CN108676123B - 一种均匀分散型光催化水凝胶的制备方法 - Google Patents
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Abstract
本发明公开的是一种均匀分散型光催化水凝胶的制备方法,在水凝胶中加入核壳光催化纳米粒子,然后加入过硫酸钾和N,N‑亚甲基双丙烯酰胺,通过UV照射条件下制备出一种具有光催化效果的复合水凝胶,本发明可以制备出具有多孔网状的水凝胶,其网络均匀,纳米粒子分散性好,具有优良的光催化降解污染物的能力,制备过程简单,条件易于控制,便于工业化应用,可以有效地降解甲醛、苯、甲苯、二甲苯、氨、TVOC等污染物,并具有高效广泛的消毒性能。
Description
技术领域
本发明涉及一种水凝胶的制备方法,更具体一点说,涉及一种均匀分散型光催化水凝胶的制备方法。
背景技术
水凝胶是由具有网状交联结构的水溶性高分子中引入一部分疏水基团和亲水残基,亲水残基与水分子结合,将水分子连接在网状内部,而疏水残基遇水膨胀的交联聚合物,其性质柔软,能保持一定的形状,能吸收大量的水,目前人工合成的水凝胶通常存在凝胶强度低、韧性差和吸水速度慢等缺点,无法满足使用的要求,研究者针对提高水凝胶的力学性能开展了大量的研究工作,开发了几类具有优异机械性能的新型凝胶,如拓扑型水凝胶、双网络结构水凝胶、复合水凝胶、大分子微球复合水凝胶、疏水缔合凝胶和均一链结构水凝胶等,其中复合水凝胶,由于具有高强度、复合手段多样化而受到广泛关注,但是目前在复合水凝胶制备中,无机纳米粒子难以均匀分散到有机聚合物网络中,这是由于纳米粒子存在较大界面自由能,导致粒子容易发生团聚,仅仅采用一般的搅拌等方法,很难消除无机纳米粒子与聚合物基体之间高界面能差,而通过化学方法也存在工艺操作复杂、制备困难的缺陷。
发明内容
本发明的目的在于解决现有技术问题,本发明在水凝胶制备时加入羧甲基纤维素钠,然后加入核壳光催化纳米粒子后超声分散,利用化学键结合的方式制备出一种均匀分散的复合水凝胶,进一步进行光催化降解作用,使其具有较好的有机物污染物降解能力。
为了实现上述目的,本发明是通过以下技术方案实现的:
一种均匀分散型光催化水凝胶的制备方法,该制备方法包括如下步骤:
步骤1):向锥形瓶中加入5-15mL去离子水,再加入0.05-0.15g羧甲基纤维素钠,在室温下搅拌溶解20-40min,然后加入0.5-1.5g丙烯酰胺和1-2g丙烯酸,搅拌5-15min,获得混合物A;
步骤2):向步骤1)获得的混合物A中加入5-15mg的核壳光催化纳米粒子,超声分散20-40min,搅拌20-40min,再加入1-3mgN,N-亚甲基双丙烯酰胺,10-30mg过硫酸钾,0.5-1.5g氢氧化钠,搅拌5-10min,获得混合物B;
步骤3):向装有混合物B的锥形瓶中充入N2曝气20-40min,密封,并将锥形瓶放入光化学反应仪中,在磁力搅拌下,采用紫外光进行光照反应0.5-1h,获得粗制的均匀分散型光催化水凝胶;
步骤4):将步骤3)获得的均匀分散型光催化水凝胶取出,用去离子水浸泡去除未反应的单体,获得精制的均匀分散型光催化水凝胶。
作为一种改进,所述核壳光催化纳米粒子包括若干个二氧化钛颗粒,所述二氧化钛颗粒外包裹有一层带有若干个小孔的球型外壳,所述球型外壳为二氧化硅。
作为一种改进,所述核壳光催化纳米粒子纳米细度为6-8纳米。
有益效果:1)可以制备出具有多孔网状的水凝胶,其网络均匀,纳米粒子分散性好;2)制备的水凝胶具有优良的光催化降解污染物的能力;3)制备过程简单,条件易于控制,便于工业化应用;4)可以有效地降解甲醛、苯、甲苯、二甲苯、氨、TVOC等污染物,并具有高效广泛的消毒性能;5)能将细菌或真菌释放出的毒素分解及无害化处理,可以防止油污、灰尘等产生;6)对浴室中的霉菌、水锈、便器的黄碱及铁锈和涂染面褪色等现象同样具有防止其产生的功效;7)具有水污染的净化及水中有机有害物质的净化功能,且表面具有超亲水性;8)本发明创造性采用纳米细度6-8纳米的核壳光催化纳米粒子,使得网络均匀,纳米粒子分散性好,不容易团聚,分散均匀。
附图说明
图1是本发明制备的均匀分散型光催化水凝胶电镜照片之一。
图2是本发明制备的均匀分散型光催化水凝胶电镜照片之二。
图3是实施例1中光催化降解罗丹明B的紫外吸收曲线图。
具体实施方式
以下结合附图并通过具体的实施例对本发明作进一步的说明,但本发明的实施例并不受以下实施例的限制。
实施例1
一种均匀分散型光催化水凝胶的制备方法,该制备方法包括如下步骤:
步骤1):向锥形瓶中加入5mL去离子水,再加入0.05g羧甲基纤维素钠,在室温下搅拌溶解20min,然后加入0.5g丙烯酰胺和1g丙烯酸,搅拌5min,获得混合物A;
步骤2):向步骤1)获得的混合物A中加入5mg的核壳光催化纳米粒子,超声分散20min,搅拌20min,再加入1mgN,N-亚甲基双丙烯酰胺,10mg过硫酸钾,0.5g氢氧化钠,搅拌5min,获得混合物B,所述核壳光催化纳米粒子包括若干个二氧化钛颗粒,所述二氧化钛颗粒外包裹有一层带有若干个小孔的球型外壳,所述球型外壳为二氧化硅,其中所述核壳光催化纳米粒子纳米细度为6纳米,核壳光催化纳米粒细度越小,催化性能越强,但纳米细度细度越小,制作成本越高,性价比不高,特别是纳米细度少于一定程度后,会降低粒子性光能的吸收率,后期越容易团聚,本发明创造性采用纳米细度为6纳米的核壳光催化纳米粒子,使得网络均匀,纳米粒子分散性好,不容易团聚,分散均匀;
步骤3):向装有混合物B的锥形瓶中充入N2曝气20min,密封,并将锥形瓶放入光化学反应仪中,在磁力搅拌下,采用紫外光进行光照反应0.5h,获得粗制的均匀分散型光催化水凝胶;
步骤4):将步骤3)获得的均匀分散型光催化水凝胶取出,用去离子水浸泡去除未反应的单体,获得精制的均匀分散型光催化水凝胶,如图1、2所示,本发明制备的均匀分散型光催化水凝胶具有多孔网状的水凝胶,其网络均匀,纳米粒子分散性好。
将本发明制备获得的均匀分散型光催化水凝胶与未经过光催化降解的均匀分散型水凝胶分别用于光催化降解罗丹明B(其中各成分量等同),如图3所示,通过紫外光进行光照反应0.5h后的均匀分散型光催化水凝胶紫外吸收率更高。
实施例2
一种均匀分散型光催化水凝胶的制备方法,该制备方法包括如下步骤:
步骤1):在室温下搅拌溶解30min,然后加入1g丙烯酰胺和1.5g丙烯酸,搅拌10min,获得混合物A;
步骤2):向步骤1)获得的混合物A中加入10mg的核壳光催化纳米粒子,超声分散30min,搅拌30min,再加入2mgN,N-亚甲基双丙烯酰胺,20mg过硫酸钾,1g氢氧化钠,搅拌7.5min,获得混合物B,所述核壳光催化纳米粒子包括若干个二氧化钛颗粒,所述二氧化钛颗粒外包裹有一层带有若干个小孔的球型外壳,所述球型外壳为二氧化硅,其中所述核壳光催化纳米粒子纳米细度为7纳米,核壳光催化纳米粒细度越小,催化性能越强,但纳米细度细度越小,制作成本越高,性价比不高,特别是纳米细度少于一定程度后,会降低粒子性光能的吸收率,后期越容易团聚,本发明创造性采用纳米细度为7纳米的核壳光催化纳米粒子,使得网络均匀,纳米粒子分散性好,不容易团聚,分散均匀;
步骤3):向装有混合物B的锥形瓶中充入N2曝气30min,密封,并将锥形瓶放入光化学反应仪中,在磁力搅拌下,采用紫外光进行光照反应0.75h,获得粗制的均匀分散型光催化水凝胶;
步骤4):将步骤3)获得的均匀分散型光催化水凝胶取出,用去离子水浸泡去除未反应的单体,获得精制的均匀分散型光催化水凝胶,如图1、2所示,本发明制备的均匀分散型光催化水凝胶具有多孔网状的水凝胶,其网络均匀,纳米粒子分散性好。
实施例3
一种均匀分散型光催化水凝胶的制备方法,该制备方法包括如下步骤:
步骤1):向锥形瓶中加入15mL去离子水,再加入0.15g羧甲基纤维素钠,在室温下搅拌溶解40min,然后加入1.5g丙烯酰胺和2g丙烯酸,搅拌15min,获得混合物A;
步骤2):向步骤1)获得的混合物A中加入15mg的核壳光催化纳米粒子,超声分散40min,搅拌40min,再加入3mgN,N-亚甲基双丙烯酰胺,30mg过硫酸钾,1.5g氢氧化钠,搅拌10min,获得混合物B,所述核壳光催化纳米粒子包括若干个二氧化钛颗粒,所述二氧化钛颗粒外包裹有一层带有若干个小孔的球型外壳,所述球型外壳为二氧化硅,其中所述核壳光催化纳米粒子纳米细度为8纳米,核壳光催化纳米粒细度越小,催化性能越强,但纳米细度细度越小,制作成本越高,性价比不高,特别是纳米细度少于一定程度后,会降低粒子性光能的吸收率,后期越容易团聚,本发明创造性采用纳米细度为8纳米的核壳光催化纳米粒子,使得网络均匀,纳米粒子分散性好,不容易团聚,分散均匀;
步骤3):向装有混合物B的锥形瓶中充入N2曝气40min,密封,并将锥形瓶放入光化学反应仪中,在磁力搅拌下,采用紫外光进行光照反应1h,获得粗制的均匀分散型光催化水凝胶;
步骤4):将步骤3)获得的均匀分散型光催化水凝胶取出,用去离子水浸泡去除未反应的单体,获得精制的均匀分散型光催化水凝胶,如图1、2所示,本发明制备的均匀分散型光催化水凝胶具有多孔网状的水凝胶,其网络均匀,纳米粒子分散性好。
最后,需要注意的是,本发明不限于以上实施例,还可以有很多变形。本领域的普通技术人员能从本发明公开的内容中直接导出或联想到的所有变形,均应认为是本发明的保护范围。
Claims (2)
1.一种均匀分散型光催化水凝胶的制备方法,其特征在于该制备方法包括如下步骤:
步骤1):向锥形瓶中加入5-15mL去离子水,再加入0.05-0.15g羧甲基纤维素钠,在室温下搅拌溶解20-40min,然后加入0.5-1.5g丙烯酰胺和1-2g丙烯酸,搅拌5-15min,获得混合物A;
步骤2):向步骤1)获得的混合物A中加入5-15mg的核壳光催化纳米粒子,超声分散20-40min,搅拌20-40min,再加入1-3mgN,N-亚甲基双丙烯酰胺,10-30mg过硫酸钾,0.5-1.5g氢氧化钠,搅拌5-10min,获得混合物B;所述核壳光催化纳米粒子纳米细度为6-8纳米;
步骤3):向装有混合物B的锥形瓶中充入N2曝气20-40min,密封,并将锥形瓶放入光化学反应仪中,在磁力搅拌下,采用紫外光进行光照反应0.5-1h,获得粗制的均匀分散型光催化水凝胶;
步骤4):将步骤3)获得的均匀分散型光催化水凝胶取出,用去离子水浸泡去除未反应的单体,获得精制的均匀分散型光催化水凝胶。
2.根据权利要求1所述的一种均匀分散型光催化水凝胶的制备方法,其特征在于,所述核壳光催化纳米粒子包括若干个二氧化钛颗粒,所述二氧化钛颗粒外包裹有一层带有若干个小孔的球型外壳,所述球型外壳为二氧化硅。
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