CN106379934B - 一种制备Ho2TiO5粉体的方法 - Google Patents
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- 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
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- WDVGLADRSBQDDY-UHFFFAOYSA-N holmium(3+);trinitrate Chemical compound [Ho+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O WDVGLADRSBQDDY-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 238000000862 absorption spectrum Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 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
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- YNTQLDAKESBVBG-UHFFFAOYSA-N [O-2].[Ti+4].[Ho+3] Chemical compound [O-2].[Ti+4].[Ho+3] YNTQLDAKESBVBG-UHFFFAOYSA-N 0.000 description 1
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- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 description 1
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- 238000013032 photocatalytic reaction Methods 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract
一种制备Ho2TiO5粉体的方法，涉及一种Ho2TiO5材料的制备方法。本发明利用微波加热处理再煅烧的技术，以柠檬酸、硝酸钬、钛酸四丁酯和尿素为原料制备了颗粒平均粒径0.2μm～0.5μm和带隙3.3eV，并且具有良好紫外光催化活性的Ho2TiO5粉体。其步骤分为反应溶液的配制和粉体产品的制备两步。本发明具有制备时间短和能耗低，达到了快速高效、可工业化生产Ho2TiO5粉体的优点。
Description
技术领域
本发明涉及钛酸盐材料的制备，特别是涉及一种制备Ho2TiO5粉体的方法。
背景技术
Ho2TiO5(Holmium Titanium Oxide)是稀土钛酸盐系列的一种，如文献(PHYSICALREVIEW B，2007，76：054430)报道Ho2TiO5是一种具有烧绿石结构的复合氧化物(pyrochlorecompounds)，具有良好的磁性，在磁性材料等领域有广泛的应用前景。
目前，制备Ho2TiO5的方法主要是高温固相反应法。如文献(PHYSICAL REVIEW B，2007，76：054430)报道以Ho2O3和TiO2为起始原料，采用高温固相反应法在氩气气氛条件下，于1700℃煅烧12h制备得到Ho2TiO5。高温固相反应法的高温煅烧过程易导致Ho2TiO5颗粒的团聚和长大，实现1700℃的高温需要较昂贵的特殊设备，并且1700℃的高温煅烧会消耗更多的能源，存在制备工艺较复杂、耗时长和成本高等缺点，工业化应用前景堪忧。
微波加热技术具有加热速度快、效率高、反应条件易于控制、易于工业化和节能高效等优点，在材料制备领域具有广泛的应用，但利用微波加热技术来协助制备Ho2TiO5粉体还未见报道。
发明内容
本发明的目的在于克服现有技术的不足，提供一种制备Ho2TiO5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，将柠檬酸溶于蒸馏水中制得浓度为0.3mol/L的柠檬酸溶液30毫升；在强烈搅拌条件下，向柠檬酸溶液中加入X mol/L的硝酸钬溶液100毫升，然后缓慢加入Y摩尔钛酸四丁酯，再向溶液中加入Z摩尔尿素，继续搅拌20min得到反应液。
(2)粉体产品的制备
将130毫升反应液放入微波炉中，在保持微波功率1000W～1200W条件下反应25min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700℃～800℃温度范围煅烧2h，冷却至室温取出研磨细得到Ho2TiO5粉体产品。
本发明将X限定在0.04至0.08范围，将Y限定在0.002摩尔至0.004摩尔范围，控制使X∶Y等于20∶1。将Z限定在0.016摩尔至0.032摩尔范围，控制使Z∶Y等于8∶1；本发明 中柠檬酸的络合作用和可燃性，以及尿素提供的碱性环境都为Ho2TiO5的最终形成创造了条件；本发明将微波功率限定在1000W～1200W的范围，马弗炉温度限定700℃～800℃的范围，因为适当的微波功率和温度范围才能为反应的持续进行提供合适的能量。
与现有采用高温固相反应法在氩气气氛条件下于1700℃煅烧12h制备Ho2TiO5的技术相比，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700℃～800℃温度煅烧2h即可得到Ho2TiO5粉体产品，具有制备时间短、能耗低和成本低等优点，达到了快速高效、可工业化生产Ho2TiO5粉体的目的。
附图说明
图1：实施例1所得Ho2TiO5产品的XRD图；
图2：实施例1所得Ho2TiO5产品的扫描电镜照片；
图3：实施例1所得Ho2TiO5产品的漫反射吸收谱；
图4：实施例1所得Ho2TiO5产品光催化降解甲基橙的降解率随时间的变化曲线。
具体实施方式
实施例1
在室温条件下，称取1.9克柠檬酸溶于蒸馏水中，配置得到浓度为0.3mol/L的柠檬酸溶液30毫升。在强烈搅拌条件下，向柠檬酸溶液中加入0.04mol/L的硝酸钬溶液100毫升，然后缓慢加入0.002摩尔钛酸四丁酯，再向溶液中加入0.016摩尔尿素，继续搅拌20min得到反应液。将反应液放入微波炉中，调节微波炉的功率为1000W，微波反应25min至其完全燃烧，冷却至室温取出初产物，将初产物放入马弗炉中于700℃煅烧2h，冷却至室温取出研磨细得到Ho2TiO5粉体产品。对得到的产品分别进行X射线衍射分析(XRD)、扫描电镜(SEM)和漫反射吸收谱(DRS)测试，结果如图1、图2和图3所示。
图1是采用XD-6型X射线衍射分析仪，粉末法分析测试产品得到的XRD图。从图1可知，所得产品的XRD图谱与标准的Ho2TiO5(PDF#36-1236)完全吻合，这表明制备得到的产品是Ho2TiO5。
图2是采用日立S-3400N型扫描电镜测试产品的扫描电镜照片。从图2可知，Ho2TiO5产品以平均粒径0.2μm～0.5μm的颗粒存在为主，颗粒虽有团聚，但总体上均匀性好。
图3是采用美国热电公司的带积分球的EV220型紫外-可见光谱仪，以标准的BaSO4作参比，将Ho2TiO5粉末压片，然后进行测试得到的漫反射谱，并通过Kubelka-Munk方程转换为漫反射吸收谱。从图3可知，Ho2TiO5的吸收边波长λ为375nm。根据Kubelka-Munk理论， 利用公式E(eV)＝1240/λ计算得到Ho2TiO5的带隙宽度为3.3eV，这为Ho2TiO5粉体的光催化活性奠定了基础。
为了表征Ho2TiO5粉末的光催化活性，光催化实验在自制的光催化反应装置中进行：光源为150W高压汞灯；将20mg Ho2TiO5粉体加入到10毫升20mg/L的模拟污水甲基橙溶液中，避光吸附平衡15min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末，以甲基橙溶液最大吸收峰464nm处吸光度的标准曲线计算其脱色降解率，实验结果如图4所示。从图4可知，Ho2TiO5对甲基橙溶液的脱色降解率在120min范围内，随光照时间的增加近似线性增加，120min时已经接近100％完全降解，Ho2TiO5产品表现出了良好的紫外光催化活性。
实施例2
在室温条件下，称取1.9克柠檬酸溶于蒸馏水中，配置得到浓度为0.3mol/L的柠檬酸溶液30毫升。在强烈搅拌条件下，向柠檬酸溶液中加入0.06mol/L的硝酸钬溶液100毫升，然后缓慢加入0.003摩尔钛酸四丁酯，再向溶液中加入0.024摩尔尿素，继续搅拌20min得到反应液。将反应液放入微波炉中，调节微波炉的功率为1200W，微波反应25min至其完全燃烧，冷却至室温取出初产物，将初产物放入马弗炉中于700℃煅烧2h，冷却至室温取出研磨细得到Ho2TiO5粉体产品。按照实施例1相同的光催化实验方法，光催化降解20mg/L的甲基橙溶液120min时，甲基橙脱色率达到99.8％，Ho2TiO5粉体产品表现出了良好的光催化活性。
实施例3
在室温条件下，称取1.9克柠檬酸溶于蒸馏水中，配置得到浓度为0.3mol/L的柠檬酸溶液30毫升。在强烈搅拌条件下，向柠檬酸溶液中加入0.08mol/L的硝酸钬溶液100毫升，然后缓慢加入0.004摩尔钛酸四丁酯，再向溶液中加入0.032摩尔尿素，继续搅拌20min得到反应液。将反应液放入微波炉中，调节微波炉的功率为1200W，微波反应25min至其完全燃烧，冷却至室温取出初产物，将初产物放入马弗炉中于800℃煅烧2h，冷却至室温取出研磨细得到Ho2TiO5粉体产品。按照实施例1相同的光催化实验方法，光催化降解20mg/L的甲基橙溶液120min时，甲基橙脱色率达到99.3％，Ho2TiO5粉体产品表现出了良好的光催化活性。
Claims (1)
1.一种制备Ho2TiO5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，将柠檬酸溶于蒸馏水中制得浓度为0.3mol/L的柠檬酸溶液30毫升；在强烈搅拌条件下，向柠檬酸溶液中加入X mol/L的硝酸钬溶液100毫升，其中将X限定在0.04至0.08范围；然后缓慢加入Y摩尔钛酸四丁酯，其中将Y限定在0.002摩尔至0.004摩尔范围，并控制使X∶Y等于20∶1；再向溶液中加入Z摩尔尿素，其中将Z限定在0.016摩尔至0.032摩尔范围，并控制使Z∶Y等于8∶1；继续搅拌20min得到反应液；(2)粉体产品的制备：将130毫升反应液放入微波炉中，在保持微波功率1000W～1200W条件下反应25min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700℃～800℃温度范围煅烧2h，冷却至室温取出研磨细得到Ho2TiO5粉体产品。
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