CN108889322B - 一种纳米片状磷酸银及其制备方法和作为可见光催化剂的应用 - Google Patents
一种纳米片状磷酸银及其制备方法和作为可见光催化剂的应用 Download PDFInfo
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Abstract
本发明公开了一种纳米片状磷酸银及其制备方法和作为可见光催化剂的应用;纳米片状磷酸银具有不规则多边形薄片状结构,边长为微米尺寸,厚度为纳米尺寸。其制备方法是将钼酸铵溶液滴加至硝酸银溶液中搅拌均匀,得到混合液;在所述混合液中滴加磷酸氢二钠溶液,搅拌反应,即得纳米片状磷酸银晶体;该制备工艺简单,成本较低,且纳米片状磷酸银在可见光下对双酚A(BPA)等有机物具有良好的降解效果,可以广泛的应用于有机废水的降解。
Description
技术领域
本发明涉及一种光催化剂,特别涉及一种具有纳米薄片状的磷酸银,还涉及纳米片状磷酸银的制备方法及其作为光催化剂在降解有机废水中的应用,属于有机废水处理技术领域。
背景技术
药品与个人护理用品(PPCPs)及它们各自代谢物与转换产物是近十年来新兴的有机污染物,具有高度水溶性、持久性、生物积累性、长距离迁移的特性,被称作“假性持久性有机污染物”。由于该类物质的使用与人类活动息息相关,所以每天都会有低剂量的药物排入环境中,使人类和环境长时间处于低剂量的暴露状态,严重影响到人类的生存健康和环境生态安全。
目前有机污染物的去除方法有物理法、生物法和化学法三种,生物降解处理周期长,效率低。物理法不能彻底降解有机污染物,化学法具有快速,高效等特点,在有机污染物去除领域发挥了重要的作用。在各类化学处理法中,高级氧化技术(AOPs)具有易于操作、去除效率高、氧化彻底和容易控制等特点,广泛应用处理难降解有机污染物。光催化技术利用太阳光照射半导体产生的空穴和电子从而氧化降解有机污染已经得到广泛的关注,磷酸银作为一种新型的光催化剂,以其超高的量子效率及优异的可见光催化性能备受研究者的青睐。磷酸银的形貌对其性质有较大的影响,不同形貌的磷酸银其光催化活性和稳定性也各不相同。中国专利(公开号:CN104495777A)公开了一种多面体磷酸银纳米材料及其制备方法,其以硝酸银和磷酸盐作为反应原料,以三乙醇胺作为晶体调节剂,通过控制硝酸银与磷酸盐的浓度,从而实现磷酸银形貌的调控,从而获得多面体磷酸银材料,但其并没有明确其催化效果性能好坏。中国专利(CN107442145A)公开了一种多面体磷酸银可见光催化剂的制备方法,其以硝酸银和磷酸氢二钠作为原料,在离子液体和水溶液中通过水热法合成多面体状磷酸银可见光催化剂,其在可见光催化下对有机染料罗丹明B有良好的降解效果,加入1g/L催化剂,在8h内可将10mg/L的罗丹明B降解90%以上。这种多面体状磷酸银其催化效率是相对较低的。
发明内容
针对现有技术中磷酸银光催化材料存在的缺陷,本发明的第一个目的是在于提供一种比表面大、活性位点暴露多、结晶度高、纯度高的大面积纳米薄片状磷酸银。
本发明的第二个目的是在于提供一种操作简单、低成本的制备纳米片状磷酸银的方法。
本发明的第三个目的是在于提供所述片状磷酸银作为有机废水光催化剂的应用,相对其他形貌的磷酸银材料,纳米片状磷酸银催化效率高,在添加量较少的条件下,可以较短时间内获得较高的降解率,达到有效降解污染物的目的。
为实现上述目的,本发明提供了一种纳米片状磷酸银。
优选的方案,所述纳米片状磷酸银具有不规则多边形薄片状结构,边长为微米尺寸,厚度为纳米尺寸。
优选的方案,边长为1~10微米,厚度为50~600纳米。
本发明的纳米片状磷酸银具有大面积纳米薄片状结构,其比表面积大,暴露的活性位点多,催化活性大大提高,且结晶度高,稳定性好。
本发明提供了一种纳米片状磷酸银的制备方法,该方法是将钼酸铵溶液滴加至硝酸银溶液中搅拌均匀,得到混合液;在所述混合液中滴加磷酸氢二钠溶液,搅拌反应,即得纳米片状磷酸银晶体;
其中,硝酸银溶液的浓度为50~82g/L,钼酸铵溶液的浓度为0.1~1.8g/L,磷酸氢二钠溶液的浓度为27~60g/L;钼酸铵溶液、硝酸银溶液和磷酸氢二钠溶液按等体积比反应。
本发明提供的纳米片状磷酸银的制备方法采用钼酸铵溶液作为磷酸银晶体调节剂,通过协调控制钼酸铵溶液、硝酸银溶液、磷酸氢二钠溶液的浓度和物料比例以及添加方式等条件,可以获得形貌为纳米片状,且纯度较高,结晶度高的磷酸银晶体。钼酸铵是作为磷酸银晶体调节剂,其添加比例和浓度控制是比较重要的:如果其相对用量比例较低或者浓度较低,难以调控磷酸银晶体生长成纳米片状结构,形成不规则颗粒形貌;如果其相对用量比例较高或者浓度过高,一方面难以得到纳米片状形貌的磷酸银晶体,起不到晶体调控作用,主要趋向于生长成不规则的颗粒形貌,另一方面,部分钼酸根会以杂质形式掺入磷酸银的晶格中,而得不到纯的磷酸银。同时硝酸银溶液和磷酸氢二钠的浓度对晶体的形貌控制也具有较大的影响,在优选的浓度范围内,有利于获得纳米片状形貌。本发明的钼酸铵溶液通过滴加形式添加至反应体系中,以获得均匀的银络合物体系,有利于后续磷酸银晶体均匀生长。此外,磷酸氢二钠溶液也是以滴加形式添加至反应体系中,主要目的是控制磷酸银晶体的生长速率,一方面防止杂质掺杂,提高磷酸银晶体纯度,另一方面改善磷酸银的结晶性能以获得结晶度高的磷酸银晶体,提高磷酸银晶体稳定性。
优选的方案,钼酸铵溶液的滴加速率为0.5~1.5mL/秒。
优选的方案,在混合液中滴加磷酸氢二钠溶液,在200~300转/分钟的搅拌速率下反应18~30小时。
优选的方案,硝酸银溶液的浓度为60~70g/L,钼酸铵溶液的浓度为1~1.6g/L,磷酸氢二钠溶液的浓度为30~40g/L。
优选的方案,磷酸氢二钠溶液的滴加速率为0.5~1.5mL/秒。
本发明还提供了一种纳米片状磷酸银的应用,其作为可见光催化剂应用于光催化降解有机废水。
本发明的纳米片状磷酸银催化有机废水的过程(以含BPA的有机废水为例):在可见光下,将磷酸银催化剂加入BPA有机废水中,磷酸银催化剂的用量为1g/L,BPA浓度为15mg/L,1h的降解率可达到95%。磷酸银催化剂的用量根据BPA浓度实际情况进行调节。
本发明的片状磷酸银可见光催化剂的制备方法,包括以下具体步骤:
1)将硝酸银溶于去离子水中,在常温常压下采用超声波进行震荡,使硝酸银充分的溶解于水中,同时将钼酸铵溶于去离子水中,在搅拌下,将钼酸铵溶液逐滴的滴加到硝酸银溶液当中,形成乳白色溶液;钼酸铵的浓度为0.1~1.8g/L,加入量为30~50mL所述钼酸铵的添加速度为1mL/秒;硝酸银溶液浓度为50~82g/L,加入量为30~50mL
2)将磷酸氢二钠溶于去离子水中,并逐滴的加入到上述乳白色溶液中,以200~300转/分钟的转速磁力搅拌24小时,过滤,60~80摄氏度烘干、研磨,得固体黄色粉末,即得到片状磷酸银光催化剂;磷酸氢二钠浓度为27~60g/L,加入量为30~50mL。
与现有技术相比,本发明的技术方案带来的有益技术效果是:
1)本发明的磷酸银具有特殊纳米片状形貌,比表面大,活性位点暴露多,催化活性高。
2)本发明的磷酸银结晶性好,稳定性高,且纯度高。
3)本发明的制备方法操作简单,成本较低。
4)本发明的纳米片状磷酸银相对现有普通形貌的磷酸银具有更高光催化活性,以处理有机污染物双酚A(BPA)为例,得到光催化效果明显,有机物降解率较高,可广泛用于有机废水的降解领域。
附图说明
【图1】为片状磷酸X射线衍射(XRD);
【图2】为片状磷酸银扫描电镜(SEM);
【图3】为片状磷酸银降解BPA降解率图;
【图4】为对比实施3制备的磷酸银扫描电镜(SEM)。
具体实施方式
以下实施例旨在进一步说明本发明内容,而不是限制本发明权利要求的保护范围。
实施例1
(1)采用共沉淀法制备片纳米状磷酸银光催化剂。
制备纳米片状磷酸银:将硝酸银加入超纯水中,配成浓度为60.65g/L的硝酸银溶液40mL,磁力搅拌,同时将0.5g/L的钼酸铵溶液40mL以1mL/秒的速度滴加到硝酸银溶液当中,生成白色絮状,再向其中以1mL的速度滴入37.3g/L的磷酸氢二钠溶液40mL,以250转/分钟的转速磁力搅拌24小时,确保磷酸银可以生长成纳米片状结构,过滤,60℃烘12h,得到固体黄色粉末,标记为磷酸银-1。
(2)降解BPA:将0.2g纳米片状磷酸银加入200mL浓度为15mg/L的BPA溶液中,转移至多功能光化学反应仪中,在300W氙灯照射下进行光催化反应。隔不同时间取样,离心分离,取上层清液,用液相色谱仪测其BPA反应前后的浓度,计算降解率。
磷酸银-1的XRD如图1,可以看出其与磷酸银的XRD标准卡片峰是完全吻合的,且没有出现杂质峰,显示出纯Ag3PO4的衍射峰。
磷酸银-1的SEM图如图2,从图2中可以看出合成的磷酸银是边长为1~10微米的不规则多边体,且厚度为50~600纳米,为纳米薄片状结构。
磷酸银-1在可见光照射下对BPA的降解率曲线如图3,可见光下照射20min对BPA的光降解率为91%。
实施例2
制备步骤同实施例1,所不同的是加入钼酸铵的量为1g/L,标记为磷酸银-2,由图1可知合成的是纯磷酸银,该磷酸银是边长为1~10微米的不规则多边体,厚度在50~600纳米范围内的片状结构,降解率如图3所示,20min对BPA的光降解率为96%。
实施例3
制备步骤同实施例1,所不同的是加入钼酸铵的量为1.6g/L,标记为磷酸银-3,由图1可知合成的是纯磷酸银,该磷酸银是边长为1~10微米的不规则多边体,厚度在50~600纳米范围内的片状结构,降解率如图3所示,20min对BPA的光降解率为96%。
对比实施例1
制备步骤同实例1,所不同的是不加入钼酸铵,标记为磷酸银-0,合成的磷酸银是边0.5~3微米的八面体块状结构,20min对BPA的降解率为30%。
对比实施例2
制备步骤同实例1,所不同的是加入钼酸铵的量为7.63g/L,由XRD图可知合成的为磷钼酸银/磷酸银,20min对BPA的降解率为80%。
对比实施例3
制备步骤同实例1,所不同的是加入钼酸铵溶液的浓度为0.05g/L,由XRD图可知合成的为磷酸银,其形貌不规则的微米级颗粒为主,以20min对BPA的降解率为82%。
以上,例举的实施例仅为本发明的较佳实施例,并非仅限于本发明的实施范围,凡依本发明范围的内容所做的等效变化和修饰,都应为本发明的技术范畴。
Claims (6)
1.一种纳米片状磷酸银的制备方法,其特征在于:将钼酸铵溶液滴加至硝酸银溶液中搅拌均匀,得到混合液;在所述混合液中滴加磷酸氢二钠溶液,搅拌反应,即得纳米片状磷酸银晶体;其中,硝酸银溶液的浓度为50~82g/L,钼酸铵溶液的浓度为0.1~1.8g/L,磷酸氢二钠溶液的浓度为27~60g/L;钼酸铵溶液、硝酸银溶液和磷酸氢二钠溶液按等体积比反应。
2.根据权利要求1所述的一种纳米片状磷酸银的制备方法,其特征在于:具有不规则多边形薄片状结构,边长为微米尺寸,厚度为纳米尺寸。
3.根据权利要求2所述的一种纳米片状磷酸银的制备方法,其特征在于:边长为1~10微米,厚度为50~600纳米。
4.根据权利要求1所述的一种纳米片状磷酸银的制备方法,其特征在于:钼酸铵溶液的滴加速率为0.5~1.5mL/秒。
5.根据权利要求1所述的一种纳米片状磷酸银的制备方法,其特征在于:在混合液中滴加磷酸氢二钠溶液,在200~300转/分钟的搅拌速率下反应18~30小时。
6.根据权利要求5所述的一种纳米片状磷酸银的制备方法,其特征在于:磷酸氢二钠溶液的滴加速率为0.5~1.5mL/秒。
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