CN114920281A - 一种球形纳米氧化锌的制备方法 - Google Patents
一种球形纳米氧化锌的制备方法 Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims description 13
- 238000000034 method Methods 0.000 claims abstract description 18
- 150000003751 zinc Chemical class 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000012716 precipitator Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical group [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical group [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 14
- 238000006731 degradation reaction Methods 0.000 abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 8
- 239000002351 wastewater Substances 0.000 abstract description 5
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 239000012071 phase Substances 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000000975 dye Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明一种球形纳米氧化锌的制备方法是在可溶性锌盐溶液中，加入醇类表面活性剂，混合均匀，形成可溶性锌盐的混合溶液，其中可溶性锌盐溶液与醇类表面活性剂的体积比为7∶8；将可溶性锌盐的混合溶液水浴加热至90°C，滴入沉淀剂溶液，搅拌加热反应3 h后冷却至室温，再分别经离心分离、洗涤、干燥、研磨和煅烧，得到球形纳米氧化锌，其粒径分布均匀，直径约为20 nm。本发明方法无需使用高温高压设备，工艺简便，氧化锌形貌规整可控，产率高，后处理容易，杂质少，分散度高，应用于有机染料的工业废水催化降解，降解率高，可见光照射1h 20min后，对废水的降解率是锐钛矿相二氧化钛对废水降解率的2倍。
Description
技术领域
本技术涉及一种球形纳米氧化锌的制备方法，具体属于纳米材料技术领域。
背景技术
氧化锌因其较宽的带隙(3.37eV)、较大的激发结合能(60 meV)和优越的物理和化学性质而得到了广泛研究。ZnO作为重要的半导体材料，其比表面积大、生物安全性高，广泛应用于光催化杀菌、环境净化、有机污染物降解等，是一种优良的光催化材料。然而，电子-空穴对的高复合率和较低的日光利用率限制了氧化锌在有机染料降解中的实际应用。其形貌的控制对其活性有重要影响，对ZnO颗粒的形貌进行设计是控制其光催化活性的重要参数。通过改变形貌可以提高比表面积，是光催化反应过程中的一个重要因素。例如，光降解实验结果表明，亚微球(ZOHS)的光降解率高于商业氧化锌纳米颗粒，因为ZOHS的纳米颗粒的平均尺寸更小。([1] Yefei Guo, Xiaonan Fu, Ruijie Liu, et al.. Effificientgreen photocatalyst of Ag/ZnO nanoparticles for methylene bluephotodegradation[J]. J Mater Sci: Mater Electron (2022) 33:2716-2728. [2]Haitham Mohammad Abdelaala, Ahmed Shaikjeeb, Mohamed Esmat. High performingphotocatalytic ZnO hollow sub-micro-spheres fabricated by microwave inducedself-assembly approach[J]. Ceramics International, 2020, 46(12): 19815-19821.)
球形ZnO纳米颗粒通常具有高度对称性结构、独特光响应特性、比表面积较大的优点，在光催化降解有机染料领域应用广泛。球形的氧化锌一般需定向的制备方法，例如水热法、固相法、液相法和气相法、直接沉淀法等。但这些制备方法或均需复杂的反应过程，例如高温反应，或者所得样品粒径分布宽，分散性差，导致光催化活性差。“锌离子-硫氰酸根”体系用于合成形态可控的氧化锌纳米材料。这种合成方法采用超声辅助法，成本低，所得氧化锌形貌可控。（[3]徐伟;王涛;笪仕旭;徐琳绮.形态可控氧化锌纳米材料的绿色制备方法.发明专利申请号: CN201910359373.0)。而采用超声辅助法通常也会对材料的磁性及光学性能有影响，难以控制氧化锌纳米材料的光催化活性。
本发明采用简单的沉淀法，以乙二醇为表面活性剂制备球形纳米氧化锌，具有制备过程绿色简单、成本低的优点，所得产品粒径分布均匀，分散性良好，光催化降解亚甲基蓝活性高，优于锐钛矿相二氧化钛颗粒。
发明内容
本发明的目的在于提供一种制备工艺简单，形貌可控的氧化锌制备方法，无需使用高温高压设备，具有产率高和反应易处理的特点，成功地解决了产品中易有杂质，难清洁，形貌不规整的问题。
本发明一种球形纳米氧化锌的制备方法具体步骤为：
步骤1：在0.1 mol/L的可溶性锌盐溶液中，加入醇类表面活性剂，混合均匀，形成可溶性锌盐的混合溶液；所述的可溶性锌盐溶液与醇类表面活性剂的体积比为7∶8；
步骤2：将上述可溶性锌盐的混合溶液水浴加热至90°C，并滴入0.1 mol/L的沉淀剂溶液，搅拌加热反应3 h；
步骤3：步骤2的反应产物冷却至室温，其后进行离心分离、洗涤、干燥、研磨和煅烧，得到球形纳米氧化锌。
所述的可溶性锌盐的混合溶液与沉淀剂溶液的体积比为1∶1。
所述的可溶性锌盐为硫酸锌。
所述的沉淀剂为碳酸铵。
所述的醇类表面活性剂为乙二醇。
所述的洗涤的过程为：先用水洗至pH为7.0，其后再用甲醇洗涤2次。
所述的煅烧温度为500℃。
本发明的有益效果：本发明制备方法无需使用高温高压设备，工艺简便，氧化锌形貌规整可控，产率高，产物后处理容易，杂质少，分散度高，应用于有机染料的工业废水催化降解，降解率高，可见光照射1h 20min 后，对废水的降解率是锐钛矿相二氧化钛对废水降解率的2倍。
附图说明
图1为本发明纳米球形氧化锌的XRD谱图；
图2为本发明纳米球形氧化锌的SEM谱图；
图3为本发明纳米球形氧化锌的光催化降解亚甲基蓝活性曲线图；
图4为锐钛矿相TiO2的光催化降解亚甲基蓝活性曲线图。
具体实施方式
实施例1
室温下量取35 mL浓度为0.1 mol/L的ZnSO4溶液于烧杯中，再加入40 mL乙二醇，将混合溶液搅拌30 min，形成混合溶液A。将35 mL浓度为0.1 mol/L的(NH4)2CO3溶液缓慢滴加到混合溶液A中，90 ℃水浴加热持续搅拌3 h，冷却后将生成白色沉淀用蒸馏水洗涤5次，至pH为7.0，其后再用甲醇洗涤2次，再于80 ℃烘箱中烘干，然后研磨成粉末，再于马弗炉中500 ℃煅烧3 h，冷却至室温后研磨，所得样品即为纳米氧化锌，其形貌为球形颗粒，分布均匀，直径约为20 nm。制备的纳米球形氧化锌应用于降解染料废水：在300 W氙灯模拟可见光照射1小时20 min后，对5 mg/L亚甲基蓝的降解率为88.64%。
实施例2
室温下量取35 mL浓度为0.1mol/L的ZnSO4溶液于烧杯中，再加入40 mL乙二醇，将混合溶液搅拌30 min，形成溶液A。将35 mL浓度为0.1 mol/L的(NH4)2CO3溶液缓慢滴加到溶液A中，90 ℃水浴加热持续搅拌5 h，冷却后将生成白色沉淀用蒸馏水洗涤5次，再于80 ℃烘箱中烘干，然后研磨成粉末，再于马弗炉中500 ℃煅烧3 h，冷却至室温后研磨，所得样品即为ZnO-9。其形貌为球形颗粒组成的纳米棒，分散均匀，长约为100 nm，宽约20 nm，300 W氙灯模拟可见光照射1小时20 min后，对5 mg/L亚甲基蓝的降解率为68.64%。
实施例3
锐钛矿相二氧化钛降解亚甲基蓝的对比试验
室温下量取20.0mL无水乙醇于烧杯中，搅拌10min，然后缓慢滴加6mL钛酸四丁酯，搅拌混合均匀。继续滴加浓盐酸0.6mL，用pH试纸测得pH=3，搅拌至形成凝胶，再将凝胶置于80℃干燥箱中烘干，然后研磨成粉末，再于电阻炉中煅烧3h，所的样品即为锐钛矿相TiO2。300 W氙灯模拟可见光照射3小时后，亚甲基蓝的降解率为78.44%，在1h 30min内对5 mg/L亚甲基蓝的降解率为42.20%。对比可知，本发明所制备的球形纳米氧化锌的对废水的降解率1h 20min后是锐钛矿相TiO2的对废水的降解率的2倍。
Claims (8)
1.一种球形纳米氧化锌的制备方法，其特征在于：所述的制备方法具体步骤为：
步骤1：在0.1 mol/L的可溶性锌盐溶液中，加入醇类表面活性剂，混合均匀，形成可溶性锌盐的混合溶液；所述的可溶性锌盐溶液与醇类表面活性剂的体积比为7∶8；
步骤2：将上述可溶性锌盐的混合溶液水浴加热至90°C，并滴入0.1 mol/L的沉淀剂溶液，搅拌加热反应3 h；
步骤3：步骤2的反应产物冷却至室温，其后进行离心分离、洗涤、干燥、研磨和煅烧，得到球形纳米氧化锌。
2.根据权利要求1所述的一种球形纳米氧化锌的制备方法，其特征在于：所述的可溶性锌盐的混合溶液与沉淀剂溶液的体积比为1∶1。
3.根据权利要求1所述的一种球形纳米氧化锌的制备方法，其特征在于：所述的可溶性锌盐为硫酸锌。
4.根据权利要求1所述的一种球形纳米氧化锌的制备方法，其特征在于：所述的沉淀剂为碳酸铵。
5.根据权利要求1所述的一种球形纳米氧化锌的制备方法，其特征在于：所述的醇类表面活性剂为乙二醇。
6.根据权利要求1所述的一种球形纳米氧化锌的制备方法，其特征在于：所述的洗涤的过程为：先用水洗至pH为7.0，其后再用甲醇洗涤2次。
7.根据权利要求1所述的一种球形纳米氧化锌的制备方法，其特征在于：所述的干燥温度为80℃。
8.根据权利要求1所述的一种球形纳米氧化锌的制备方法，其特征在于：所述的煅烧温度为500℃。
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