CN116099384A - 一种尖晶石纳米颗粒改性的陶瓷膜制备方法 - Google Patents
一种尖晶石纳米颗粒改性的陶瓷膜制备方法 Download PDFInfo
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Abstract
本发明专利涉及分离膜材料技术领域,具体为一种尖晶石纳米颗粒改性的陶瓷膜制备方法。本发明通过尿素模板牺牲法以及高温核化和晶化处理技术在陶瓷膜表面和孔隙壁上原位制备纳米尖晶石型催化剂,在陶瓷膜孔隙中构建了“纳米催化反应器”,纳米尺寸的尖晶石型催化,比表面积大,催化活化双氧水产生羟基自由基,原位降解陶瓷膜孔隙中的不可污染物。该改性方法不影响陶瓷膜的渗透通量,而且陶瓷膜污堵后不需要酸碱化学清洗,不污染环境,不劣化陶瓷膜材料和膜组件,可广泛应用于生活污水处理的膜生物反应器和饮用水的深度净化等领域。
Description
技术领域
本发明专利涉及无机及多孔材料技术领域,特别涉及陶瓷分离膜材料技术领域,具体为一种尖晶石纳米颗粒改性的陶瓷膜制备方法。
背景技术
目前,为了响应国家可持续发展战略,高效的处理水污染已经成为了重要的焦点问题。当前用于污水水处理与饮用水净化中最常见的是膜分离技术,膜分离技术具有高效、节能、无相变、操作方便、无二次污染等优点,成为缓解资源短缺、能源危机和治理环境污染的重要措施,并得到世界各国的普遍重视。
膜元件按照材质可分为有机膜和陶瓷膜。与有机膜相比,陶瓷膜具有更好的机械性能和化学稳定性,既能在较高的膜渗透通量下稳定运行,又能承受高的反冲洗强度以取得更好的反冲洗效果。但是陶瓷膜在用于水处理、水资源回收利用或者饮用水深度净化过程中,会不可避免的遭受膜污染问题。
陶瓷膜的污染是指在过滤过程中,被过滤水体中的微粒、胶态粒子或溶解性物质与膜之间存在物理、化学、生物或机械相互作用而在膜表面形成滤饼层或在膜孔内吸附、沉积使膜孔窄化或堵塞,导致膜过滤性能和分离特性大大下降的现象。膜污染造成的最直接的后果就是降低了膜的过滤性能,使水通量下降,从而提高了应用成本。根据水力反洗对膜通量的恢复情况可以将膜污染分为:可逆污染和不可逆污染。可逆污染主要由膜表面的累积滤饼层导致,可以通过水洗或气水反洗去除;不可逆污染主要是在化学作用或生物作用下,小分子物质在膜表面或膜孔内吸附造成的,通过物理清洗方法很难去除。由于不可逆污染较去除比较困难,是导致膜污染降的主要原因,因此不可逆污染去除成为膜科学研究的重点。
目前,市场上常用于处理不可逆污染的方法是酸洗和碱洗,酸洗碱洗对于陶瓷膜的通量恢复确实有一定效果,但处理时间过长或处理次数过多会对陶瓷膜造成不可挽回的损伤,即导致膜劣化,因此,如何找到一种既能处理陶瓷膜的不可逆污染,又能不对膜造成损伤的方法十分关键。
发明内容
本发明的目的是针对上述陶瓷膜过滤过程中不可避免的膜污染的瓶颈问题,以及酸洗和碱洗带来膜材料劣化等问题,提出一种在陶瓷膜表面和孔隙中原位生长尖晶石纳米颗粒(MnFe2O4),用来催化活化双氧水降解陶瓷膜孔隙中不可逆污染物的方法。原位生长的尖晶石纳米颗粒是通过尿素模板牺牲法以及高温核化和晶化处理技术,缓释效果优异,不会导致溶出物重金属超标问题。尖晶石纳米颗粒催化活化双氧水产生羟基自由基,可以无选择性氧化降解陶瓷膜中的不可逆污染,高效、安全和稳定。
为了达到上述目的,本发明通过以下技术方案来实现:
一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:该改性陶瓷膜的制备包括以下步骤:(1)催化剂前驱体液的制备,(2)陶瓷膜饱和吸附,(3)目标金属纳米颗粒均匀沉积处理,(4)高温晶化热处理。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(1)是称取一定量的尿素,加入去离子水中,随后称取一定浓度的Fe(NO3)3·9H2O与Mn(NO3)2·4H2O,加入去离子水中,搅拌至完全溶解,获得深红色的催化剂前驱体溶液。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(1)中,所述的Fe(NO3)3·9H2O浓度为0.1~1mol/L。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(1)中,所述的Mn(NO3)2·4H2O浓度为0.05~0.5mol/L。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(2)是将陶瓷膜浸泡在步骤(1)中制备的深红色前驱体溶液中1-12h。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(3)是将步骤(2)中浸泡后的陶瓷膜放入90℃的烘箱中保温1-12h。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(4)是将步骤(3)中均匀沉积处理后的陶瓷膜放入马弗炉中,升温至450℃保温3h进行高温晶化热处理。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(1)中所述的尿素、Fe(NO3)3·9H2O和Mn(NO3)2·4H2O摩尔比为Fe:Mn=2:1。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(2)中所述的陶瓷膜膜形状是管式单通道、管式多通道、密集多通道或平板状。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(2)中所述的陶瓷膜材质是氧化铝、氧化锆、氧化钛、氧化硅、碳化硅或上述几种制备的复合陶瓷膜。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(2)中所述的陶瓷膜孔径范围是0.04~1μm。
作为优选,上述一种尖晶石纳米颗粒改性的陶瓷膜制备方法的步骤(4)中所述的马弗炉气氛环境是空气气氛。
本发明一种尖晶石纳米颗粒改性的陶瓷膜制备方法的技术方案有如下的有益效果:
1.本发明所述的尖晶石纳米颗粒改性的陶瓷膜陶瓷膜经过尿素模板牺牲法和晶化热处理技术制备的纳米级FeMn2O4尖晶石颗粒在陶瓷膜中分布均匀,稳定性非常好,24h浸泡水后平均Fe、Mn含量仅为0.009mg/L,低于《生活饮用水卫生标准》(GB5749-2006)中规定的1mg/L,展现出优异的安全性能。
2.本发明所述的尖晶石纳米颗粒改性的陶瓷膜被严重污染后,用一定浓度的双氧水浸泡膜片,即可催化降解陶瓷膜孔隙中的污染物,但是不会破坏陶瓷膜内结构。
3.本发明所述的尖晶石纳米颗粒改性的陶瓷膜表面和孔隙通过尿素模板牺牲法形成的纳米尖晶石(FeMn2O4)颗粒小,分布均匀,对陶瓷膜的渗透通量无明显影响。
4.本发明所述的尖晶石纳米颗粒改性的陶瓷膜制备方法简单、与双氧水的催化作用效果好且规模化实施可行性好。
具体实施方式:
下面结合实例进一步说明本发明,但并不是本发明内容范围的任何限制。
实施例1
步骤(1)是称取尿素作为模板,倒入去离子中,搅拌至全部溶解;随后称取Fe(NO3)3·9H2O与Mn(NO3)2·4H2O,在确保摩尔比为Fe:Mn=2:1时,将称取好的Fe(NO3)3·9H2O与Mn(NO3)2·4H2O加入尿素溶液中,充分搅拌,全部溶解后得到无沉淀且深红色的透明溶液。
步骤(2)是将孔径为0.1μm的碳化硅平板陶瓷膜浸泡在步骤(1)中制备的深红色透明溶液中1h。
步骤(3)是将步骤(2)中浸泡后的碳化硅平板陶瓷膜取出,随后放入90℃烘箱中保温12h,确保目标纳米颗粒在陶瓷膜表面及孔隙中完全沉积。
步骤(4)是将步骤(3)完全沉积的碳化硅陶瓷膜放入马弗炉中,在450℃下保温3h进行高温晶化热处理。
实施例2
步骤(1)是1中制备的尖晶石纳米颗粒改性的陶瓷膜进行纯水通量测试,在-0.01MPa在,原碳化硅平板陶瓷膜渗透通量是1203.6LMH,尖晶石纳米颗粒改性的陶瓷膜渗透通量为1196.8LMH。这充分说明利用尿素模板牺牲法在陶瓷膜表面和孔隙中制备的纳米尖晶石(FeMn2O4)颗粒,对陶瓷膜的渗透通量的影响不是很明显。
实施例3
将实施例1中制备的尖晶石纳米颗粒改性的陶瓷膜与原碳化硅陶瓷膜进行油水乳浊液的分离性能,并通过双氧水渗透陶瓷膜进行纯水通量恢复的性能测试,测试结果如下表:
实施例数据对比:
以上所述,仅为本发明专利较佳实施例而已,不能依次限定本发明实施的范围,即依本发明专利范围及说明书内容所着的等效变化及修饰,皆应属于本发明涵盖的范围内。
Claims (7)
1.一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:包括以下步骤:
(1)催化剂前驱体液的制备;是称取一定量的尿素,加入去离子水中,随后称取一定量的Fe(NO3)3·9H2O与Mn(NO3)2·4H2O,加入去离子水中,搅拌至充分溶解,获得深红色的前驱体溶液;
(2)陶瓷膜饱和吸附:将陶瓷膜浸泡在步骤(1)中制备的深红色前驱体溶液中1-12h;
(3)目标金属纳米颗粒均匀沉积处理;将步骤(2)中浸泡后的陶瓷膜放入90℃的烘箱中保温1-12h;
(4)高温晶化热处理:将步骤(3)中均匀沉积处理后的陶瓷膜放入马弗炉中,升温至450℃保温3h进行高温晶化热处理。
2.如权利要求1所述的一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:步骤(1)中,所述的Fe(NO3)3·9H2O浓度为0.1~1mol/L。
3.如权利要求1所述的一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:步骤(1)中,所述的Mn(NO3)2·4H2O浓度为0.05~0.5mol/L。
4.如权利要求1所述的一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:步骤(1)中所述的添加的Fe(NO3)3·9H2O与Mn(NO3)2·4H2O中,摩尔比为Fe:Mn=2:1。
5.如权利要求1所述的一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:步骤(2)中所述的陶瓷膜膜形状是管式单通道、管式多通道、密集多通道或平板状。
6.如权利要求1所述的一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:步骤(2)中所述的陶瓷膜材质是氧化铝、氧化锆、氧化钛、氧化硅、碳化硅或上述几种制备的复合陶瓷膜。
7.如权利要求1所述的一种尖晶石纳米颗粒改性的陶瓷膜制备方法,其特征在于:步骤(2)中所述的陶瓷膜孔径范围是0.04~1μm。
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