CN107311233A - 一种制备MnYbO3粉体的方法 - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
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- VQWQYXBWRCCZGX-UHFFFAOYSA-N acetic acid;manganese Chemical compound [Mn].CC(O)=O.CC(O)=O VQWQYXBWRCCZGX-UHFFFAOYSA-N 0.000 claims description 5
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- 229940012189 methyl orange Drugs 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
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- 238000002474 experimental method Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 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 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
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- 229910052748 manganese Inorganic materials 0.000 description 1
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- 239000012528 membrane Substances 0.000 description 1
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- 238000013032 photocatalytic reaction Methods 0.000 description 1
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- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
一种制备MnYbO3粉体的方法，它涉及一种ABO3型钙钛矿复合氧化物MnYbO3材料的制备方法。本发明采用微波协助法，以硝酸镱、乙酸锰、柠檬酸和尿素为原料，制备了平均粒径约为0.5μm至1.0μm，并且具有良好紫外光催化活性的MnYbO3粉体。其步骤分为反应溶液的配制和粉体产品的制备两步。本发明为MnYbO3粉体产品的制备开发了新工业，达到了快速高效、可工业化生产MnYbO3粉体的目的。
Description
技术领域
本发明涉及ABO3型钙钛矿复合氧化物材料的制备，特别是涉及一种制备MnYbO3粉体的方法。
背景技术
MnYbO3(镱酸锰)属于一种ABO3型钙钛矿复合氧化物。正如文献(硅酸盐通报，2014，33(12)：3239-3244)报道：钙钛矿型复合氧化物是一类具有独特物理性质和化学性能的新型无机复合材料，由于这类化合物在催化和电化学等领域表现出优异的性能而受到外界广泛的关注。文献(发明专利申请号201310521706.8)指出：铋基钙钛矿结构氧化物BiYbO3具有很高的居里温度和很好的压电性能，成为研究和开发新型具有更高居里温度的陶瓷和薄膜材料的一个突破点，基于此类材料的研究受到国内外研究者的广泛关注。而关于ABO3型钙钛矿复合氧化物MnYbO3的研究报道非常的少，文献(Materials Research Bulletin，1967，2：819-822)报道采用相应的盐为原料，在700℃下高温煅烧反应制备得到了MnYbO3。
发明内容
本发明的目的在于克服现有技术的不足，提供一种微波协助法制备MnYbO3粉体的方法。
本发明的目的是通过以下技术方案来实现的，具体步骤为：
(1)反应溶液的配制
在室温条件下，分别将0.005mol乙酸锰和0.005mol硝酸镱分别溶于50mL的蒸馏水中备用。在搅拌条件下，向加热至50℃的50mL的乙酸锰溶液中加入0.012mol至0.015mol的柠檬酸，待柠檬酸溶解后加入备用的50mL硝酸镱溶液，然后再加入0.05mol至0.06mol的尿素得到混合溶液，将混合溶液继续搅拌反应15min得到反应溶液。
(2)粉体产品的制备
将100mL反应液放入微波炉中，在保持微波功率1250W～1500W条件下反应18min至完全燃烧得到初产物，冷却至室温取出初产物，将初产物放入马弗炉中于600℃～650℃温度范围煅烧1h，冷却至室温取出研磨细得到MnYbO3粉体产品。
本发明的积极效果是：采用微波法快捷的制备出初产物，再经600℃～650℃温度煅烧1h即可得到MnYbO3粉体产品，为MnYbO3粉体产品的制备开发了新工业，达到了快速高效、可工业化生产MnYbO3粉体的目的。
附图说明
图1：实施例1所得MnYbO3产品的XRD图；
图2：实施例1所得MnYbO3产品的扫描电镜照片；
图3：实施例1所得MnYbO3产品对甲基橙溶液的紫外光催化降解曲线。
具体实施方式
实施例1
在室温条件下，分别将0.005mol的乙酸锰和0.005mol的硝酸镱分别溶于50mL的蒸馏水中备用。向加热至50℃的50ml乙酸锰溶液中加入0.012mol的柠檬酸，待柠檬酸溶解后加入备用的50mL硝酸镱溶液，然后再加入0.05mol的尿素得到混合溶液，将混合溶液继续搅拌反应15min得到反应溶液。将100mL反应液放入微波炉中，在保持微波功率1250W条件下反应18min至完全燃烧得到初产物，冷却至室温取出初产物，将初产物放入马弗炉中于650℃煅烧1h，冷却至室温取出研磨细得到MnYbO3粉体产品。对得到的产品分别进行X射线衍射(XRD)分析和扫描电镜(SEM)观测，结果分别如图1和图2所示。
图1是采用XD-6型X射线衍射分析仪，粉末法分析测定得到的产品的XRD图。从图1可知，所得产品的XRD图谱与标准的MnYbO3(PDF#38-1246)完全吻合，这表明制备得到的产品是MnYbO3。
图2是采用日立S-3400N扫描电子显微镜测试得到的产品的扫描电镜照片。从图2可知，MnYbO3产品以平均粒径0.5μm至1.0μm左右的颗粒存在为主，颗粒虽略有团聚，但总体上均匀性好。
为了表征MnYbO3粉体的光催化活性，光催化实验在自制的光催化反应装置中进行：光源为150W紫外线高压汞灯，将20mg的MnYbO3粉体加入到20mg/L的模拟污水甲基橙溶液中避光10min后，进行光催化降解实验；降解所需时间后取出离心分离去除粉体，通过紫外可见分光光度计(λ＝464nm)对离心后的澄清溶液进行吸光度的测定，从而求得MnYbO3对甲基橙的降解率，实验结果如图3所示。从图3可知，光催化反应的前60min，MnYbO3对甲基橙的光催化降解速率较快；而60min至150min范围内，光催化降解速率有所变慢，经过150min光催化反应后，甲基橙的降解率达到了90.1％，这表明MnYbO3对甲基橙具有良好的紫外光催化降解活性。
实施例2
在室温条件下，分别将0.005mol乙酸锰和0.005mol硝酸镱分别溶于50mL的蒸馏水中备用。向加热至50℃的50ml乙酸锰溶液中加入0.015mol的柠檬酸，待柠檬酸溶解后加入备用的50mL硝酸镱溶液，然后再加入0.06mol的尿素得到混合溶液，将混合溶液继续搅拌反应15min得到反应溶液。将100mL反应液放入微波炉中，在保持微波功率1500W条件下反应18min至完全燃烧得到初产物，冷却至室温取出初产物，将初产物放入马弗炉中于600℃煅烧1h，冷却至室温取出研磨细得到MnYbO3粉体产品。按照实施例1相同的光催化实验方法，MnYbO3光催化降解20mg/L的甲基橙溶液150min时，甲基橙降解率达到了90.8％，MnYbO3粉体产品对甲基橙表现出了良好的紫外光催化降解活性。
实施例3
在室温条件下，分别将0.005mol的乙酸锰和0.005mol的硝酸镱分别溶于50mL的蒸馏水中备用。向加热至50℃的50ml乙酸锰溶液中加入0.013mol的柠檬酸，待柠檬酸溶解后加入备用的50mL硝酸镱溶液，然后再加入0.055mol的尿素得到混合溶液，将混合溶液继续搅拌反应15min得到反应溶液。将100mL反应液放入微波炉中，在保持微波功率1400W条件下反应18min至完全燃烧得到初产物，冷却至室温取出初产物，将初产物放入马弗炉中于625℃煅烧1h，冷却至室温取出研磨细得到MnYbO3粉体产品。按照实施例1相同的光催化实验方法，MnYbO3光催化降解20mg/L的甲基橙溶液150min时，甲基橙降解率达到了90.5％，MnYbO3粉体产品对甲基橙表现出了良好的紫外光催化降解活性。
Claims (3)
1.一种MnYbO3粉体的方法，其特征在于包括以下步骤(1)反应溶液的配制：在室温条件下，分别将0.005mol乙酸锰和0.005mol硝酸镱分别溶于50mL的蒸馏水中备用；在搅拌条件下，向加热至50℃的50mL的乙酸锰溶液中加入0.012mol至0.015mol的柠檬酸，待柠檬酸溶解后加入备用的50mL硝酸镱溶液，然后再加入0.05mol至0.06mol的尿素得到混合溶液，将混合溶液继续搅拌反应15min得到反应溶液；(2)将100mL反应液放入微波炉中，微波反应18min至完全燃烧得到初产物，冷却至室温取出初产物，将初产物放入马弗炉中煅烧1h，冷却至室温取出研磨细得到MnYbO3粉体产品。
2.如权利要求1所述的一种MnYbO3粉体的方法，其特征在于微波反应时的微波功率为1250W～1500W。
3.如权利要求1所述的一种MnYbO3粉体的方法，其特征在于初产物在马弗炉中煅烧时的温度为600℃～650℃。
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