CN103771493B - A kind of method preparing one-D nano zinc oxide - Google Patents
A kind of method preparing one-D nano zinc oxide Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 63
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011259 mixed solution Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 239000007864 aqueous solution Substances 0.000 claims abstract description 23
- 150000003751 zinc Chemical class 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZDFBXXSHBTVQMB-UHFFFAOYSA-N 2-ethylhexoxy(2-ethylhexyl)phosphinic acid Chemical compound CCCCC(CC)COP(O)(=O)CC(CC)CCCC ZDFBXXSHBTVQMB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 4
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 3
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 15
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 13
- 239000002086 nanomaterial Substances 0.000 description 8
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- 238000003917 TEM image Methods 0.000 description 4
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- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004530 micro-emulsion Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000005616 pyroelectricity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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Abstract
本发明涉及纳米氧化锌，特指一种纳米氧化锌的液相制备方法，具体步骤为：配制0.5M锌盐水溶液，4M的氢氧化钠水溶液；配制PN混合溶液，萃取剂PC-88A和N1923的摩尔比为1-3：1；配制PN和庚烷的混合溶液，PN的质量分数为16%；将PN-庚烷溶液与0.5M的锌盐溶液混合，PN-庚烷溶液与锌盐溶液的体积比为：4:1-4:3，室温下搅拌充分混合；量取4M的NaOH水溶液，缓慢滴加到混合溶液中，锌盐溶液与NaOH溶液的体积比为2:1，室温搅拌；待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤，置于烘箱中干燥，获得白色的ZnO粉体。本发明合成方法简单，条件温和，反应在室温下就可以进行，无需煅烧。
The present invention relates to nano-zinc oxide, in particular to a liquid-phase preparation method of nano-zinc oxide. The specific steps are: preparing 0.5M zinc salt aqueous solution and 4M sodium hydroxide aqueous solution; preparing PN mixed solution, extractant PC-88A and N1923 The molar ratio of PN and heptane is 1-3:1; prepare a mixed solution of PN and heptane, the mass fraction of PN is 16%; mix PN-heptane solution with 0.5M zinc salt solution, PN-heptane solution and zinc salt The volume ratio of the solution is: 4:1-4:3, stir and mix well at room temperature; measure 4M NaOH aqueous solution, and slowly add it to the mixed solution, the volume ratio of zinc salt solution to NaOH solution is 2:1, at room temperature Stir; after the reaction is completed, centrifuge, filter, wash with ethanol and distilled water, and dry in an oven to obtain white ZnO powder. The synthesis method of the invention is simple, the condition is mild, and the reaction can be carried out at room temperature without calcining.
Description
技术领域 technical field
本发明涉及纳米氧化锌，具体地说，涉及的是一种纳米氧化锌的液相制备方法。 The invention relates to nano zinc oxide, in particular to a liquid-phase preparation method of nano zinc oxide.
背景技术 Background technique
一维纳米ZnO结构因其特殊的量子尺寸效应、界面效应和量子限制效应，在磁、光、力等方面具备了薄膜材料所不具备的许多优异性能，各种一维纳米ZnO结构的制备和性能研究已成为当今材料领域研究的热点；与其它半导体纳米材料相比，氧化锌的一维纳米结构易于合成，且提供的表面形态较多，更由于它较大的直接宽带隙(3.37eV)和优良的压电性、热电性，其更适宜应用于室温紫外发光、激光材料和光电子器件，对新型传感器、存储器件和场效应晶体管等的开发具有潜在的研究价值，目前国内外均投入了相当大的力量进行一维ZnO纳米结构的研制工作。 Due to its special quantum size effect, interface effect and quantum confinement effect, the one-dimensional nano-ZnO structure has many excellent properties that thin film materials do not have in terms of magnetism, light, and force. The preparation and application of various one-dimensional nano-ZnO structures Performance research has become a hot spot in the field of materials research; compared with other semiconductor nanomaterials, the one-dimensional nanostructure of zinc oxide is easy to synthesize, and provides more surface morphology, and because of its large direct wide band gap (3.37eV) With excellent piezoelectricity and pyroelectricity, it is more suitable for room temperature ultraviolet luminescence, laser materials and optoelectronic devices, and has potential research value for the development of new sensors, storage devices and field effect transistors. At present, both at home and abroad have invested Considerable efforts have been made to develop one-dimensional ZnO nanostructures.
一维ZnO纳米结构主要包括纳米带、纳米线、纳米棒和纳米管等，目前制备ZnO纳米结构的方法众多，包括气相法与液相法，如热蒸发法、物理气相沉积法（PVD）、金属有机化学气相沉积法（MOCVD)、模板法和水热法等；气相法虽然制得的产品品质高，但设备昂贵，制作成本高，而且实验条件要求苛刻，与气相法相比，液相法具有工艺简单、操作简便、对设备要求低、容易批量生产等优点，而且合成出的纳米微粒表面活性好、产物组成精确可控，更具有工业化前景。 One-dimensional ZnO nanostructures mainly include nanobelts, nanowires, nanorods, and nanotubes. There are many methods for preparing ZnO nanostructures, including gas phase and liquid phase methods, such as thermal evaporation, physical vapor deposition (PVD), Metal-organic chemical vapor deposition (MOCVD), template method and hydrothermal method, etc.; although the product quality of the gas phase method is high, the equipment is expensive, the production cost is high, and the experimental conditions are harsh. Compared with the gas phase method, the liquid phase method It has the advantages of simple process, easy operation, low equipment requirements, and easy mass production, and the synthesized nanoparticles have good surface activity, precise and controllable product composition, and have more industrialization prospects.
反胶团萃取法主要是利用微乳液体系通过萃取剂与被萃物之间的静电作用进行萃取，使化学反应在油相包裹的“水池”中进行，以获得分散性好，形貌规则的纳米材料；本发明以2-乙基己基膦酸-单-2-乙基己基酯(PC-88A)和伯胺N1923为萃取剂，庚烷为有机溶剂，采用反胶团微乳液萃取体系制备ZnO一维纳米材料；基于萃取剂的界面性质和萃取体系的界面现象，萃取有机相中存在多种纳米级分子聚集体，可以利用萃取体系的特殊聚集现象来制备不同表面性能的纳米材料以满足实际应用需要，杨传芳等(YangC.Eetal.J.Mater.Sci.Technol.,11,217(1995))在详细研究TBP-煤油/HCl-ZrOCl2和TBP-煤油/HNO3-ZrO(NO3)2体系基础上成功制备了超细ZrO2粒子，从萃取体系中直接制备纳米粒子它不但提高了金属的负载量，同时萃取过程本身对金属离子进行了纯化，而且萃取剂和有机溶剂在试验过程中不易流失，易于回收，可重复利用，为从实验室研究转化到工业成果提供了一条很好的“分离—制备一应用”一体化的思路。 The reverse micellar extraction method is mainly to use the microemulsion system to extract through the electrostatic interaction between the extractant and the extract, so that the chemical reaction is carried out in the "water pool" wrapped in the oil phase, so as to obtain good dispersion and regular shape. Nanomaterials; the present invention uses 2-ethylhexylphosphonic acid-mono-2-ethylhexyl ester (PC-88A) and primary amine N1923 as extraction agent, heptane as organic solvent, and adopts reverse micellar microemulsion extraction system to prepare ZnO one-dimensional nanomaterials; based on the interface properties of the extractant and the interface phenomena of the extraction system, there are a variety of nano-scale molecular aggregates in the extracted organic phase, and the special aggregation phenomenon of the extraction system can be used to prepare nanomaterials with different surface properties to meet the requirements. Practical application needs, Yang Chuanfang et al. (YangC.Eetal.J.Mater.Sci.Technol., 11,217 (1995)) in detailed research TBP-kerosene/HCl-ZrOCl 2 and TBP-kerosene/HNO 3 -ZrO(NO 3 ) 2 Ultrafine ZrO 2 particles were successfully prepared on the basis of the system, and nanoparticles were directly prepared from the extraction system. It not only increased the loading capacity of metals, but also purified the metal ions during the extraction process itself, and the extraction agent and organic solvent were in the test process. It is not easy to be lost, easy to recycle, and can be reused. It provides a good integration of "separation-preparation-application" for the transformation from laboratory research to industrial results.
发明内容 Contents of the invention
本发明的目的之一是提供单分散一维纳米氧化锌颗粒，得到的一维纳米氧化锌颗粒分散性好，长径比较大。 One of the objectives of the present invention is to provide monodisperse one-dimensional nano-zinc oxide particles, and the obtained one-dimensional nano-zinc oxide particles have good dispersibility and large long-diameter ratio.
本发明的另一目的是针对现有技术中存在的缺陷与不足，提出一种一维纳米氧化锌的制备方法，无需煅烧，用萃取法直接制备单分散的一维纳米氧化锌，本发明是通过以下技术方案实现的，本发明包括以下步骤： Another object of the present invention is to propose a method for preparing one-dimensional nano-zinc oxide aimed at the defects and deficiencies in the prior art, without calcination, and directly prepare monodisperse one-dimensional nano-zinc oxide by extraction method. The present invention is Realized by the following technical solutions, the present invention comprises the following steps:
第一步，配制浓度为0.5M锌盐水溶液，浓度为4M的氢氧化钠水溶液。 The first step is to prepare a 0.5M zinc salt solution and a 4M sodium hydroxide solution.
所述锌盐，选用六水合硝酸锌。 The zinc salt is selected from zinc nitrate hexahydrate.
第二步，配制PN混合溶液。 The second step is to prepare PN mixed solution.
所述PN混合溶液中，萃取剂PC-88A和N1923的摩尔比为1-3：1。 In the PN mixed solution, the molar ratio of extractant PC-88A and N1923 is 1-3:1.
第三步，配制PN和庚烷的混合溶液，PN的质量分数为16%。 The third step is to prepare a mixed solution of PN and heptane, and the mass fraction of PN is 16%.
第四步，将PN-庚烷溶液与0.5M的锌盐溶液混合，PN-庚烷溶液与锌盐溶液的体积比为：4:1-4:3，于室温下搅拌使之充分混合。 The fourth step is to mix PN-heptane solution with 0.5M zinc salt solution, the volume ratio of PN-heptane solution and zinc salt solution is: 4:1-4:3, stir at room temperature to make it fully mixed.
第五步，量取4M的NaOH水溶液，缓慢滴加到混合溶液中，锌盐溶液与NaOH溶液的体积比为2:1,同时搅拌速度调至600~800转/分钟，室温持续搅拌2小时。 The fifth step is to measure 4M NaOH aqueous solution and slowly add it dropwise to the mixed solution. The volume ratio of zinc salt solution to NaOH solution is 2:1. At the same time, adjust the stirring speed to 600~800 rpm, and continue stirring at room temperature for 2 hours. .
第六步，待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤，置于烘箱中干燥，获得白色的ZnO粉体。 In the sixth step, after the reaction is completed, centrifuge, filter, wash with ethanol and distilled water, and dry in an oven to obtain white ZnO powder.
第七步，将离心分离后获得的上层清液PN和庚烷的混合溶液纯化处理，回收再利用。 In the seventh step, the mixed solution of supernatant PN and heptane obtained after centrifugation is purified and recycled for reuse.
常规的微乳液体系中，采用的表面活性剂和有机物难以回收再利用，而且要得到单分散的一维纳米ZnO粉体需要高温高压的实验条件，本发明的有益效果在于： In conventional microemulsion systems, the surfactants and organics used are difficult to recycle and reuse, and the experimental conditions of high temperature and high pressure are required to obtain monodisperse one-dimensional nano ZnO powder. The beneficial effects of the present invention are:
(1)PC-88A和N1923这两种萃取剂廉价易得，而且性质稳定，可通过离心分离后回收再利用，大大节约了成本； (1) The two extractants PC-88A and N1923 are cheap and easy to obtain, and have stable properties, which can be recycled and reused after centrifugation, which greatly saves the cost;
(2)合成方法简单，条件温和，反应在室温下就可以进行，无需煅烧，不需要大型精密设备，可适用于大规模生产。 (2) The synthesis method is simple, the conditions are mild, and the reaction can be carried out at room temperature without calcination and large-scale precision equipment, and is applicable to large-scale production.
附图说明 Description of drawings
图1为本发明所得一维纳米氧化锌的XRD图： Fig. 1 is the XRD pattern of the one-dimensional nano zinc oxide of gained of the present invention:
从XRD图中可以看出，制备获得的ZnO为六方晶系纤锌矿结构，所有的衍射峰均与ZnO的标准图谱（PDF#65-3411）相吻合，图中未出现Zn(NO3)2，Zn(OH)2等其他的杂质峰，说明所得产品的纯度很高，窄而尖锐的衍射峰形表明产品的晶化质量很好。 It can be seen from the XRD pattern that the prepared ZnO has a hexagonal wurtzite structure, and all the diffraction peaks are consistent with the standard spectrum of ZnO (PDF#65-3411), and Zn(NO 3 ) does not appear in the figure 2 , Zn(OH) 2 and other impurity peaks, indicating that the product obtained is of high purity, and the narrow and sharp diffraction peak shape indicates that the crystallization quality of the product is very good.
图2为实施例1所得的针状纳米氧化锌的TEM图，分散性较好，长径比为13~15。 Fig. 2 is the TEM image of the needle-shaped nano-zinc oxide obtained in Example 1, which has good dispersion and an aspect ratio of 13 to 15.
图3为实施例2所得的棒状纳米氧化锌的TEM图，形貌呈花瓣状，长径比为2~3。 Fig. 3 is the TEM image of the rod-shaped nano-zinc oxide obtained in Example 2, the morphology is petal-shaped, and the aspect ratio is 2-3.
图4为实施例3所得的棒状纳米氧化锌的TEM图，分散性很好，形状规则，长径比可达15~20。 Figure 4 is a TEM image of the rod-shaped nano-zinc oxide obtained in Example 3, which has good dispersion, regular shape, and an aspect ratio of 15-20.
图5为实施例4所得的棒状纳米氧化锌的TEM图，形貌呈短棒状，长径比为3~4。 Figure 5 is a TEM image of the rod-shaped nano-zinc oxide obtained in Example 4, which has a short rod shape and an aspect ratio of 3-4.
具体实施方式 detailed description
实施例1 Example 1
配制浓度为0.5M六水合硝酸锌水溶液，浓度为4M的NaOH水溶液，萃取剂PC-88A和N1923的摩尔比为1:1，配制PN和庚烷的混合溶液，PN的质量分数为16%，将40mLPN和庚烷的有机混合溶液与10mL锌盐水溶液混合，置于250mL圆底烧瓶中，室温搅拌0.5h；量取5mLNaOH溶液，缓慢滴加入混合溶液中，同时搅拌速度调至600转/分钟，室温持续搅拌2h；待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤数遍，置于烘箱中60℃干燥6h得到氧化锌粉体，透射电子显微镜结果见图2。 The preparation concentration is 0.5M zinc nitrate hexahydrate aqueous solution, the concentration is 4M NaOH aqueous solution, the molar ratio of extraction agent PC-88A and N1923 is 1:1, the mixed solution of preparation PN and heptane, the mass fraction of PN is 16%, Mix 40mL of the organic mixed solution of PN and heptane with 10mL of zinc salt aqueous solution, put it in a 250mL round bottom flask, and stir at room temperature for 0.5h; measure 5mL of NaOH solution, slowly add it dropwise to the mixed solution, and at the same time adjust the stirring speed to 600 rpm , kept stirring at room temperature for 2 hours; after the reaction was completed, centrifuged, filtered, washed several times with ethanol and distilled water, and dried in an oven at 60°C for 6 hours to obtain zinc oxide powder. The transmission electron microscope results are shown in Figure 2.
实施例2 Example 2
配制浓度为0.5M六水合硝酸锌水溶液，浓度为4M的NaOH水溶液，萃取剂PC-88A和N1923的摩尔比为1:1，配制PN和庚烷的混合溶液，PN的质量分数为16%，将40mLPN和庚烷的有机混合溶液与20mL锌盐水溶液混合，置于250mL圆底烧瓶中，室温搅拌0.5h；量取10mLNaOH溶液，缓慢滴加入混合溶液中，同时搅拌速度调至800转/分钟，室温持续搅拌2h；待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤数遍，置于烘箱中60℃干燥6h得到氧化锌粉体，透射电子显微镜结果见图3。 The preparation concentration is 0.5M zinc nitrate hexahydrate aqueous solution, the concentration is 4M NaOH aqueous solution, the molar ratio of extraction agent PC-88A and N1923 is 1:1, the mixed solution of preparation PN and heptane, the mass fraction of PN is 16%, Mix 40mL of PN and heptane organic mixed solution with 20mL of zinc salt aqueous solution, place in a 250mL round bottom flask, stir at room temperature for 0.5h; measure 10mL of NaOH solution, slowly drop into the mixed solution, and at the same time adjust the stirring speed to 800 rpm , kept stirring at room temperature for 2 hours; after the reaction was completed, centrifuged, filtered, washed several times with ethanol and distilled water, and dried in an oven at 60°C for 6 hours to obtain zinc oxide powder. The transmission electron microscope results are shown in Figure 3.
实施例3 Example 3
配制浓度为0.5M六水合硝酸锌水溶液，浓度为4M的NaOH水溶液，萃取剂PC-88A和N1923的摩尔比为1:1，配制PN和庚烷的混合溶液，PN的质量分数为16%，将40mLPN和庚烷的有机混合溶液与30mL锌盐水溶液混合，置于250mL圆底烧瓶中，室温搅拌0.5h；量取15mLNaOH溶液，缓慢滴加入混合溶液中，同时搅拌速度调至700转/分钟，室温持续搅拌2h；待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤数遍，置于烘箱中60℃干燥6h得到氧化锌粉体，透射电子显微镜结果见图4。 The preparation concentration is 0.5M zinc nitrate hexahydrate aqueous solution, the concentration is 4M NaOH aqueous solution, the molar ratio of extraction agent PC-88A and N1923 is 1:1, the mixed solution of preparation PN and heptane, the mass fraction of PN is 16%, Mix 40mL of PN and heptane organic mixed solution with 30mL of zinc salt aqueous solution, place in a 250mL round bottom flask, stir at room temperature for 0.5h; measure 15mL of NaOH solution, slowly drop into the mixed solution, and at the same time adjust the stirring speed to 700 rpm , kept stirring at room temperature for 2 hours; after the reaction was completed, centrifuged, filtered, washed several times with ethanol and distilled water, and dried in an oven at 60°C for 6 hours to obtain zinc oxide powder. The transmission electron microscope results are shown in Figure 4.
实施例4 Example 4
配制浓度为0.5M六水合硝酸锌水溶液，浓度为4M的NaOH水溶液，萃取剂PC-88A和N1923的摩尔比为3:1，配制PN和庚烷的混合溶液，PN的质量分数为16%，将40mLPN和庚烷的有机混合溶液与20mL锌盐水溶液混合，置于250mL圆底烧瓶中，室温搅拌0.5h；量取10mLNaOH溶液，缓慢滴加入混合溶液中，同时搅拌速度调至800转/分钟，室温持续搅拌2h；待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤数遍，置于烘箱中60℃干燥6h得到氧化锌粉体，透射电子显微镜结果见图5。 The preparation concentration is 0.5M zinc nitrate hexahydrate aqueous solution, the concentration is 4M NaOH aqueous solution, the molar ratio of extraction agent PC-88A and N1923 is 3:1, the mixed solution of preparation PN and heptane, the mass fraction of PN is 16%, Mix 40mL of PN and heptane organic mixed solution with 20mL of zinc salt aqueous solution, place in a 250mL round bottom flask, stir at room temperature for 0.5h; measure 10mL of NaOH solution, slowly drop into the mixed solution, and at the same time adjust the stirring speed to 800 rpm , kept stirring at room temperature for 2 hours; after the reaction was completed, centrifuged, filtered, washed several times with ethanol and distilled water, and dried in an oven at 60°C for 6 hours to obtain zinc oxide powder. The transmission electron microscope results are shown in Figure 5.
实施例5 Example 5
配制浓度为0.5M六水合硝酸锌水溶液，浓度为4M的NaOH水溶液，萃取剂PC-88A和N1923的摩尔比为2:1，配制PN和庚烷的混合溶液，PN的质量分数为16%，将40mLPN和庚烷的有机混合溶液与20mL锌盐水溶液混合，置于250mL圆底烧瓶中，室温搅拌0.5h；量取10mLNaOH溶液，缓慢滴加入混合溶液中，同时搅拌速度调至800转/分钟，室温持续搅拌2h；待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤数遍，置于烘箱中60℃干燥6h得到氧化锌粉体，为棒状纳米氧化锌，长径比为5~8。 The preparation concentration is 0.5M zinc nitrate hexahydrate aqueous solution, the concentration is 4M NaOH aqueous solution, the molar ratio of extractant PC-88A and N1923 is 2:1, the mixed solution of preparation PN and heptane, the mass fraction of PN is 16%, Mix 40mL of PN and heptane organic mixed solution with 20mL of zinc salt aqueous solution, place in a 250mL round bottom flask, stir at room temperature for 0.5h; measure 10mL of NaOH solution, slowly drop into the mixed solution, and at the same time adjust the stirring speed to 800 rpm , keep stirring at room temperature for 2 hours; after the reaction is completed, centrifuge, filter, wash several times with ethanol and distilled water, and dry in an oven at 60°C for 6 hours to obtain zinc oxide powder, which is rod-shaped nano-zinc oxide with an aspect ratio of 5~ 8.
实施例6 Example 6
配制浓度为0.5M六水合硝酸锌水溶液，浓度为4M的NaOH水溶液，萃取剂PC-88A和N1923的摩尔比为2:1，配制PN和庚烷的混合溶液，PN的质量分数为16%，将40mLPN和庚烷的有机混合溶液与10mL锌盐水溶液混合，置于250mL圆底烧瓶中，室温搅拌0.5h；量取5mLNaOH溶液，缓慢滴加入混合溶液中，同时搅拌速度调至600转/分钟，室温持续搅拌2h；待反应完毕后，离心分离，过滤，用乙醇、蒸馏水洗涤数遍，置于烘箱中60℃干燥6h得到氧化锌粉体，为棒状纳米氧化锌，长径比为9~12。 The preparation concentration is 0.5M zinc nitrate hexahydrate aqueous solution, the concentration is 4M NaOH aqueous solution, the molar ratio of extractant PC-88A and N1923 is 2:1, the mixed solution of preparation PN and heptane, the mass fraction of PN is 16%, Mix 40mL of the organic mixed solution of PN and heptane with 10mL of zinc salt aqueous solution, put it in a 250mL round bottom flask, and stir at room temperature for 0.5h; measure 5mL of NaOH solution, slowly add it dropwise to the mixed solution, and at the same time adjust the stirring speed to 600 rpm , keep stirring at room temperature for 2 hours; after the reaction is completed, centrifuge, filter, wash several times with ethanol and distilled water, and dry in an oven at 60°C for 6 hours to obtain zinc oxide powder, which is rod-shaped nano-zinc oxide with an aspect ratio of 9~ 12.
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