CN108855157B - 一种磷酸锌光催化剂及其制备方法与应用 - Google Patents
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- 229910000165 zinc phosphate Inorganic materials 0.000 title claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 title claims abstract description 19
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical group C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 15
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 15
- 239000002957 persistent organic pollutant Substances 0.000 claims description 11
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- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 5
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000356 contaminant Substances 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000013032 photocatalytic reaction Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 abstract description 16
- 239000011701 zinc Substances 0.000 abstract description 13
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
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Abstract
本发明公开了一种磷酸锌光催化剂,该光催化剂的化学式为Zn3(PO4)2·2H2O,呈纳米片结构,规格尺寸为:厚度为300‑500 nm,大小为(10‑15μm)×(20‑25μm)。本发明通过简单的水热反应即可制备得到性能优越的光催化材料Zn3(PO4)2·2H2O。另一方面,相较于无结晶水的Zn3(PO4)2,我们所合成的Zn3(PO4)2·2H2O光催化剂的活性,提高了1.92倍,具有良好的应用前景。
Description
技术领域
本发明涉及一种新型磷酸锌光催化剂及其简易制备方法、以及光催化活性。
背景技术
进入21世纪,人类面临着能源和环境两个非常严峻的问题,特别是有毒且难降解有机污染物(如多环芳烃、多氯联苯、农药、染料等)引起的环境问题,已成为影响人类生存与健康的重大问题。利用半导体氧化物材料在太阳光照射下表面能受激活化的特性,可有效地氧化分解有机污染物。与传统的净化环境处理方法相比,半导体光催化技术拥有反应条件温和、无二次污染、操作简单和降解效果显著等优势。磷酸锌作为最重要的一种磷酸盐,被广泛应用于涂料、电极以及自动化等工业领域。近年来,磷酸盐由于其在工业、商业以及科学上的大量应用而得到了广泛关注。在已有的报道中,胡云章等人报道了一种磷酸锌疫苗佐剂(申请公布号:CN 101972477A)。调研表明,尚未有含结晶水的磷酸锌作为光催化材料的报道。
发明内容
本发明的目的是为了解决现有技术中存在的缺陷,提供一种制备方法简单,且光催化性能优异的新型材料。
为了达到上述目的,本发明提供了一种磷酸锌光催化剂,该光催化剂的化学式为Zn3(PO4)2·2H2O,呈纳米片结构,规格尺寸为:厚度为300-500 nm,大小为(10-15 μm)×(20-25 μm)。
本发明还提供了上述磷酸锌光催化剂的制备方法,包括以下步骤:
1)在烧杯中加入30mL水,搅拌条件下,加入3mmol的六水合硝酸锌;
2)加入2mmol的磷酸氢二铵,搅拌30min;
3)然后,将步骤(2)中制备得到的混合体系加入到聚四氟乙烯内衬中,180℃恒温水热反应24小时;反应24小时后,自然冷却至室温,离心、洗涤、干燥后得产物Zn3(PO4)2·4H2O;
4)将步骤(3)所得产物加入无水乙醇中,搅拌1.5小时;随后将悬浮液加入到聚四氟乙烯内衬中,180℃恒温水热反应24小时;反应24小时后,自然冷却至室温,离心、洗涤、干燥,产物即为Zn3(PO4)2·2H2O。
本发明还提供了上述磷酸锌光催化剂在有机污染物光催化降解方面的应用。
具体在进行有机污染物光催化降解时,在有机污染物废水溶液中加入所述磷酸锌光催化剂,避光搅拌30min后,开启氙灯光源在紫外光照射下进行光催化反应165-180min,即可;其中,有机污染物废水水溶液的浓度不高于于50mg/L;磷酸锌光催化剂的加入量为每200mL有机污染物废水溶液加入0.1g。
进行光催化降解的有机污染物优选亚甲基蓝。
本发明相比现有技术具有以下优点:
本发明通过简单的水热反应即可制备得到性能优越的光催化材料Zn3(PO4)2·2H2O。另一方面,相较于无结晶水的Zn3(PO4)2,我们所合成的Zn3(PO4)2·2H2O光催化剂的活性,提高了1.92倍,具有良好的应用前景。
本发明制备方法简易、成本低廉,具有可重现性,紫外光下能够很好降解亚甲基蓝(MB)废水溶液。
附图说明
图1为实施例一制备的Zn3(PO4)2·2H2O及对比实施例二制备的Zn3(PO4)2的X射线衍射(XRD)图;
图2为实施例一制备的Zn3(PO4)2·2H2O光催化剂的扫描电子显微镜(SEM)图;
图3为效果实施例三,Zn3(PO4)2·2H2O光催化剂及Zn3(PO4)2对亚甲基蓝(MB)染料废水溶液降解的活性对比图;
其中C0为MB的初始浓度,C为经过紫外光照射一段时间后测量的MB浓度,t为时间。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
实施例一:
室温下,将3mmol的六水合硝酸锌加入盛有30mL水溶液的烧杯中,搅拌20分钟;然后加入2mmol的磷酸氢二铵,搅拌半小时后,转移到聚四氟乙烯内衬中,180℃恒温水热反应24小时;反应24小时后,自然冷却至室温,离心、洗涤、干燥;将所得产物加入30mL无水乙醇中,搅拌1.5小时;随后将悬浮液加入到聚四氟乙烯内衬中,180℃恒温水热反应24小时;反应24小时后,自然冷却至室温,离心、洗涤、干燥,产物即为Zn3(PO4)2·2H2O。
由图1可以看出,实施例一制备的产品与Zn3(PO4)2·2H2O标准卡(JCPDS:10-0333)一致,实施例一制备产品是纯相Zn3(PO4)2·2H2O 2光催化剂。
由图2可见,本发明制备的Zn3(PO4)2·2H2O产品形貌为纳米片厚度在300-500 nm左右,大小为(10-15 μm)×(20-25 μm)左右。
对比实施例二:
将实施例一制备得到的产物放到马弗炉中,600℃恒温煅烧反应6小时,得到Zn3(PO4)2。
由图1可以看出,对比实施例二制备的产品Zn3(PO4)2标准卡(JCPDS: 29-1390)一致,该产品是Zn3(PO4)2光催化剂。
效果实施例三:
测试过程如下:
将实施例一制得到的Zn3(PO4)2·2H2O光催化剂、对比实施例二制得的Zn3(PO4)2,降解含有MB的废水溶液。
分别称取上述两个实施例制备得到的样品0.1g,分别加入200ml MB水溶液,其中MB浓度都50mg/L,先避光搅拌30min,使染料在催化剂表面达到吸附/脱附平衡。然后开启氙灯光源在紫外光照射下进行光催化反应,上清液用分光光度计检测。根据Lambert–Beer定律,有机物特征吸收峰强度的变化,可以定量计算其浓度变化。当吸光物质相同、厚度相同时,可以用吸光度的变化直接表示溶液浓度的变化。因为MB在663 nm处有一个特征吸收峰,所以可以利用吸光度的变化来衡量溶液中MB的浓度变化。
如图3所示(横坐标:紫外光照射时间;纵坐标:经过紫外光照射一段时间后测量的MB浓度值与MB的初始浓度的比值),相较于无结晶水的Zn3(PO4)2,实施例一所合成的Zn3(PO4)2·2H2O光催化剂的活性,提高了1.92倍。
Claims (5)
1.一种磷酸锌光催化剂,其特征在于:所述光催化剂的化学式为Zn3(PO4)2·2H2O;所述磷酸锌光催化剂呈纳米片结构,规格尺寸为:厚度为300-500nm,大小为(10-15μm)×(20-25μm)。
2.权利要求1所述磷酸锌光催化剂的制备方法,其特征在于:包括以下步骤:
1)在烧杯中加入30mL水,搅拌条件下,加入3mmol的六水合硝酸锌;
2)加入2mmol的磷酸氢二铵,搅拌30min;
3)然后,将步骤(2)中制备得到的混合体系加入到聚四氟乙烯内衬中,180℃恒温水热反应24小时;反应24小时后,自然冷却至室温,离心、洗涤、干燥后得产物Zn3(PO4)2·4H2O;
4)将步骤(3)所得产物加入无水乙醇中,搅拌1.5小时;随后将悬浮液加入到聚四氟乙烯内衬中,180℃恒温反应24小时;反应24小时后,自然冷却至室温,离心、洗涤、干燥,产物即为Zn3(PO4)2·2H2O。
3.权利要求1所述磷酸锌光催化剂在有机污染物光催化降解方面的应用。
4.根据权利要求3所述的应用,其特征在于:所述磷酸锌光催化剂在进行有机污染物光催化降解时,在有机污染物废水溶液中加入所述磷酸锌光催化剂,避光搅拌30min后,开启氙灯光源在紫外光照射下进行光催化反应165-180min,即可;所述有机污染物废水溶液的浓度不高于50mg/L;所述磷酸锌光催化剂的加入量为每200mL有机污染物废水溶液加入0.1g。
5.根据权利要求4所述的应用,其特征在于:所述有机污染物为亚甲基蓝。
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