CN106398316A - 一种掺杂金属镍离子的纳米氧化锌的制备方法 - Google Patents
一种掺杂金属镍离子的纳米氧化锌的制备方法 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title abstract description 10
- 239000011787 zinc oxide Substances 0.000 title abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001509 sodium citrate Substances 0.000 claims abstract description 10
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 10
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 229910001453 nickel ion Inorganic materials 0.000 claims description 37
- 229910052751 metal Inorganic materials 0.000 claims description 34
- 239000002184 metal Substances 0.000 claims description 34
- 150000002739 metals Chemical class 0.000 claims description 34
- 238000004458 analytical method Methods 0.000 claims description 16
- 238000013019 agitation Methods 0.000 claims description 13
- 229940078494 nickel acetate Drugs 0.000 claims description 9
- BEAZKUGSCHFXIQ-UHFFFAOYSA-L zinc;diacetate;dihydrate Chemical compound O.O.[Zn+2].CC([O-])=O.CC([O-])=O BEAZKUGSCHFXIQ-UHFFFAOYSA-L 0.000 claims description 9
- 239000013049 sediment Substances 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 abstract description 19
- 238000006731 degradation reaction Methods 0.000 abstract description 19
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 16
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 14
- 229940012189 methyl orange Drugs 0.000 abstract description 14
- 239000000047 product Substances 0.000 abstract description 13
- 239000001048 orange dye Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 3
- 230000002045 lasting effect Effects 0.000 abstract 2
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 abstract 2
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 abstract 2
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 abstract 2
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 1
- 230000005764 inhibitory process Effects 0.000 abstract 1
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 230000000844 anti-bacterial effect Effects 0.000 description 17
- 238000002835 absorbance Methods 0.000 description 15
- 239000000975 dye Substances 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 11
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 10
- 238000005070 sampling Methods 0.000 description 9
- 239000011701 zinc Substances 0.000 description 9
- 230000003385 bacteriostatic effect Effects 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000001963 growth medium Substances 0.000 description 5
- 239000002609 medium Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000011858 nanopowder Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000022 bacteriostatic agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
- 235000013904 zinc acetate Nutrition 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/04—Compounds of zinc
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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Abstract
一种掺杂金属镍离子的纳米氧化锌的制备方法是：取10.56g~9.68g二水乙酸锌和0.1592g~1.6979g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h。所制备一种掺杂金属镍离子的纳米氧化锌。在紫外灯照射50min时，对甲基橙染料达到最大降解率为91%，对金黄色葡萄球菌的抑菌圈最大为19.6mm。
Description
技术领域
本发明涉及降解剂和抑菌类生长技术领域，特别涉及一种掺杂金属镍离子的纳米氧化锌的制备方法。
背景技术
纳米氧化锌具有较高的比表面积，较好的生物相容性和较强的生物活性，在降解有机染料和抑菌金黄色葡萄球菌上表现出优异的性能；同时与有机抑菌剂相比，纳米氧化锌的耐热性和稳定性好、降解有机染料效率高，抑菌时效长。
纳米氧化锌在降解有机染料和抑菌金黄色葡萄球菌的研究和实践过程中，本发明的发明人发现：将金属镍离子掺杂进纳米氧化锌晶格中替代部分的锌离子，能够影响其晶体结构，提高纳米氧化锌的性能。本发明旨在获得一种具有高效光催化降解有机染料和抑菌活性的掺杂金属镍离子的纳米氧化锌的制备方法。
发明内容
本发明提供一种掺杂金属镍离子的纳米氧化锌的制备方法，所制备出的一种掺杂金属镍离子的纳米氧化锌具有降解有机染料和抑菌金黄色葡萄球菌的的制备方法。
采用的技术方案
本发明一种掺杂金属镍离子的纳米氧化锌的制备方法，包括如下步骤：
将10.56g~9.68g二水乙酸锌和0.1592g~1.6979g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h。
光催化降解有机染料的实验方法如下：
将制成的一种掺杂金属镍离子的纳米氧化锌50mg加入到100mL浓度为50mg/L的甲基橙溶液中，避光磁力搅拌15min，超声分散15min，测定其初始吸光度数值。然后将上述溶液放入到125W的紫外光灯源下，每隔10min取样一次，根据需要确定取样次数，取样后立即进行离心分离，取上层清液3mL，测定其吸光度数值。光催化甲基橙的降解率采用如下公式计算
，
公式中RE为降解率，A 0 和A t 分别为甲基橙溶液的初始吸光度和反应时间为t 时的吸光度。
抑菌实验方法如下：
预先培植金黄色葡萄球菌16h，将浓度为1.0×106cfu/mL的菌液25µL均匀涂布于固体培养基，将已灭菌的滤片置于培养皿中，取0.2mL浓度为0.5mg/mL的一种掺杂金属镍离子的纳米氧化锌溶液滴于滤片上，将培养基放置在培养箱中24h, 测量抑菌圈直径。
所制备的纳米粉的性能测试结果为：在紫外灯照射50min时，对甲基橙染料达到最大降解率为82%~91%，对金黄色葡萄球菌的抑菌圈直径为7.2mm~19.6mm。
二水乙酸锌、乙二醇、柠檬酸三钠、无水乙醇、丙酮、四水乙酸镍均为市购产品。
优点
1、氧化锌纳米粉和将制成的一种掺杂金属镍离子的纳米氧化锌在相同的实验条件下其结果如下：
纳米氧化锌，对有机染料甲基橙的降解率为20%~62%，对金黄色葡萄球菌的抑菌圈直径为5.2mm。
10.56g~9.68g二水乙酸锌和0.1592g~1.6979g四水乙酸镍制成的一种掺杂金属镍离子的纳米氧化锌，对有机染料甲基橙的降解率为82%~91%，对金黄色葡萄球菌的抑菌圈直径为7.2mm~19.6mm。
2．由于金属镍离子掺杂进纳米氧化锌晶格中，替代部分的锌离子，影响其晶体结构，导致纳米氧化锌的晶粒尺寸减小，微应力增大，晶格常数增大，从而使本发明产品降解有机染料甲基橙效率高，抑制金黄色葡萄球菌效果好。
3. 本发明产品属于无机抑菌剂，耐热性和稳定性高，与生物相容性好。
附图说明
图1为纳米Ni x Zn1-x O（x=0, 0.04, 0.08和0.12）的XRD谱图；
图2为纳米Ni x Zn1-x O（x=0, 0.04, 0.08和0.12）粒子的平均粒径分布图；
图3为纳米Ni x Zn1-x O（x=0, 0.04, 0.08和0.12）的抑菌圈直径分布图；
图4为纳米Ni x Zn1-x O粉体对甲基橙的降解率曲线a-x=0, b-x=0.04, c-x=0.08和d-x=0.12图。
具体实施方式
实施例
1
本发明一种掺杂金属镍离子的纳米氧化锌的制备方法，包括如下步骤：
取10.56g二水乙酸锌和0.1592g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h；
光催化降解有机染料的实验方法如下：
将制成的一种掺杂金属镍离子的纳米氧化锌50mg加入到100mL浓度为50mg/L的甲基橙溶液中，避光磁力搅拌15min，超声分散15min，测定其初始吸光度数值；然后将上述溶液放入到125W的紫外光灯源下，每隔10min取样一次，根据需要确定取样次数，取样后立即进行离心分离，取上层清液3mL，测定其吸光度数值；光催化甲基橙的降解率采用如下公式计算
，
公式中RE为降解率，A 0 和A t 分别为甲基橙溶液的初始吸光度和反应时间为t 时的吸光度；
抑菌实验方法如下：
预先培植金黄色葡萄球菌16h，将浓度为1.0×106cfu/mL的菌液25µL均匀涂布于固体培养基，将已灭菌的滤片置于培养皿中，取0.2mL浓度为0.5mg/mL的一种掺杂金属镍离子的纳米氧化锌溶液滴于滤片上，将培养基放置在培养箱中24h, 测量抑菌圈直径；
所制备的纳米粉的性能测试结果为：在紫外灯照射50min时，对甲基橙染料达到最大降解率为82%，对金黄色葡萄球菌的抑菌圈直径为7.2mm。
实施例
2
本发明一种掺杂金属镍离子的纳米氧化锌的制备方法，包括如下步骤：
取10.12g二水乙酸锌和1.084g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h；
光催化降解有机染料的实验方法如下：
将制成的一种掺杂金属镍离子的纳米氧化锌50mg加入到100mL浓度为50mg/L的甲基橙溶液中，避光磁力搅拌15min，超声分散15min，测定其初始吸光度数值；然后将上述溶液放入到125W的紫外光灯源下，每隔10min取样一次，根据需要确定取样次数，取样后立即进行离心分离，取上层清液3mL，测定其吸光度数值；光催化甲基橙的降解率采用如下公式计算
，
公式中RE为降解率，A 0 和A t 分别为甲基橙溶液的初始吸光度和反应时间为t 时的吸光度；
抑菌实验方法如下：
预先培植金黄色葡萄球菌16h，将浓度为1.0×106cfu/mL的菌液25µL均匀涂布于固体培养基，将已灭菌的滤片置于培养皿中，取0.2mL浓度为0.5mg/mL的一种掺杂金属镍离子的纳米氧化锌溶液滴于滤片上，将培养基放置在培养箱中24h, 测量抑菌圈直径；
所制备的纳米粉的性能测试结果为：在紫外灯照射50min时，对甲基橙染料达到最大降解率为88%，对金黄色葡萄球菌的抑菌圈直径为14.5mm。
实施例
3
本发明一种掺杂金属镍离子的纳米氧化锌的制备方法，包括如下步骤：
取9.68g二水乙酸锌和1.6797g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h；
光催化降解有机染料的实验方法如下：
将制成的一种掺杂金属镍离子的纳米氧化锌50mg加入到100mL浓度为50mg/L的甲基橙溶液中，避光磁力搅拌15min，超声分散15min，测定其初始吸光度数值；然后将上述溶液放入到125W的紫外光灯源下，每隔10min取样一次，根据需要确定取样次数，取样后立即进行离心分离，取上层清液3mL，测定其吸光度数值；光催化甲基橙的降解率采用如下公式计算
，
公式中RE为降解率，A 0 和A t 分别为甲基橙溶液的初始吸光度和反应时间为t 时的吸光度；
抑菌实验方法如下：
预先培植金黄色葡萄球菌16h，将浓度为1.0×106cfu/mL的菌液25µL均匀涂布于固体培养基，将已灭菌的滤片置于培养皿中，取0.2mL浓度为0.5mg/mL的一种掺杂金属镍离子的纳米氧化锌溶液滴于滤片上，将培养基放置在培养箱中24h, 测量抑菌圈直径；
所制备的纳米粉的性能测试结果为：在紫外灯照射50min时，对甲基橙染料达到最大降解率为91%，对金黄色葡萄球菌的抑菌圈直径为19.6mm。
工作原理
金属镍离子掺杂进纳米氧化锌晶格中替代部分的锌离子，能够影响其晶体结构，提高纳米氧化锌的性能。本发明旨在获得一种具有高效光催化降解有机染料和抑菌活性的掺杂金属镍离子的纳米氧化锌的制备方法。
光催化降解有机染料的实验方法如下：
将制成的一种掺杂金属镍离子的纳米氧化锌50mg加入到100mL浓度为50mg/L的甲基橙溶液中，避光磁力搅拌15min，超声分散15min，测定其初始吸光度数值。然后将上述溶液放入到125W的紫外光灯源下，每隔10min取样一次，取样后立即进行离心分离，取上层清液3mL，测定其吸光度数值。光催化甲基橙的降解率采用如下公式计算
，
公式中RE为降解率，A 0 和A t 分别为甲基橙溶液的初始吸光度和反应时间为t 时的吸光度。
抑菌实验方法如下：
预先培植金黄色葡萄球菌16h，将浓度为1.0×106cfu/mL的菌液25µL均匀涂布于固体培养基，将已灭菌的滤片置于培养皿中，取0.2mL浓度为0.5mg/mL的一种掺杂金属镍离子的纳米氧化锌溶液滴于滤片上，将培养基放置在培养箱中24h, 测量抑菌圈直径。
Claims (4)
1.一种掺杂金属镍离子的纳米氧化锌的制备方法，其特征在于：
取10.56g~9.68g二水乙酸锌和0.1592g~1.6979g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h。
2.根据权利要求1所述的一种掺杂金属镍离子的纳米氧化锌的制备方法，其特征在于：
取10.56g二水乙酸锌和0.1592g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h。
3.根据权利要求1所述的一种掺杂金属镍离子的纳米氧化锌的制备方法，其特征在于：
取10.12g二水乙酸锌和1.084g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h。
4.根据权利要求1所述的一种掺杂金属镍离子的纳米氧化锌的制备方法，其特征在于：
取9.68g二水乙酸锌和1.6797g四水乙酸镍，放入250mL的三口瓶中，加入70mL的分析乙二醇作为溶剂，1.2g 浓度为0.058mol/L的柠檬酸三钠作为分散剂，上述溶液在180℃下反应4h，整个反应过程始终在磁力搅拌，氮气保护下进行，得到的沉淀物用无水乙醇洗涤三次，每次5min，用分析丙酮洗涤一次，每次5min，再用去离子水洗涤三次，每次5min，确保产物为纯的一种掺杂金属镍离子的纳米氧化锌，产物在80℃的真空干燥箱中烘干8h。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140698A (zh) * | 2017-05-26 | 2017-09-08 | 扬州工业职业技术学院 | 一种用于检测氢气的镍掺杂氧化锌材料的制备方法 |
| CN106966444B (zh) * | 2017-05-26 | 2018-04-06 | 扬州工业职业技术学院 | 一种镍掺杂的氧化锌材料及其在制备气敏传感器中的应用 |
| CN108301066A (zh) * | 2018-02-10 | 2018-07-20 | 深圳源广安智能科技有限公司 | 一种抗菌聚酯纤维 |
| CN108324031A (zh) * | 2018-02-10 | 2018-07-27 | 深圳市晟达机械设计有限公司 | 一种酒店抗菌防螨阻尼枕 |
| CN108437589A (zh) * | 2018-02-10 | 2018-08-24 | 梧州井儿铺贸易有限公司 | 一种窗帘用抗菌性能良好的面料 |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390892A (zh) * | 2002-06-28 | 2003-01-15 | 杨学良 | 一种纳米级抗菌除味复合粉体的制造方法 |
| CN101563294A (zh) * | 2006-10-11 | 2009-10-21 | 巴斯夫欧洲公司 | 生产表面改性的纳米颗粒状金属氧化物、金属氢氧化物和/或金属羟基氧化物的方法 |
| CN103285866A (zh) * | 2013-05-16 | 2013-09-11 | 马玉山 | 一种液相糠醛加氢制糠醇催化剂及其制备方法和用法 |
| CN103651569A (zh) * | 2013-11-26 | 2014-03-26 | 南通职业大学 | 一种制备表面包覆改性Ag/ZnO纳米复合抗菌剂的工艺 |
| CN103657662A (zh) * | 2013-11-27 | 2014-03-26 | 浙江师范大学 | 镍掺杂氧化锌分级结构光催化纳米材料及其制备方法 |
| CN103974906A (zh) * | 2011-11-17 | 2014-08-06 | 堺化学工业株式会社 | 表面处理氧化锌粉体、抗菌剂和抗菌性组合物 |
| CN103977806A (zh) * | 2014-05-16 | 2014-08-13 | 盐城工学院 | 一种光催化降解材料Co掺杂纳米ZnO及其制备方法 |
| CN104275173A (zh) * | 2014-07-30 | 2015-01-14 | 浙江师范大学 | 碳包覆金属掺杂氧化锌复合光催化纳米材料及其制备方法 |
| CN104445363A (zh) * | 2013-09-14 | 2015-03-25 | 金秀华 | 一种纳米氧化锌的制备方法 |
-
2016
- 2016-06-01 CN CN201610379448.8A patent/CN106398316B/zh not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390892A (zh) * | 2002-06-28 | 2003-01-15 | 杨学良 | 一种纳米级抗菌除味复合粉体的制造方法 |
| CN101563294A (zh) * | 2006-10-11 | 2009-10-21 | 巴斯夫欧洲公司 | 生产表面改性的纳米颗粒状金属氧化物、金属氢氧化物和/或金属羟基氧化物的方法 |
| CN103974906A (zh) * | 2011-11-17 | 2014-08-06 | 堺化学工业株式会社 | 表面处理氧化锌粉体、抗菌剂和抗菌性组合物 |
| CN103285866A (zh) * | 2013-05-16 | 2013-09-11 | 马玉山 | 一种液相糠醛加氢制糠醇催化剂及其制备方法和用法 |
| CN104445363A (zh) * | 2013-09-14 | 2015-03-25 | 金秀华 | 一种纳米氧化锌的制备方法 |
| CN103651569A (zh) * | 2013-11-26 | 2014-03-26 | 南通职业大学 | 一种制备表面包覆改性Ag/ZnO纳米复合抗菌剂的工艺 |
| CN103657662A (zh) * | 2013-11-27 | 2014-03-26 | 浙江师范大学 | 镍掺杂氧化锌分级结构光催化纳米材料及其制备方法 |
| CN103977806A (zh) * | 2014-05-16 | 2014-08-13 | 盐城工学院 | 一种光催化降解材料Co掺杂纳米ZnO及其制备方法 |
| CN104275173A (zh) * | 2014-07-30 | 2015-01-14 | 浙江师范大学 | 碳包覆金属掺杂氧化锌复合光催化纳米材料及其制备方法 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140698A (zh) * | 2017-05-26 | 2017-09-08 | 扬州工业职业技术学院 | 一种用于检测氢气的镍掺杂氧化锌材料的制备方法 |
| CN106966444B (zh) * | 2017-05-26 | 2018-04-06 | 扬州工业职业技术学院 | 一种镍掺杂的氧化锌材料及其在制备气敏传感器中的应用 |
| CN108301066A (zh) * | 2018-02-10 | 2018-07-20 | 深圳源广安智能科技有限公司 | 一种抗菌聚酯纤维 |
| CN108324031A (zh) * | 2018-02-10 | 2018-07-27 | 深圳市晟达机械设计有限公司 | 一种酒店抗菌防螨阻尼枕 |
| CN108437589A (zh) * | 2018-02-10 | 2018-08-24 | 梧州井儿铺贸易有限公司 | 一种窗帘用抗菌性能良好的面料 |
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