CN105642348A - 磁性可回收纳米复合水凝胶催化材料原位辐射制备方法 - Google Patents
磁性可回收纳米复合水凝胶催化材料原位辐射制备方法 Download PDFInfo
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Abstract
本发明公开了一种磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法。将天然聚多糖、辐照敏化剂、金属离子源、羟基自由基清除剂以及pH调节剂和水进行配比,通过电子束轰击溶液产生的次级粒子eaq-还原离子源,利用电子束辐射交联制备所得的金属单质或金属氧化物能均匀嵌插在交联的水凝胶骨架内的水凝胶“软反应器”催化材料。将制得的样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒。既可实现废催化材料中磁性金属或金属氧化物的回收再利用,也完成金属单质或金属氧化物和天然聚多糖水凝胶多元复合协同催化效果。具有快速回收、成本低、柔韧性好等特点,尤其适合环境污水处理和有机催化领域。
Description
技术领域
本发明涉及一种磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,特别是一种通过电子束原位还原负载磁性纳米金属颗粒的方法。
背景技术
随着现代工业的迅猛发展,有机试剂及染料的用量呈指数增长,随之伴随的水体污染给人类的生存健康带来了严峻的挑战,有机污染已经成为当前亟待妥善解决的环境问题。为此各国政府一方面加强制定措施严控污水的排放质量和标准,另一方面投入巨资与人力来开发新型水资源净化材料。目前,工业废水处理方法大致可以分为三类:物理处理法(活性炭、膜技术),生物处理法(微生物、植物等)和化学法。当处理高浓度有机工农业污水时,常优先考虑一些化学法(氧化还原法、光催化矿化法)来处理,虽然可以通过化学反应改变污染物的化学性质,使其转化为无害的或可分离的物质,但在方法上存在着不可避免的二次污染问题和成本高缺陷;生物法技术日趋成熟且费用较低,但此法治理效率低,周期较长,不适于处理重污染的水体;而采用物理法法处理时,无论是传统的吸附材料(例如活性炭、沸石分子筛、树脂),还是近年来备受关注的常规水凝胶,都面临同一个问题,就是只能通过简单的物理吸附,同时伴随被吸附的污染物的脱附过程,污染物会进一步出现“渗漏”现象。对磁性可回收纳米复合水凝胶催化材料研究,很好地解决了这个问题,它不仅具有水凝胶的吸附性和良好的催化性能,可以有效降解水体中的有机污染物。天然高分子水凝胶在吸附催化降解有机物的同时自身发生降解,磁性金属材料可以进一步回收再利用。
传统的水凝胶催化材料普遍采用化学交联法与化学还原法。但是该法制备的水凝胶不仅易在水体中释放残余的剧毒交联剂与还原剂,而且会出现不均匀交联,局部发生“烧焦现象”,并且化学交联难以控制交联度;其次化学还原法(NaBH4)还原出的金属颗粒不仅不能均匀分布在凝胶骨胶体系,而且其与凝胶分子间的作用力太弱甚至没有,让其易从凝胶孔洞中流失,从而影响了水凝胶的催化稳定性,制约了水凝胶作为多功能材料的应用。为克服化学交联法与化学还原法带来的不足,辐射合成磁性纳米复合水凝胶的方法应运而生。辐射法相对于化学法实现了有效的补充和完善,具体表现为:①反应过程不需要添加任何对人体有毒的物质,交联度高,水凝胶纯度高;②反应条件温和,在室温下即可进行,操作简便,反应周期短;③通过控制聚合物组分和辐照条件可以准确调控水凝胶的力学性能;④水凝胶制备、塑形及离子源的还原过程可同步完成;⑤原位还原负载的金属颗粒可均匀分布在凝胶骨胶中,且不易流失。从综合和长远的角度看,利用辐照技术制备水凝胶催化材料所花费的经济成本较低。因此,辐射合成技术已成为智能水凝胶制备极富前景的研究途径。
天然聚多糖是绿色高分子,是指自然界生物体内存在的高分子化合物。其独特的结构不仅赋予同合成高分子相当甚至更好的功能,而且其常具有无(低)毒、助催化、可生物降解等特性使其应用更加广泛。基于各种天然聚多糖的功能性产品、材料越来越引人注目。
本发明所要解决的问题是公开一种磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,以克服现有技术存在的上述缺陷。
经检索,国内尚未有与本发明相同的专利申请。
发明内容
针对现有技术的不足,本发明提供一种磁性可回收纳米复合水凝胶催化材料的制备方法,既实现了复合水凝胶性能的最大优化,将吸附、催化有机统一,实现了废催化材料中金属的回收再利用,也完成了金属单质和天然聚多糖水凝胶多元复合协同催化效果。该磁性可回收纳米复合水凝胶催化材料具有快速回收、成本低、柔韧性好等特点,尤其适合环境污水处理和有机催化领域。
本发明的技术方案是:通过电子束轰击溶液产生的次级粒子eaq-还原离子源,电子束辐射交联制备金属单质均匀嵌插在交联的水凝胶骨架内的水凝胶“软反应器”催化材料。所述的一种原位辐射法制备针对环境污水处理和有机催化的可回收纳米复合水凝胶催化材料合成方法,包括以下步骤:
一种磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于,包括步骤:
①、利用超声波,将1.0~6.0份羟基自由基清除剂、85~93份蒸馏水或去离子水共同分散0.5~4.0份离子源0.5~2h,使其均匀形成稳定的溶液体系;
②、取天然聚多糖5~15份、辐照敏化剂0.5~2.0份、pH调节剂0.1份~2.0份溶于蒸馏水或去离子水中,搅拌制成均匀高分子溶液;
③、将步骤②所得中间产品缓慢加入到步骤①所得的离子源溶液体系,超声搅拌均匀后,通入N2约为0.5~1h,之后负压下静置除泡;
④、将步骤③所得混合体系注射至PE密封袋中(厚度2mm),并置于电子束下进行原位还原与辐射交联反应,选择的电子束能量为1~5MeV,辐射剂量为20~80kGy,剂量率为5~40kGy/pass,最后所得的产物即为磁性可回收纳米复合水凝胶催化材料;
⑤、将步骤④所得样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒。制得的凝胶催化材料微球颗粒的交联度为20%~60%,平衡吸水率为100%~1200%。
优选地、所述的辐照敏化剂为胶原蛋白、聚乙烯醇、N-异丙基丙烯酰胺等中的一种或几种。在辐照过程中,辐照敏化剂首先迅速产生活性自由基,从而引发天然聚多糖产生活性自由基,彼此之间迅速发生交联而制备出复合水凝胶。辐照敏化剂的引入,缩短了辐照交联所需的时间,提高了生产效率,确保了复合水凝胶具有适当的交联度。
优选地、所述的羟基自由基清除剂为异丙醇、叔丁醇、邻羟基苯甲酸、对苯二甲酸等中的一种或几种。羟基自由基清除剂能够有效去除辐照中产生的次级粒子羟基自由基,而其它次级活性粒子不受影响,提高了离子源的还原率。
优选地、所述的天然聚多糖为壳聚糖及其衍生物、纤维素及其衍生物、海藻酸钠等中的一种或几种等中的一种或几种。一种或几种天然聚多糖在辐照的过程中,可以发生自交联或彼此相互交联,提高水凝胶力学性和柔韧性,而且其分子链上引入的特殊官能团还起到协同催化作用。
优选地、所述的离子源为七水硫酸亚铁,九水硫酸铁,六水硝酸亚钴,七水硫酸钴,六水硫酸镍,六水硝酸镍中的一种。在辐照过程中,离子源可以被次级活性粒子eaq-原位还原并均匀镶嵌在凝胶骨架中,这样不仅使其有磁性,便于回收,而且具有高效的有机催化活性。
优选地、所述的pH调节剂为磷酸氢二钠、磷酸一氢钠、碳酸氢钠、己二酸、乙酸、Tris-HCl、亚氨基二乙酸、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。
采用该一种eaq-原位还原与辐射交联合成方法制备得到可用于环境污水处理和有机催化领域的磁性可回收纳米复合水凝胶催化材料。
本发明的有益效果是:
1、将吸附、催化有机统一,实现了废催化材料中金属的回收再利用,也完成了金属单质和天然聚多糖水凝胶多元复合协同催化效果。
2、辐照技术无毒、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。
3、水凝胶制备、塑形及离子源原位还原同步完成,大大简化了生产工艺,节约成本,综合经济效益显著,提高了产品的使用寿命。
用本发明方法制备的磁性可回收纳米复合水凝胶催化材料可广泛推广运用作针对水中有机污染物的高速高效吸附催化复合材料。
具体实施方式
以下实施例,仅为了进一步说明本发明,并不限制本发明的内容。
实施例1:取七水硫酸亚铁0.167g、邻羟基苯甲酸0.333g,分别加入到25ml去离子水中,超声0.5h,形成形成稳定的Fe2+离子源乳液体系。将0.167g聚乙烯醇(聚合度1670)投入到95℃的6ml去离子水中,搅拌速率为150r/min,加热搅拌时间2h,完全溶解后,冷却至50℃,分别加入1.669g羧甲基壳聚糖、0.033g三乙醇胺,搅拌1h,使其完全溶解形成均匀溶液后,在搅拌下,加入到Fe2+离子源乳液体系中,继续超声机械搅拌0.5h后,通入N20.5h,之后负压下静置除泡2h,注入到15×5×1mm3的PE模具中,快速真空冷冻-干燥成型,取出产品用PE薄膜袋真空封装并置于室温下解冻。经过3次循环冷冻-解冻过程后,用电子束加速器辐照,选用辐照剂量为20kGy,剂量率为5kGy/pass的条件进行辐照,即可制备磁性铁氧化物可回收纳米复合水凝胶催化材料。在制得的水凝胶样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒.
磁性铁氧化物可回收纳米复合水凝胶催化材料的交联度和吸水性能测试采用CN1273128A中报道方法进行检测,其结果如下:交联度为20%,平衡吸水率为1200%。取定量产品投入250mL、4mg/L的环戊酮(模拟有机污染物)中,在50℃下,对模拟物进行有机催化实验,反应3h后,测得转化率达到88%。
实施例2:取六水硝酸镍0.736g、异丙醇0.368g,分别加入到25ml去离子水中,超声0.5h,形成形成稳定的Ni2+离子源乳液体系。将0.368g胶原蛋白投入到50℃的7ml去离子水中,搅拌速率为150r/min,加热搅拌时间2h,完全溶解后,冷却至20℃,分别加入2.943g羟丙基壳聚糖、0.368g冰乙酸,搅拌1h,使其完全溶解形成均匀溶液后,在搅拌下,加入到Ni2+离子源乳液体系中,继续超声机械搅拌0.5h后,通入N20.5h,之后负压下静置除泡2h,注入到15×5×1mm3的PE模具中,快速真空冷冻-干燥成型,取出产品用PE薄膜袋真空封装并置于室温下解冻。经过3次循环冷冻-解冻过程后,用电子束加速器辐照,选用辐照剂量为30kGy,剂量率为10kGy/pass的条件进行辐照,即可制备磁性镍可回收纳米复合水凝胶催化材料。在制得的水凝胶样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒.
磁性镍可回收纳米复合水凝胶催化材料的交联度和吸水性能测试采用CN1273128A中报道方法进行检测,其结果如下:交联度为46%,平衡吸水率为187.6%。取定量产品投入200mL、5mg/L的溴代烃(模拟物)中,在室温下,对模拟物进行有机催化实验,反应3h后,测得转化率达到92%。
实施例3:取六水硫酸镍0.257g、异丙醇0.368g,分别加入到25ml去离子水中,超声0.5h,形成形成稳定的Ni2+离子源乳液体系。将0.184gN-异丙基丙烯酰胺投入到60℃的7ml去离子水中,搅拌速率为150r/min,加热搅拌时间2h,完全溶解后,冷却至20℃,分别加入3.862g羧甲基纤维素、0.110g碳酸氢钠,搅拌1h,使其完全溶解形成均匀溶液后,在搅拌下,加入到Ni2+离子源乳液体系中,继续超声机械搅拌0.5h后,通入N20.5h,之后负压下静置除泡2h,注入到15×5×1mm3的PE模具中,快速真空冷冻-干燥成型,取出产品用PE薄膜袋真空封装并置于室温下解冻。经过3次循环冷冻-解冻过程后,用电子束加速器辐照,选用辐照剂量为60kGy,剂量率为30kGy/pass的条件进行辐照,即可制备磁性镍氧化物可回收纳米复合水凝胶催化材料。在制得的水凝胶样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒。
磁性镍氧化物可回收纳米复合水凝胶催化材料的交联度和吸水性能测试采用CN1273128A中报道方法进行检测,其结果如下:交联度为42%,平衡吸水率为227.6%。取定量产品投入250mL、5mg/L的溴代烃(模拟物)中,在60℃下,对模拟物进行有机催化实验,反应3h后,测得转化率达到95%。
实施例4:取六水硝酸亚钴0.185g、叔丁醇0.369g,分别加入到25ml去离子水中,超声0.5h,形成形成稳定的Co2+离子源乳液体系。将0.185g胶原蛋白投入到45℃的7ml去离子水中,搅拌速率为150r/min,加热搅拌时间2h,完全溶解后,冷却至50℃,分别加入4.059g海藻酸钠、0.111g磷酸氢二钠,搅拌1h,使其完全溶解形成均匀溶液后,在搅拌下,加入到Co2+离子源乳液体系中,继续超声机械搅拌0.5h后,通入N20.5h,之后负压下静置除泡2h,注入到15×5×1mm3的PE模具中,快速真空冷冻-干燥成型,取出产品用PE薄膜袋真空封装并置于室温下解冻。经过3次循环冷冻-解冻过程后,用电子束加速器辐照,选用辐照剂量为30kGy,剂量率为10kGy/pass的条件进行辐照,即可制备磁性钴可回收纳米复合水凝胶催化材料。在制得的水凝胶样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒.
磁性钴可回收纳米复合水凝胶催化材料的交联度和吸水性能测试采用CN1273128A中报道方法进行检测,其结果如下:交联度为36%,平衡吸水率为231.5%。取定量产品投入200mL、5mg/L的苯并噻唑前体(如,二甲基氨基二硫代甲酸苯酯模拟物)中,在室温下,对模拟物进行有机催化实验,反应3h后,测得转化率达到98%。
实施例5:取七水硫酸钴0.376g、叔丁醇0.753g,分别加入到25ml去离子水中,超声0.5h,形成形成稳定的Co2+离子源乳液体系。将0.376gN-异丙基丙烯酰胺投入到60℃的7ml去离子水中,搅拌速率为150r/min,加热搅拌时间2h,完全溶解后,冷却至20℃,分别加入3.765g羧甲基壳聚糖、0.376g亚氨基二乙酸,搅拌1h,使其完全溶解形成均匀溶液后,在搅拌下,加入到Co2+离子源乳液体系中,继续超声机械搅拌0.5h后,通入N20.5h,之后负压下静置除泡2h,注入到15×5×1mm3的PE模具中,快速真空冷冻-干燥成型,取出产品用PE薄膜袋真空封装并置于室温下解冻。经过3次循环冷冻-解冻过程后,用电子束加速器辐照,选用辐照剂量为80kGy,剂量率为40kGy/pass的条件进行辐照,即可制备磁性钴氧化物可回收纳米复合水凝胶催化材料。在制得的水凝胶样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒。
磁性钴氧化物可回收纳米复合水凝胶催化材料的交联度和吸水性能测试采用CN1273128A中报道方法进行检测,其结果如下:交联度为60%,平衡吸水率为100%。取定量产品投入250mL、5mg/L的苯并噻唑前体(如,二甲基氨基二硫代甲酸苯酯模拟物)中,在60℃下,对模拟物进行有机催化实验,反应3h后,测得转化率达到93%。
最后应说明的是:以上实施例仅用以说明本发明而并非限制本发明所描述的技术方案;因此,尽管本说明书参照上述的各个实施例对本发明已进行了详细的说明,但是,本领域的普通技术人员应当理解,仍然可以对本发明进行修改或等同替换;而一切不脱离本发明的精神和范围的技术方案及其改进,其均应涵盖在本发明的权利要求范围中。
Claims (7)
1.一种磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于,包括步骤:
①、利用超声波,将1.0~6.0份羟基自由基清除剂、85~93份蒸馏水或去离子水共同分散0.5~4.0份离子源0.5~2h,使其均匀形成稳定的溶液体系;
②、取天然聚多糖5~15份、辐照敏化剂0.5~2.0份、pH调节剂0.1份~2.0份溶于蒸馏水或去离子水中,搅拌制成均匀高分子溶液;
③、将步骤②所得中间产品缓慢加入到步骤①所得的离子源溶液体系,超声搅拌均匀后,通入N2约为0.5~1h,之后负压下静置除泡;
④、将步骤③所得混合体系注射至PE密封袋中(厚度2mm),并置于电子束下进行原位还原与辐射交联反应,选择的电子束能量为1~5MeV,辐射剂量为20~80kGy,剂量率为5~40kGy/pass,最后所得的产物即为磁性可回收纳米复合水凝胶催化材料;
⑤、将步骤④所得样品经水洗、干燥、粉碎、过筛、分级,即得不同颗粒度的凝胶催化材料微球颗粒。
2.根据权利要求1所述的磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于:所述的天然聚多糖为壳聚糖及其衍生物、纤维素及其衍生物、海藻酸钠等中的一种或几种。
3.根据权利要求1所述的磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于:所述的辐照敏化剂为胶原蛋白、聚乙烯醇、N-异丙基丙烯酰胺等中的一种或几种。
4.根据权利要求1所述的磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于:所述的羟基自由基清除剂为异丙醇、叔丁醇、邻羟基苯甲酸、对苯二甲酸等中的一种或几种。
5.根据权利要求1所述的磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于,所述的离子源为七水硫酸亚铁,九水硫酸铁,六水硝酸亚钴,七水硫酸钴,六水硫酸镍,六水硝酸镍中的一种或几种。
6.根据权利要求1所述的磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于,所述的pH调节剂为磷酸氢二钠、磷酸二氢钠、碳酸氢三钠、己二酸、乙酸、Tris-HCl、亚氨基二乙酸、三乙醇胺中的一种或几种。
7.根据权利要求1所述的磁性可回收纳米复合水凝胶催化材料的原位辐射制备方法,其特征在于,制得的凝胶催化材料微球颗粒的交联度为20%~60%,平衡吸水率为100%~1200%。
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