CN107008333A - 磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法及该材料的应用 - Google Patents
磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法及该材料的应用 Download PDFInfo
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Abstract
本发明属于催化剂技术领域，具体涉及一种磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法，该制备过程以六水合氯化镍、六水合三氯化铁、二水合醋酸锌、乙二醇甲醚、乙醇胺、氢氧化钠和去离子水为原料。首先六水合氯化镍和六水合三氯化铁配制成混合溶液，然后对混合溶液进行加热、分离、洗涤、烘干，得到磁性异相光芬顿催化剂NiFe2O4。其次，二水合醋酸锌搅拌溶于乙二醇甲醚，再把NiFe2O4固体粉末加入到混合溶液中，搅拌加入乙醇胺和分散剂，加热、分离、洗涤、烘干获得磁性异相光芬顿NiFe2O4/ZnO复合纳米半导体材料。该材料不但能效且快速吸附‑光催化去除水体中的有机染料，而且能通过磁铁回收催化剂。同时，具有制备简单和能重复使用的特点。
Description
技术领域
本发明属于催化剂技术领域，具体涉及一种磁性异相光芬顿 NiFe2O4/ZnO复合纳米材料的制备方法及该材料的应用。
背景技术
目前我国各种染料产量已达90万吨，染料废水已成为环境重点污染源之一。染料行业品种繁多，工艺复杂，其废水中含有大量的有机物，具有CODCr高、色泽深、酸碱性强等特点，一直是废水处理中的难题。于是开发新型水处理材料和新型工艺，控制有毒有机污染物已成为环境领域亟待解决的关键问题之一。经过几十年的研究发现，利用ZnO和TiO2半导体可发生光催化使水分解成氢和氧，光催化反应能将有机污染物完全矿化成CO2、H2O等无机小分子物质，且反应条件温和，能耗低，安全无毒，操作简便，被视为一种理想的高效、低耗的绿色环境治理技术而受到环境专家的关注。据文献报道，人们已经合成了许多ZnO纳米结构并广泛应用在光催化等领域。然而，纳米ZnO是一种宽带隙的半导体材料，对光的吸收仅限于紫外区，且光生载流子的复合率高，导致光催化效率很低。而且，太阳光谱中紫外光能(400nm以下)不到5％，而波长为400-750nm的可见光则占到近 43％，因此，发展高效的具有可见光响应的复合光催化剂是目前光催化已经领域的一项重要课题。
为了提高可见光或太阳光对ZnO的光催化性能，常用的方法是贵金属修饰、半导体复合、染料敏化、过渡金属离子和非金属掺杂等。目前，光催化剂(尤其纳米光催化剂)在使用过程中还存在固液分离和回收困难，严重阻碍了光催化技术的实际应用。近年来出现的将磁性分离技术与固相催化剂/吸附剂相结合的方法，在解决环境污染问题中发挥了很好的作用。由于磁性光催化剂既具备悬浮相光催化剂的高效性，又可利用磁性分离技术高效快速地回收，实现资源的再利用，是一种环境友好型催化剂，也是未来水处理光催化剂的重要发展方向之一。
发明内容
本发明主要提供了一种磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法，该方法工艺简单，制备的催化剂能效且快速吸附- 光催化去除水体中的有机染料。其技术方案如下：
一种磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法，包括以下步骤：
Ⅰ)NiFe2O4的制备：
(1)按铁和镍的摩尔比为2:1-1.5分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中；
(2)将混合溶液加热至80-100℃保温2.5-3.5h，向混合溶液中滴加碱性溶液调节pH值为10-14；
(3)将加热后的溶液转移至反应釜中，将反应釜加热到600-800℃并保温2.5-3.5h；
(4)将加热后获得的粉末固体在磁场中进行分离，然后对磁性粉末洗涤并烘干，得到磁性异相光芬顿催化剂NiFe2O4；
Ⅱ)NiFe2O4/ZnO磁性复合物的制备：
(1)将二水合醋酸锌搅拌溶于乙二醇甲醚中，再加入乙醇胺；
(2)加入制备完成的催化剂NiFe2O4，NiFe2O4与ZnO的质量比为1:3-9，并进行搅拌，得到均匀稳定的乳液；
(3)将乳液在550±50℃下保持1h，得到反应混合物；
(4)将混合物冷却，使用磁铁磁吸固体物，清洗并干燥，得磁性异相光芬顿NiFe2O4/ZnO复合纳米材料。
优选的，磁性异相光芬顿催化剂NiFe2O4的粒径为10-20nm， NiFe2O4/ZnO复合纳米材料的粒径为10-30nm。
优选的，NiFe2O4/ZnO复合纳米材料的比表面积为68.32m2/g。
磁性异相光芬顿NiFe2O4/ZnO复合纳米材料在处理染料废水有机污染物中的应用中，所述复合纳米材料对亚甲基蓝有机溶液的光催化降解效率达到98.42％以上。
采用上述方法，本发明具有以下优点：
本发明方法工艺简单，耗时较短，制得的复合纳米材料直径范围为10-30nm，材料比表面积为68.32m2/g，可以能效且快速吸附-光催化去除水体中的有机染料，对于亚甲基蓝有机溶液的光催化降解效率达到98.42％以上，对染料废水有机污染物处理效率高。而且能通过磁铁回收催化剂进行重复利用，第五次使用时对亚甲基蓝有机溶液的光催化降解效率仍达到95.20％，具有良好的重复使用性。
附图说明
图1为实施例1中NiFe2O4/ZnO的XRD图谱；
图2为实施例1中NiFe2O4/ZnO复合纳米材料的SEM图片；
图3为实施例1中NiFe2O4/ZnO复合纳米材料对亚甲基蓝溶液的降解效果曲线。
具体实施方式
实施例1
一种磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法，其包括以下步骤：
Ⅰ)NiFe2O4的制备：
(1)按铁和镍的摩尔比为2:1分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中，并超声处理60min，磁力搅拌30min；
(2)将混合溶液加热至90℃保温3h，向混合溶液中滴加氢氧化钠溶液调节pH值为13；
(3)将加热后的溶液转移至聚四氟乙烯内衬的不锈钢高压釜中，将高压釜放入马弗炉中，以每分钟升温3℃密闭加热到600℃，并保温3h；
(4)将加热后获得的粉末固体在磁场中进行分离，然后对磁性粉末洗涤并烘干，得到磁性异相光芬顿催化剂NiFe2O4；
Ⅱ)NiFe2O4/ZnO磁性复合物的制备：
(1)在50℃下，将2.195g二水合醋酸锌搅拌溶于50ml的乙二醇甲醚中，磁力搅拌30min，再加入乙醇胺6ml搅拌5min；
(2)加入0.349g制备完成的催化剂NiFe2O4，并进行搅拌15min，超声处理60min，加入德国莱茵化学生产的P400稳定剂，得到均匀稳定的乳液；
(3)将乳液转移至聚四氟乙烯内衬的不锈钢高压釜中，把密封的高压釜放入马弗炉中，以每分钟升温3℃加热到550℃保持1h，得到反应混合物；
(4)将混合物冷却至室温，使用磁铁磁吸固体物，清洗并干燥，得磁性异相光芬顿NiFe2O4/ZnO复合纳米材料，该复合材料的比表面积为68.32m2/g。
本实施制备的NiFe2O4/ZnO中NiFe2O4质量占30％，ZnO质量占 70％。对本实施制备的NiFe2O4/ZnO的XRD的图谱分析如图1所示。对本实施制备的NiFe2O4/ZnO的SEM分析检测如图2所示，从图2 可看出复合纳米颗粒的大小约10-30nm。取0.5g NiFe2O4/ZnO复合纳米材料，加入到100mL、20mg/L的亚甲蓝溶液中，置于500W的紫外可见灯下进行光催化反应，光源离反应液面距离为20cm。光催化 60分钟后其脱色率可以达到98.42％，如图3所示。
本发明的复合纳米材料在使用五次以后，检测对亚甲基蓝有机溶液的脱色率，其可以达到95.20％。
实施例2
Ⅰ)NiFe2O4的制备：
(1)按铁和镍的摩尔比为2:1.5分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中，并超声处理60min，磁力搅拌30min；
(2)将混合溶液加热至80℃保温3.5h，向混合溶液中滴加氢氧化钠溶液调节pH值为14；
(3)将加热后的溶液转移至聚四氟乙烯内衬的不锈钢高压釜中，将高压釜放入马弗炉中，以每分钟升温3℃密闭加热到800℃，并保温2.5h；
(4)将加热后获得的粉末固体在磁场中进行分离，然后对磁性粉末洗涤并烘干，得到磁性异相光芬顿催化剂NiFe2O4；
Ⅱ)NiFe2O4/ZnO磁性复合物的制备：
(1)在50℃下，将2.195g二水合醋酸锌搅拌溶于50ml的乙二醇甲醚中，磁力搅拌30min，再加入乙醇胺6ml搅拌5min；
(2)加入0.0904g制备完成的催化剂NiFe2O4，并进行搅拌15min，超声处理60min，加入德国莱茵化学生产的P400稳定剂，得到均匀稳定的乳液；
(3)将乳液转移至聚四氟乙烯内衬的不锈钢高压釜中，把密封的高压釜放入马弗炉中，以每分钟升温3℃加热到600℃保持1h，得到反应混合物；
(4)将混合物冷却至室温，使用磁铁磁吸固体物，清洗并干燥，得磁性异相光芬顿NiFe2O4/ZnO复合纳米材料。
实施例3
Ⅰ)NiFe2O4的制备：
(1)按铁和镍的摩尔比为2:1分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中，并超声处理60min，磁力搅拌30min；
(2)将混合溶液加热至100℃保温2.5h，向混合溶液中滴加氢氧化钠溶液调节pH值为10；
(3)将加热后的溶液转移至聚四氟乙烯内衬的不锈钢高压釜中，将高压釜放入马弗炉中，以每分钟升温3℃密闭加热到700℃，并保温3h；
(4)将加热后获得的粉末固体在磁场中进行分离，然后对磁性粉末洗涤并烘干，得到磁性异相光芬顿催化剂NiFe2O4；
Ⅱ)NiFe2O4/ZnO磁性复合物的制备：
(1)在50℃下，将2.195g二水合醋酸锌搅拌溶于50ml的乙二醇甲醚中，磁力搅拌30min，再加入乙醇胺6ml搅拌5min；
(2)加入0.136g制备完成的催化剂NiFe2O4，并进行搅拌15min，超声处理60min，加入德国莱茵化学生产的P400稳定剂，得到均匀稳定的乳液；
(3)将乳液转移至聚四氟乙烯内衬的不锈钢高压釜中，把密封的高压釜放入马弗炉中，以每分钟升温3℃加热到500℃保持1h，得到反应混合物；
(4)将混合物冷却至室温，使用磁铁磁吸固体物，清洗并干燥，得磁性异相光芬顿NiFe2O4/ZnO复合纳米材料。
对本领域的技术人员来说，可根据以上描述的技术方案以及构思，做出其它各种相应的改变以及形变，而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (5)
1.一种磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法，其特征在于：包括以下步骤：
Ⅰ)NiFe2O4的制备：
(1)按铁和镍的摩尔比为2:1-1.5分别称取六水合氯化镍和六水合三氯化铁溶于去离子水中；
(2)将混合溶液加热至80-100℃保温2.5-3.5h，向混合溶液中滴加碱性溶液调节pH值为10-14；
(3)将加热后的溶液转移至反应釜中，将反应釜加热到600-800℃并保温2.5-3.5h；
(4)将加热后获得的粉末固体在磁场中进行分离，然后对磁性粉末洗涤并烘干，得到磁性异相光芬顿催化剂NiFe2O4；
Ⅱ)NiFe2O4/ZnO磁性复合物的制备：
(1)将二水合醋酸锌搅拌溶于乙二醇甲醚中，再加入乙醇胺；
(2)加入制备完成的催化剂NiFe2O4，NiFe2O4与ZnO的质量比为1:3-9，并进行搅拌，得到均匀稳定的乳液；
(3)将乳液在550±50℃下保持1h，得到反应混合物；
(4)将混合物冷却，使用磁铁磁吸固体物，清洗并干燥，得磁性异相光芬顿NiFe2O4/ZnO复合纳米材料。
2.根据权利要求1所述的磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法，其特征在于：磁性异相光芬顿催化剂NiFe2O4的粒径为10-20nm，NiFe2O4/ZnO复合纳米材料的粒径为10-30nm。
3.根据权利要求1所述的磁性异相光芬顿NiFe2O4/ZnO复合纳米材料的制备方法，其特征在于：NiFe2O4/ZnO复合纳米材料的比表面积为68.32m2/g。
4.磁性异相光芬顿NiFe2O4/ZnO复合纳米材料在处理染料废水有机污染物中的应用。
5.根据权利要求4所述的磁性异相光芬顿NiFe2O4/ZnO复合纳米材料在处理染料废水有机污染物中的应用，其特征在于：所述复合纳米材料对亚甲基蓝有机溶液的光催化降解效率达到98.42％以上。
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