中加入九水合硝酸铁和二水合铋酸钠，并搅拌分散形成悬浊液；(2)得到的悬浊液加热至433±5K进行水热合成反应10～15h；(3)水热合成后的反应产物先经过超纯水反复离心洗涤至中性，最后用乙醇洗涤若干次，得到的产物经过烘干和干燥处理，得到Fe‑Bi2O4压电催化剂。本发明采用水热合成法制备的Fe‑Bi2O4，操作简单，能够快速降解污染物，可以广泛应用，在降解磺胺甲基嘧啶方面具有显著的优点。本发明催化剂具有合成便利、环境友好、性能稳定、效率高等优点。
Description
技术领域
本发明本发明属于水污染技术领域，具体涉及Fe-Bi2O4的制备方法，以及该材料压电催化降解磺胺甲基嘧啶的应用。。
背景技术
抗生素在预防和治疗人类和动植物疾病以及在养殖业和农业得到广泛的应用。由于不合理的使用，在环境介质中，特别是水环境中不断的检测出了抗生素的存在。全球范围内几乎所有地区农作物都采用抗生素来实现增加产量、提高经济效益的目的。目前经常在食品抗生素残留检测中发现磺胺类抗生素的残留，水中的磺胺抗生素，胁迫微生物产生耐药性，产生抗性基因并通过基因水平传递到有害菌群，通过食物链威胁人类的健康。
高级氧化技术(AOPs)是指在高温、电、光照、催化剂等条件下，产生具有强氧化能力的活性自由基(·OH、SO4-·、·O2-、1O2等)，使有机污染物分解为低毒或者无毒的小分子物质，或者最终矿化为CO2和H2O及其他无机物的污水处理技术。具有低能、高矿化、无污染、反应快等特点。
压电催化技术也是属于高级氧化技术的一种。压电催化效应的本质是压电效应产生电荷，电荷参与化学反应。压电催化领域涉及的材料从传统的压电材料拓展至二维过渡金属硫化物。目前压电催化效应研究领域的主要集中在有机污染物的降解与压电催化分解H2O制H2。研究的材料范围包括传统的压电材料如BaTiO3和ZnO也包括近几年来发现的具备压电效应的材料如BiOIO3，MoS2等。
发明内容
发明目的：本发明所要解决的技术问题是提供一种Fe掺杂改性的Fe-Bi2O4压电催化剂的制备方法，对污水中磺胺甲基嘧啶的压电催化降解具有显著优点，具有更高的催化效率。
发明内容：为解决上述技术问题，本发明所采用的技术手段为：一种Fe掺杂改性的Fe-Bi2O4压电催化剂的制备方法，包括以下步骤：
(1)在内村有聚四氟乙烯的反应釜中，在超纯水中加入九水合硝酸铁和二水合铋酸钠，并搅拌分散形成悬浊液；
(2)得到的悬浊液加热至433±5K进行水热合成反应10～15h；
(3)水热合成后的反应产物先经过超纯水反复离心洗涤至中性，最后用乙醇洗涤若干次，得到的产物经过烘干和干燥处理，得到Fe-Bi2O4压电催化剂。
作为优选方案，所述九水合硝酸铁的添加量为1.54～6.16g/L，二水合铋酸钠的添加量为20～30g/L。
作为优选方案，反应产物烘干时的离心转速为7500rpm/min，烘干温度328K，时间12h.。
有益效果：相比于现有技术，本发明采用了水热合成法成功制备了Fe-Bi2O4，该材料制备方法操作简单，能够快速降解污染物，可以广泛应用。压电催化降解磺胺甲基嘧啶方面具有显著的优点。本发明催化剂具有合成便利、环境友好、性能稳定、效率高等优点。
附图说明
图1是本发明实例1和对比例1所制备的Fe-Bi2O4和Bi2O4催化剂的X射线衍射谱图(XRD)。
图2是本发明实例1和对比例1所制备的(1.5％)Fe-Bi2O4和Bi2O4降解效率对比曲线图。
图3是本发明实例1和对比例1、实例2所得的1％、1.5％、3％、4％的Fe-Bi2O4催化剂和Bi2O4对SM降解效率对比曲线图。
具体实施方式
下面结合附图并以具体实施例，进一步阐明本发明。应理解这些实施例仅用于说明本发明而不用于限制本发明的范围，在阅读了本发明之后，本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定的范围。
实例1：(1.5％)Fe-Bi2O4的制备及应用
(1)采用水热合成法制备Fe-Bi2O4，称取0.0462g九水合硝酸铁和0.56g二水合铋酸钠完全分散于20mL超纯水中。
(2)将混合溶液置于50mL内衬聚四氟乙烯的不锈钢高压反应釜中进在433K的条件下进行水热合成，反应时间12h。
(3)将水热合成后产物先用超纯水离心洗涤到中性，再用乙醇洗涤若干次，然后将洗涤后的产物进行烘干、干燥，其温度为328K，时间12h，即得到Fe-Bi2O4的目标产物。
(4)将步骤(3)得到的催化剂压电催化用于降解SM：50mL初始浓度20mg/L的SM于100mL烧杯中，Fe-Bi2O4催化剂加入量0.04g，在避光的条件下进行超声。反应时间为2h(取样时间点：0min，15min，30min，45min，60min，90min，120min)后，利用0.22微米水系滤头过滤取样1mL在液相瓶里。使用高效液相色谱检测SM浓度。
在2h内，Fe-Bi2O4催化剂对SM压电催化降解作用高达90％以上，效果显著。
对比例1：Bi2O4压电催化降解SM
对于对比例1，以Bi2O4为催化剂，该催化剂采用水热法合成。将0.56g二水合铋酸钠粉末均匀分散20mL超纯水中，然后将悬浊液置于反应釜中433K反)应12小时，再经洗涤、干燥制得Bi2O4。
将得到的Bi2O4催化剂用于压电催化降解SM，实验条件同上述实例1相同。两小时后Bi2O4压电催化降解SM效率约65％左右。
由图2可知，Fe-Bi2O4压电催化降解污染物的效率明显优于Bi2O4压电催化剂。
实例2:(1％、3％、4％)Fe-Bi2O4制备及应用
分别称取0.0308g、0.0924g、0.1232g的九水合硝酸铁和0.56g的二水合铋酸钠完全分散于20mL超纯水中。其余步骤按照实例1中Fe-Bi2O4的制备方法，分别制备得到1％、3％、4％的Fe-Bi2O4。
将得到的1％、3％、4％的Fe-Bi2O4催化剂用于压电催化降解SM，实验条件同上述实例1相同。(1％、3％、4％)Fe-Bi2O4催化剂在两小时后压电催化降解SM的效率明显优于没有Fe掺杂的Bi2O4催化剂。
本发明采用了水热合成法成功制备了Fe-Bi2O4，该材料制备方法操作简单，可以广泛应用。
本发明专利通过Fe掺杂改性Bi2O4制备出Fe-Bi2O4压电催化剂，为压电催化剂增加新的一员。Fe-Bi2O4压电催化剂对污染物的降解效果明显优于Bi2O4压电催化剂。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述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；而这些修改或者替换，并不使相应技术方案的本质脱离本发明实施例技术方案的精神和范围。
Claims (3)
1.一种Fe掺杂改性的Fe-Bi2O4压电催化剂的制备方法，其特征在于包括以下步骤：
(1)在内村有聚四氟乙烯的反应釜中，在超纯水中加入九水合硝酸铁和二水合铋酸钠，并搅拌分散形成悬浊液；
(2)得到的悬浊液加热至433±5K进行水热合成反应10～15h；
(3)水热合成后的反应产物先经过超纯水反复离心洗涤至中性，最后用乙醇洗涤若干次，得到的产物经过烘干和干燥处理，得到Fe-Bi2O4压电催化剂。
2.根据权利要求1所述Fe掺杂改性的Fe-Bi2O4压电催化剂的制备方法，其特征在于：所述九水合硝酸铁的添加量为1.54～6.16g/L，二水合铋酸钠的添加量为20～30g/L。
3.根据权利要求1所述Fe掺杂改性的Fe-Bi2O4压电催化剂的制备方法，其特征在于：反应产物烘干时的离心转速为7500rpm/min，烘干温度328K，时间12h。
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| CN1799690A (zh) * | 2006-01-13 | 2006-07-12 | 南京大学 | AgTO2型复合氧化物可见光响应光催化材料及其应用 |
| CN108273492A (zh) * | 2018-04-01 | 2018-07-13 | 云南大学 | 一种氧化铋/四氧化二铋异质结光催化剂及其制法和用途 |
| CN108722458A (zh) * | 2018-05-30 | 2018-11-02 | 苏州科技大学 | 一种四氧化铋-碳酸氧铋复合材料及其制备方法和应用 |
| CN108906090A (zh) * | 2018-07-20 | 2018-11-30 | 苏州科技大学 | 一种具有p-n异质结的光催化复合材料及其制备方法和应用 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1799690A (zh) * | 2006-01-13 | 2006-07-12 | 南京大学 | AgTO2型复合氧化物可见光响应光催化材料及其应用 |
| CN108273492A (zh) * | 2018-04-01 | 2018-07-13 | 云南大学 | 一种氧化铋/四氧化二铋异质结光催化剂及其制法和用途 |
| CN108722458A (zh) * | 2018-05-30 | 2018-11-02 | 苏州科技大学 | 一种四氧化铋-碳酸氧铋复合材料及其制备方法和应用 |
| CN108906090A (zh) * | 2018-07-20 | 2018-11-30 | 苏州科技大学 | 一种具有p-n异质结的光催化复合材料及其制备方法和应用 |
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