CN110433737A - 一种多功能生物质基复合水凝胶的制备方法及其应用 - Google Patents
一种多功能生物质基复合水凝胶的制备方法及其应用 Download PDFInfo
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Abstract
一种多功能生物质基复合水凝胶的制备方法,包括如下步骤:采用水热法合成Fe系金属有机框架,通过光还原法将纳米银负载分散在MOFs上,通过与瓜尔胶物理共混,自交联制备复合水凝胶;复合多功能水凝胶集吸附‑光催化降解染料、油水分离、水体抗菌‑杀菌于一体,在处理工业废水,修复水体环境领域具有广泛的应用前景。
Description
技术领域
本发明属于纳米复合材料制备技术领域,催化降解和水体修复领域,尤其涉及一种多功能生物质基复合水凝胶的制备方法及其应用,其用于复杂废水环境治理的应用。
背景技术
近年来,随着工业经济的不断发展,全球尤其是发展中国家不断出现严重的水体污染问题。有机染料、油类和细菌等污染物对人类健康和生态安全造成的威胁越来越大,如何对复杂的水系统进行有效的处理引起了人们的广泛的关注。有机染料,如亚甲基蓝(MB)和甲基橙(MO)等,由于其芳香结构不可降解,通常被认为是有毒甚至致癌的。目前已经采用了许多技术从水中去除这些复杂的污染物,包括吸附,沉淀,过滤,生物处理等,但这些方法通常成本较高而且处理效果较差。相比于上述方法,光催化降解染料是一种安全、高效、无毒环保、成本低廉的新兴技术,具有良好的应用前景。常用到的光催化材料主要是一些金属半导体,如TiO2、Ag2O、CdS等。专利(CN103111309A)公开了一种制备ZnS-CdS复合半导体的方法,通过构筑双半导体异质结构来提高光催化效果。专利(CN108298632A)通过对TiO2进行K、Nd掺杂提升光催化效果,对染料废水展现出高的可见光降解效果。相比于上述传统金属半导体催化剂,Fe系金属有机框架材料也是一种很好的光催化MOFs材料,具有更大的比表面积,更多的反应活性位点,能够更好的吸附污染物并且与活性位点接触。但是其光电子空穴对相对容易复合,光催化性能有待进一步提高。Liang等人将贵金属纳米粒子Pt、Au负载在Fe系MOFs材料上,用于光催化降解甲基橙,贵金属纳米粒子的负载可提高MOFs的光催化性能(Nano Research,2015, 8(10), 3237-3249)。然而,Pt、Au纳米粒子价格昂贵,且催化材料作为粉体材料,可回收性较差,限制了其规模应用
另外,复杂的受污染水体中还存在多种细菌污染物(如大肠杆菌等),严重危害人们居住环境和身体健康。Ag NPs被公认为是最好的抗菌剂之一,能够有效杀死各种细菌。 专利(CN103181399A)将Ag 掺杂在TiO2薄膜上赋予了材料高效的抗菌效果。油类污染物也是造成水体污染的一大诟病,水体中油类污染物是经常造成动植物的大量死亡的主要原因之一。目前主要手段是通过吸附来进行油水分离。瓜尔胶可通过简单的自组装交联形成多孔水凝胶网络体系,其表面具有大量亲水基团,具有高效的吸水性和疏油性,能够很好的将油水混合物分离。公开号为CN109046400A的中国专利公开了一种将贵金属Pt负载在BiOI微球上构筑异质结提升光催化性能的方法,但负载贵金属Pt成本较高,而且产物不容易回收。公开号为CN108607599A的中国专利文献公开了一种量子点Au/C3N4水凝胶基光催化剂的制备方法,将Au量子点包覆在C3N4表面,然后与多糖水凝胶进行复合,制备出抗菌杀菌、光催化降解染料于一体的功能材料。但该方法采用辐射法对Au量子点进行负载,不仅操作复杂而且成本较高,难以应用于复杂废水环境的治理。
发明内容
为克服上述现有技术的不足,本发明的目的是提供了一种多功能生物质基复合水凝胶的制备方法及其应用,
为实现上述目的,本发明采用的技术方案是:一种多功能生物质基复合水凝胶的制备方法,包括以下步骤:
1)将Fe系金属粉末和均苯三甲酸(H3BTC)混合后,加入10~25ml去离子水搅拌,量取150~200µL氢氟酸(HF 48%)和90-150µL硝酸(HNO3 65%)逐滴加入上述溶液中,继续磁力搅拌15~30min;
2)将步骤1)制备的溶液转移到水热反应釜中,加入结晶试剂,继续搅拌10~20min;在100~150℃温度下持续反应12~24h;反应结束后自然冷却到室温,在4000rpm下离心5min,用乙醇洗涤3~6次,在100℃下真空干燥12h,得到MOFs产物;
3)将0.5~2g MOFs加入150~300ml乙醇和水的混合溶液当中,将Ag系金属盐加入混合溶液中,充分搅拌,然后转移到石英瓶当中,通入N2排除瓶内空气,然后在紫外灯下照射20~60min;最后将所得物用乙醇洗涤4~6次,在100℃下真空干燥12h,得到最终产物Ag NPs@MOFs;
4)将1~3g Ag NPs@MOFs置于20~60ml去离子水中,超声分散30min,然后加入0.33g~2g瓜尔胶粉末快速机械搅拌6~12h,然后按照加入氧化剂让上述物品氧化自交联,静置10~30分钟得到复合水凝胶。
所述的Fe系金属粉末为含Fe金属盐,采用还原Fe粉、硫酸铁、硝酸铁或三氯化铁中的一种,Fe系金属粉末与均苯三甲酸的混合摩尔比为Fe:H3BTC=0.5~2.5:0.67 mol。
所述的结晶试剂为十六烷基三甲基溴化铵(CTAB),其与Fe元素摩尔比为0.3~1.2:1 mol。
所述的混合溶液中,乙醇和水的体积比为1:2;所述的Ag系金属盐为含Ag元素的金属盐,采用硝酸银、氟化银中的一种,加入Ag系金属盐后,溶液的银离子浓度为10~80 mM。
所述的氧化剂为高碘酸钠NaIO4,氧化剂与瓜尔胶的质量比为0.1 ~ 0.5:1。
所述的方法制备的复合水凝胶作为光催化、抗菌、油水分离剂的应用。
本发明的目的通过以下技术方案予以实现:
本发明与现有技术相比,具有以下有益的效果:
本发明将纳米催化材料(Ag NPs@MOFs)与瓜尔胶(GG)结合,制备出三维多孔复合水凝胶,可以充分结合三种材料独特优势,克服常规水体修复材料功能单一的局限性,制备出集吸附-光催化降解染料、抗菌、油水分离多功能于一身的水体修复材料。采用绿色、简单的光还原法在Fe系MOFs上原位制备分散均匀的Ag NPs,借助MOFs多孔结构和高比表面积对AgNPs晶体的生长和分散进行调控,进一步提高Ag NPs@MOFs的反应活性;GG多孔水凝胶的构筑引入不仅对染料污染物和细菌具有富集作用外,还能够很好的负载和分散Ag NPs@MOFs纳米催化材料,一方面可有效避免纳米催化材料团聚而影响其催化和抗菌性能,另一方面可对催化材料进行分散和良好的固载作用,从而进一步促进了催化材料的高效回用。复合多功能水凝胶集吸附-光催化降解染料(100min染料去除率100%,图4)具体效果如下:
1)本发明首次将光催化,油水分离,抗菌技术三者融为一体制备出应用于水环境修复的生物质基凝胶材料,制备方法简单,成本低廉,具有很高的实用价值和应用前景。油水分离中的油包括硅油、环己烷、菜籽油等。
2)Ag NPs的引入一方面提高了MOFs的电子空穴分离性能,促进生物质基凝胶材料的光催化效果,另一方面Ag NPs本身较好的抗菌效果,赋予了凝胶材料良好的抗菌效果。水体抗菌-杀菌于一体,抑菌率高于99%。
3)瓜尔胶(GG)的引入赋予材料高效的油水分离性能,不仅具有良好的水体污染物富集作用,同时能够很好的负载和分散纳米催化材料,一方面避免其团聚影响其催化和抗菌性能,另一方面能够促进纳米粉体催化材料的高效回用。
4)该复合水凝胶为天然生物降解材料,制备方法简单,成本低廉,相比于其他金属半导体催化材料,不会对水体造成二次污染。
5)采用光还原法制备Ag NPs相比于传统化学还原法不需要添加任何化学还原剂,更加清洁、绿色、无毒,而且反应高效。借助MOFs多孔结构和高比表面积能够有效调控AgNPs晶体的生长和分散,进一步提高反应活性。
附图说明
图1为本发明实施例1制备的Ag NPs负载的MOFs的透射电镜图(TEM)。
图2为本发明实施例1制备的Ag NPs@MOFs负载在GG上的扫描电镜图(SEM)。
图3为本发明实施例1制备的Ag NPs@MOFs负载在GG上的红外图(FTIR)。
图4为本发明实施例4 制备的Ag NPs@MOFs/ GG水凝胶对亚甲基蓝的光催化降解图(UV-Vis)。
图5(a)为本发明实施例5制备的Ag NPs@MOFs对大肠杆菌的抗菌示意图。
图5(b)为本发明实施例5制备的Ag NPs@MOFs/ GG水凝胶对大肠杆菌的抗菌示意图。
图6为本发明实施例6制备的Ag NPs@MOFs/ GG水凝胶的油水分离效果图(UV-Vis)。
图7为本发明实施例6制备的Ag NPs@MOFs/ GG水凝胶的油水分离分离效率图。
图8为本发明实施例6制备的Ag NPs@MOFs/ GG水凝胶的油水分离循环效果图。
具体实施方式
下面结合具体实施案例对本发明作进一步详细说明。
多功能生物质基复合水凝胶的制备方法,包括以下步骤:
1)采用水热法合成金属有机框架(MOFs),
称取Fe系金属粉末和0.68g均苯三甲酸(H3BTC),按一定摩尔比混合,加入10~25ml去离子水搅拌。 量取150~200µL氢氟酸(HF 48%)和90-150µL硝酸(HNO3 65%)逐滴加入上述溶液中,继续磁力搅拌15~30min。
2)将上述溶液转移到水热反应釜中,加入一定比例的结晶试剂,继续搅拌10~20min;在100~150℃温度下持续反应12~24h;反应结束后自然冷却到室温,在4000rpm下离心5min,用乙醇洗涤3~6次,在100℃下真空干燥12h,收集产物;
所用Fe系金属粉末为还原Fe粉,硫酸铁,硝酸铁,三氯化铁等,与均苯三甲酸混合摩尔比为Fe :H3BTC=0.5~2.5:0.67 mol;
所加入结晶试剂与Fe元素摩尔比为0.3~1.2:1 mol;
3)光还原法将Ag NPs负载在MOFs上
将0.5~2g MOFs加入150~300ml乙醇和水的混合溶液当中,称取一定量的Ag系金属盐加入混合溶液中,充分搅拌,然后转移到石英瓶当中,通入N2排除瓶内空气,然后在紫外灯下照射20~60min。最后将样品用乙醇洗涤4~6次,在100℃下真空干燥12h,得到最终产物;
乙醇和水的混合溶液体积比为1:2,所述的Ag系金属盐为含Ag元素的金属盐,采用硝酸银、氟化银中的一种,加入溶液后银离子浓度为10~80mM;
4)Ag NPs@ MOFs与瓜尔胶(GG)自交联制备复合水凝胶
将1~3g Ag NPs@MOFs置于20~60ml去离子水中,超声分散30min,然后加入0.33g~2g GG粉末快速机械搅拌6~12h,然后按照一定的质量比加入氧化剂让样品氧化自交联,静置10~30分钟得到复合水凝胶;
加入氧化剂为高碘酸钠NaIO4, 与GG的质量比为(0.1g~0.5g)NaIO4:1g GG。
实施例1
称取0.27g还原Fe粉和0.68g均苯三甲酸(H3BTC),加入10ml去离子水搅拌,量取150µL氢氟酸(HF 48%)和90µL硝酸(HNO3 65%)逐滴加入上述溶液中,继续磁力搅拌15min;
将上述溶液转移到水热反应釜中,加入0.35g结晶试剂十六烷基三甲基溴化铵(CTAB),继续搅拌15min,在120℃温度下持续反应12h;反应结束后自然冷却到室温,在4000rpm下离心5min,用乙醇洗涤3次,在100℃下真空干燥12h,收集产物;
将0.5g MOFs加入150ml乙醇和水的混合溶液当中(乙醇与水体积比为1:2),称取170mg硝酸银加入混合溶液中(浓度为10mM),充分搅拌,然后转移到石英瓶当中,通入N2排除瓶内空气,然后在紫外灯下照射20min;最后将样品用乙醇洗涤4次,在100℃下真空干燥12h,得到最终产物;
将1gAg NPs@MOFs置于20ml去离子水中,超声分散30min,然后加入0.33g GG粉末快速机械搅拌6h,然后加入33mgNaIO4让样品氧化自交联,静置10分钟得到复合水凝胶。图1为实施例1制备的Ag NPs负载的MOFs的透射电镜图(TEM)。可以看出Ag NPs在MOFs材料的表面和内部负载的很均匀。图2为实施例1制备的Ag NPs@MOFs负载在GG上的扫描电镜图(SEM)。可以看出Ag NPs@MOFs在GG表面均匀分散。图3为实施例1 制备的Ag NPs@MOFs负载在GG上的红外图(FTIR)。
实施例2
称取1.98g硫酸铁和,0.86g均苯三甲酸(H3BTC),加入20ml去离子水搅拌,量取170µL氢氟酸(HF 48%)和120µL硝酸(HNO3 65%)逐滴加入上述溶液中,继续磁力搅拌20min;
将上述溶液转移到水热反应釜中,加入0.85g结晶试剂十六烷基三甲基溴化铵(CTAB),继续搅拌10min,在100℃温度下持续反应18h;反应结束后自然冷却到室温,在4000rpm下离心5min,用乙醇洗涤5次,在100℃下真空干燥12h,收集产物;
将1.2g MOFs加入225ml乙醇和水的混合溶液当中(乙醇与水体积比为1:2),称取0.95g氟化银加入混合溶液中(浓度为50mM),充分搅拌,然后转移到石英瓶当中,通入N2排除瓶内空气,然后在紫外灯下照射40min;最后将样品用乙醇洗涤5次,在100℃下真空干燥12h,得到最终产物;
将2g Ag NPs@MOFs置于40ml去离子水中,超声分散30min,然后加入1g GG粉末快速机械搅拌9h,然后加入100mg NaIO4让样品氧化自交联,静置20分钟得到复合水凝胶。
实施例3
称取2g硝酸铁和1.2g均苯三甲酸(H3BTC),加入25ml去离子水搅拌, 量取200µL氢氟酸(HF 48%)和150µL硝酸(HNO3 65%)逐滴加入上述溶液中,继续磁力搅拌30min;
将上述溶液转移到水热反应釜中,加入1.2g结晶试剂十六烷基三甲基溴化铵(CTAB),继续搅拌20min;在150℃温度下持续反应24h;反应结束后自然冷却到室温,在4000rpm下离心5min,用乙醇洗涤6次,在100℃下真空干燥12h,收集产物;
将2g MOFs加入300ml乙醇和水的混合溶液当中(乙醇和水体积比为1:2),称取0.68g的硝酸银加入混合溶液中(80mM),充分搅拌,然后转移到石英瓶当中,通入N2排除瓶内空气,然后在紫外灯下照射60min;最后将样品用乙醇洗涤6次,在100℃下真空干燥12h,得到最终产物;
将3gAg NPs@MOFs置于60ml去离子水中,超声分散30min,然后加入2g GG粉末快速机械搅拌12h,然后加入180mg NaIO4让样品氧化自交联,静置30分钟得到复合水凝胶。
实施例4
实施例4是制备的Ag NPs@MOFs/GG 复合水凝胶光催化降解亚甲基蓝(MB)实验。步骤如下:配置40ml浓度为40mg/L亚甲基蓝溶液,加入0.5g Ag NPs@MOFs/GG,先在黑暗条件下反应50min使反应达到饱和吸脱附平衡,然后在500w氙灯照射下反应,每隔20min取一次样在紫外可见分光光度计(UV-Vis)下测试。结果表明100min后MB被完全降解,如图4所示。
实施例5
实施例5是制备的Ag NPs@MOFs/GG 复合水凝胶对大肠杆菌的抗菌实验。采用抑菌圈法进行实验。从图5(a)和图5(b)b可以看到,负载Ag NPs的Ag NPs@MOFs(i-2)和Ag NPs@MOFs/GG (ii-1)出现了最大的抑菌圈,说明负载纳米Ag后对大肠杆菌的抗菌效果非常显著。不含AgNPs 的MOFs(i-1)和MOFs/GG(ii-2)只表现出微弱的抑菌效果,单独GG(ii-3)无抑菌效果。
实施例6
实施例6是制备的Ag NPs@MOFs/GG 复合水凝胶的油水分离实验。步骤如下:首先将AgNPs@MOFs/GG涂覆在滤纸上,然后固定在直径为80mm的玻璃漏斗上,油水分离前用去离子水润湿。然后将40ml油类物质(如硅油、菜籽油、环己烷)和40ml水混合,倒入漏斗中仅在重力作用下进行油水分离。收集过滤水称重,通过与原来加入水的重量比计算分离效率。结果如图7所示,分离效率高达99%。
图8是实例6制备的Ag NPs@MOFs/ GG水凝胶的油水分离循环效果图,从图中可以看到经过10次循环,分离效率高达95%以上,说明材料具有很好的重复使用性。
Claims (6)
1.一种多功能生物质基复合水凝胶的制备方法,其特征在于,包括以下步骤:
1)将Fe系金属粉末和均苯三甲酸(H3BTC)混合后,加入10~25ml去离子水搅拌,量取150~200µL氢氟酸(HF 48%)和90-150µL硝酸(HNO3 65%)逐滴加入上述溶液中,继续磁力搅拌15~30min;
2)将步骤1)制备的溶液转移到水热反应釜中,加入结晶试剂,继续搅拌10~20min;在100~150℃温度下持续反应12~24h;反应结束后自然冷却到室温,在4000rpm下离心5min,用乙醇洗涤3~6次,在100℃下真空干燥12h,得到MOFs产物;
3)将0.5~2g MOFs加入150~300ml乙醇和水的混合溶液当中,将Ag系金属盐加入混合溶液中,充分搅拌,然后转移到石英瓶当中,通入N2排除瓶内空气,然后在紫外灯下照射20~60min;最后将所得物用乙醇洗涤4~6次,在100℃下真空干燥12h,得到最终产物Ag NPs@MOFs;
4)将1~3g Ag NPs@MOFs置于20~60ml去离子水中,超声分散30min,然后加入0.33g~2g瓜尔胶粉末快速机械搅拌6~12h,然后加入氧化剂让上述物品氧化自交联,静置10~30分钟得到复合水凝胶。
2.根据权利要求1中所述的一种多功能纳米银@金属有机框架/瓜尔胶复合水凝胶的制备方法,其特征在于,所述的Fe系金属粉末为含Fe金属盐,采用还原Fe粉、硫酸铁、硝酸铁或三氯化铁中的一种,Fe系金属粉末与均苯三甲酸的混合摩尔比为Fe:H3BTC=0.5~2.5:0.67mol。
3.根据权利要求1中所述的一种多功能纳米银@金属有机框架/瓜尔胶复合水凝胶的制备方法,其特征在于,所述的结晶试剂为十六烷基三甲基溴化铵(CTAB),其与Fe元素摩尔比为0.3~1.2:1 mol。
4.据权利要求1中所述的一种多功能纳米银@金属有机框架/瓜尔胶复合水凝胶的制备方法,其特征在于,所述的混合溶液中,乙醇和水的体积比为1:2;所述的Ag系金属盐为含Ag元素的金属盐,采用硝酸银、氟化银中的一种,加入Ag系金属盐后,溶液的银离子浓度为10~80 mM。
5.据权利要求1中所述的一种多功能纳米银@金属有机框架/瓜尔胶复合水凝胶的制备方法,其特征在于,所述的氧化剂为高碘酸钠NaIO4,氧化剂与瓜尔胶的质量比为0.1 ~0.5:1。
6.根据权利要求1所述的方法制备的复合水凝胶作为光催化、抗菌、油水分离剂的应用。
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