CN108837851A - 一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法 - Google Patents
一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法 Download PDFInfo
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Abstract
本发明涉及污水体系中重金属离子的去除、有机污染物降解技术领域,尤其涉及一种高效吸附‑还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法。其包括以下步骤:(1)将纳米TiO2进行辐照;(2)将经所述辐照的纳米TiO2在包含乙烯基单体的乳液中分散。该法制备得到的催化剂能够高效、无污染地将高价高毒的六价铬离子转变成无毒的三价铬离子。
Description
技术领域
本发明涉及污水体系中重金属离子的去除、有机污染物降解技术领域,尤其涉及一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法。
背景技术
纳米TiO2半导体氧化物在光催化反应领域,已引起了人们的极大关注。当TiO2半导体吸收了能量大于禁带宽度的光能后,价带电子被激发至导带,产生电子一空穴对,光生空穴具有强氧化性,它能促使许多化学反应发生,如光还原、光催化、光有机合成等。纳米TiO2粒径小、比表面大、表面能高,纳米粒子很容易团聚;另一方面纳米TiO2与表面能比较低的基体的亲和性差,二者在相互混合时不能相溶,导致界面出现空隙,存在相分离现象。为了确保纳米TiO2在水相中保持较好的分散性和亲水性,纳米TiO2的表面改性成为必然。利用电离辐射接枝方法,在纳米TiO2表面引入含有亲水性官能团的单体,既能保证纳米TiO2具有良好的分散性和亲水性,也能够实现吸附-光催化还原反应的协同作用,确保了高毒性的六价铬离子转变成无毒性的三价铬离子。
高毒性的六价铬离子(Cr6+)为吞入性毒物,皮肤接触可导致敏感,具有毒性长期持续、生物不可降解的特点。Cr6+ 可以通过食物链在生物体内累积而致癌。很容易被人体吸收,它可以通过消化、呼吸道、皮肤及粘膜侵入人体。而一定浓度的三价铬离子(Cr3+)是无毒的,也是对人体有益的元素。传统的去除六价铬离子(Cr6+)的方法主要有:化学沉淀法、溶剂萃取分离、吸附法和离子交换法等,存在的不足是:①过量添加剂的引入会造成二次污染;②溶剂流失严重,消耗大;③再生效率低;④制作成本高,耗量大;⑤将污染物从一相转移到另一相,并没有将污染物彻底无公害化。因此将高价高毒的六价铬离子(Cr6+)转变成无毒的三价铬离子(Cr3+)的研究很有必要。
辐射接枝法的特点:①基材可以在温和的反应条件下产生活性位点和活性自由基相互连接,避免了高温高压等条件对材料造成损害;②基材产生活性自由基是由射线引发,不需要在其中加入催化剂、引发剂等物质,从而能得到更纯净、更清洁的接枝产物;③通过控制辐射接枝反应条件,可以对接枝率、官能团的含量及其分布等有效调控。辐射接枝法相对于上述物理、化学方法而言,实现了有效的补充和完善,有效的规避了上述的缺陷,从长远的角度来看,辐射合成技术及相关催化材料制备极富前景的研究途径。
发明内容
本发明要解决上述问题,提供一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,制备得到的催化剂能够高效、无污染地将高价高毒的六价铬离子转变成无毒的三价铬离子。
本发明解决问题的技术方案是,提供一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,包括以下步骤:(1)将纳米TiO2进行辐照;(2)将经所述辐照的纳米TiO2在包含乙烯基单体的乳液中分散。
优选地,所述乳液按照质量份包含5~30份乙烯基单体、0.5~5份表面活性剂、0.1~2.0份pH调节剂。
优选地,辐照条件:电子束能量为1~5 MeV,辐射剂量为10~120 kGy,剂量率为5~40kGy/pass。
优选地,所述步骤(2),将经辐照的纳米TiO2在包含乙烯基单体的乳液中分散后,继续通氮气并搅拌0.5 ~ 2 h。
优选地,还包括步骤(3)提纯干燥。
优选地,所述提纯干燥包括:醇洗、水洗,洗涤后于60℃真空干燥24 h。
优选地,所述提纯干燥还包括:于40~100℃下索氏抽提8~48 h后真空干燥。
优选地,所述乙烯基单体为甲基丙烯酸二甲氨基乙酯、甲基丙烯酸二乙氨基乙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸叔丁基氨基乙酯中的一种或几种。
优选地,所述表面活性剂为脂肪醇聚醚系列、聚乙二醇系列、吐温系列、司盘系列中的一种或几种。
优选地,所述pH调节剂为磷酸二氢钠,碳酸氢二钠,乙酸,三乙醇胺中的一种或几种。pH调节剂的引入,可以调节高分子和纳米材料形成的混合乳液体系的等电点和稳定的分散性,确保高分子自身不缠结,有利于后期辐射交联与原位还原的顺利进行。
本发明的有益效果:
1.在纳米TiO2表面引入含有亲水性官能团的单体,既能保证纳米TiO2具有良好的分散性和亲水性,也能够实现吸附-光催化还原反应的协同作用,实现了吸附-光催化还原的有机统一,达到了二者优势互补的应用目的。
2.所得催化剂能高效、无污染的将有毒的高价重金属离子氧化为低价无毒的金属离子,使得催化剂的作用得以最大发挥,有望有效应用于污水体系中重金属离子的去除、有机污染物降解等技术领域。
3.辐照接枝技术无毒、反应条件温和,反应过程不添加交联剂、引发剂以及任何对人体有毒的物质,可有效避免二次污染。
4.制备得到的纳米TiO2基光催化剂可广泛推广运用于污水体系中重金属离子的去除、有机污染物降解等技术领域。
具体实施方式
以下是本发明的具体实施方式,对本发明的技术方案作进一步的描述,但本发明并不限于这些实施例。
实施例1
称取一定量的纳米TiO2粉末放入真空PE密封袋中,该密封袋厚度约2 mm,置于电子束下进行辐照,选择的电子束能量为1 MeV,辐射剂量为10 kGy,剂量率为5 kGy/pass,将辐照后的纳米TiO2样品,迅速投入到按质量份含有5 份甲基丙烯酸二甲氨基乙酯、0.5份吐温80、0.1 份磷酸二氢钠溶液的三口烧瓶当中,通入N2并搅拌0.5 h,取所得样品,经醇洗,水洗后,于60℃真空干燥箱中干燥24 h后,在温度为40℃下,经索氏抽提8 h,再次进行真空干燥,即可制得高效吸附-还原高毒性的六价铬离子的纳米TiO2基光催化剂。
取定量的纳米TiO2基光催化剂溶于20 mL、10 ppm Cr6+溶液,调节pH为3,超声时间为10 min,将所得溶液暗吸附0.5 h,在紫外灯下照射2 h,用0.22 μm滤膜过滤样品,用DPCI显色法测定滤液当中Cr6+和Cr3+的含量。结果表明:Cr6+的吸附-还原率为82.5 %。
实施例2
称取一定量的纳米TiO2粉末放入真空PE密封袋中,该密封袋厚度约2 mm,置于电子束下进行辐照,选择的电子束能量为1 MeV,辐射剂量为30 kGy,剂量率为10 kGy/pass,将辐照后的纳米TiO2样品,迅速投入到按质量份含有10 份甲基丙烯酸二乙氨基乙酯、1 份聚乙二醇2000、0.2 份三乙醇胺溶液的三口烧瓶当中,通入N2并搅拌1 h,取所得样品,经醇洗,水洗后,于60℃真空干燥箱中干燥24 h后,在温度为60℃下,经索氏抽提10 h,再次进行真空干燥,即可制得高效吸附-还原高毒性的六价铬离子的纳米TiO2基光催化剂。
取定量的纳米TiO2基光催化剂溶于20 mL、10 ppm Cr6+溶液,调节pH为3,超声时间为10 min,将所得溶液暗吸附0.5 h,在紫外灯下照射2 h,用0.22 μm滤膜过滤样品,用DPCI显色法测定滤液当中Cr6+和Cr3+的含量。结果表明:Cr6+的吸附-还原率为84.3 %。
实施例3
称取一定量的纳米TiO2粉末放入真空PE密封袋中,该密封袋厚度约2 mm,置于电子束下进行辐照,选择的电子束能量为1 MeV,辐射剂量为60 kGy,剂量率为30 kGy/pass,将辐照后的纳米TiO2样品,迅速投入到按质量份含有20 份甲基丙烯酸叔丁基氨基乙酯、2 份司盘60、1 份乙酸溶液的三口烧瓶当中,通入N2并搅拌2 h,取所得样品,经醇洗,水洗后,于60℃真空干燥箱中干燥24 h后,在温度为80℃下,经索氏抽提24 h,再次进行真空干燥,即可制得高效吸附-还原高毒性的六价铬离子的纳米TiO2基光催化剂。
取定量的纳米TiO2基光催化剂溶于20 mL、10 ppm Cr6+溶液,调节pH为3,超声时间为10 min,将所得溶液暗吸附0.5 h,在紫外灯下照射2 h,用0.22 μm滤膜过滤样品,用DPCI显色法测定滤液当中Cr6+和Cr3+的含量。结果表明:Cr6+的吸附-还原率为87.6 %。
实施例4
称取一定量的纳米TiO2粉末放入真空PE密封袋中,该密封袋厚度约2 mm,置于电子束下进行辐照,选择的电子束能量为1 MeV,辐射剂量为120 kGy,剂量率为40 kGy/pass,将辐照后的纳米TiO2样品,迅速投入到按质量份含有30份甲基丙烯酸缩水甘油酯、5 份高碳脂肪醇聚氧乙烯醚、2 份乙酸溶液的三口烧瓶当中,通入N2并搅拌2 h,取所得样品,经醇洗,水洗后,于60℃真空干燥箱中干燥24 h后,在温度为100℃下,经索氏抽提48 h,再次进行真空干燥,即可制得高效吸附-还原高毒性的六价铬离子的纳米TiO2基光催化剂。
取定量的纳米TiO2基光催化剂溶于20 mL、10ppm Cr6+溶液,调节pH为3,超声时间为10 min,将所得溶液暗吸附0.5 h,在紫外灯下照射2 h,用0.22 μm滤膜过滤样品,用DPCI显色法测定滤液当中Cr6+和Cr3+的含量。结果表明:Cr6+的吸附-还原率为78.1 %。
本文中所描述的具体实施例仅仅是对本发明精神作举例说明。本发明所属技术领域的技术人员可以对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (10)
1.一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:包括以下步骤:(1)将纳米TiO2进行辐照;(2)将经所述辐照的纳米TiO2在包含乙烯基单体的乳液中分散。
2.根据权利要求1所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:所述乳液按照质量份包含5~30份乙烯基单体、0.5~5份表面活性剂、0.1~2.0份pH调节剂。
3.根据权利要求1所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:辐照条件:电子束能量为1~5 MeV,辐射剂量为10~120kGy,剂量率为5~40 kGy/pass。
4.根据权利要求1所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:所述步骤(2),将经辐照的纳米TiO2在包含乙烯基单体的乳液中分散后,继续通氮气并搅拌0.5 ~ 2 h。
5.根据权利要求1所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:还包括步骤(3)提纯干燥。
6.根据权利要求5所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:所述提纯干燥包括:醇洗、水洗,洗涤后于60℃真空干燥24 h。
7.根据权利要求6所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:所述提纯干燥还包括:于40~100℃下索氏抽提8~48 h后真空干燥。
8.根据权利要求2所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:所述乙烯基单体为甲基丙烯酸二甲氨基乙酯、甲基丙烯酸二乙氨基乙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸叔丁基氨基乙酯中的一种或几种。
9.根据权利要求2所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:所述表面活性剂为脂肪醇聚醚系列、聚乙二醇系列、吐温系列、司盘系列中的一种或几种。
10.根据权利要求2所述的一种高效吸附-还原高毒性六价铬离子的纳米TiO2基光催化剂的预辐射接枝合成方法,其特征在于:所述pH调节剂为磷酸二氢钠,碳酸氢二钠,乙酸,三乙醇胺中的一种或几种。
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