CN106145185B - 一种片状氟氧铋光催化剂的制备方法 - Google Patents
一种片状氟氧铋光催化剂的制备方法 Download PDFInfo
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- VLIDWTIBMJLJIS-UHFFFAOYSA-N [Bi]=O.[F] Chemical compound [Bi]=O.[F] VLIDWTIBMJLJIS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000003054 catalyst Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 235000019628 coolness Nutrition 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 5
- 239000011259 mixed solution Substances 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 3
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
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- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- UOBPHQJGWSVXFS-UHFFFAOYSA-N [O].[F] Chemical compound [O].[F] UOBPHQJGWSVXFS-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910001451 bismuth ion Inorganic materials 0.000 description 1
- -1 bismuthino compound Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种片状氟氧铋的制备方法。本发明的制备方法以乙醇和纯水的混合溶液为溶剂,依次加入五水硝酸铋、氟化铵和氨水,制备出了片状氟氧铋,该种氟氧铋晶体形貌呈片状。本发明的制备方法简单,有利于大规模推广,且制备出的催化剂具有良好的光催化活性。该光催化剂制备方法环保,简单,成本低廉,能够有效去除水中有机污染物,催化剂具有良好的应用前景。
Description
技术领域
本发明涉及一种片状氟氧铋光催化剂的制备方法,属化学材料技术领域。
背景技术
目前随着工业的发展,有机污染污染物的排放已经成为了一个严重的环境问题。半导体光催化材料,能够解决当前的环境和能源问题,已经引起了相当大的关注。目前研究方向除了工作集中于二氧化钛,也开始着手开发其他新型高效的催化剂,可一般分为氧化物、硫化物、含氧酸盐和聚合物。因为铋离子具有孤对电子,铋基化合物被发现具有杂化结构,所以光催化剂作为新型的光催化剂吸引了大家的关注。众所周知,氟原子有较强的电负性,因此氟暴露可以强烈吸附或陷阱电子,氟可以有效地影响电子分布。同时,氟可以有效改善光催化剂的催化活性已经被广泛的被报道。经过实验证明片状氟氧铋比锐钛矿有更宽的带隙,这样有利于阻止空穴和电子的复合,这样能提高光催化剂的催化效率。由此可见它在光催化方面具有巨大的潜力。据此,我们利用液相沉淀法制备了片状氟氧铋,该方法操作简便、具有可控性,生成的产物具有更高的化学均匀性、粒度较细、颗粒尺寸分布较窄且具有一定形貌。同时,在紫外光照下其降解罗丹眀B的速率要高于商业金红石,因此片状氟氧铋可作为一种易于合成,利于推广,催化活性良好的光催化剂。
发明内容
本发明的目的是提供一种简单易行,有利于大规模推广,催化活性良好的片状氟氧铋光催化剂的制备方法。
本发明的技术方案如下:
本发明的片状氟氧铋光催化剂的制备方法为:
该方法以无水乙醇和水的混合溶液为溶剂,在高压釜内反应生成片状氟氧铋,具体步骤包括:
步骤1,在容器中加入水和无水乙醇,搅拌条件下,加入五水硝酸铋;水和无水乙醇的体积比为14:1,五水硝酸铋对应每毫升无水乙醇的加入量为0.4g-0.5g;
步骤2,搅拌20min加入氟化铵;五水硝酸铋和氟化铵的摩尔比要为1:6;
步骤3,再加入0.1mol/L氨水;氨水对应每毫升无水乙醇的加入量为15mL;
步骤4,搅拌10min后倒入高压釜,将高压釜密闭放入160℃的烘箱,放置12h后取出,静置2h冷却;
步骤5,将上层清液倒掉,用纯水将下层固体洗入离心管内,先用纯水离心洗涤2遍,在用无水乙醇离心洗涤2遍,120-160℃烘干2小时。
本发明的进一步设计在于:
所用五水硝酸铋和氟化铵的摩尔比要为1:6。
所用的氨水对应每毫升无水乙醇的加入量为15mL,氨水的浓度为0.1mol/L。
在乙醇和纯水混合溶液中加入五水硝酸铋和氟化铵是在搅拌条件下进行的。
离心洗涤时,先用纯水洗2遍,再用无水乙醇洗2遍。
本发明的有益效果如下:
本发明的制备方法以乙醇和纯水的混合溶液为溶剂,依次加入五水硝酸铋、氟化铵和氨水,制备出了片状氟氧铋,该种氟氧铋晶体形貌呈片状。
本发明的制备方法简单,有利于大规模推广,且制备出的催化剂具有良好的光催化活性。
附图说明:
图1是该种方法制备的片状氟氧铋的XRD图谱,经过比对所有衍射峰和标准卡一致(JCPDS:73-1595),无杂质峰,可表明氟氧铋纯相形成;
图2是在扫描电子显微镜(SEM)下的图像,可以看出晶体形貌为片状;
图3分别是透射电子显微镜(TEM),可以看出片状边长为3-4μm左右;
图4为高分辨透射电镜(HRTEM)表现出明显晶格条纹间距d为0.31,可以索引到(002)面图;图4右上角插图是选区电子衍射(SAED)。
具体实施方式
实施例一:
在容器中加入14mL水和1mL无水乙醇,搅拌条件下,加入0.4g-0.5g的五水硝酸铋;搅拌20min后加入0.2g-0.3g氟化铵;搅拌10min后再加入15mL0.1mol/L氨水,最后倒入高压釜,将高压釜密闭放入160℃的烘箱,放置12h后取出,静置2h等待冷却;将上层清液倒掉,用纯水将下层固体洗入离心管内,先用纯水离心洗涤2遍,在用无水乙醇离心洗涤2遍,150℃干燥2小时,自然冷却即得。
上述方法制备的片状氟氧铋其晶体片尺寸约为3-4×3-4μm。图1是该片状氟氧铋的XRD图谱,经过比对所有衍射峰和标准卡一致(JCPDS:73-1595),无杂质峰,可表明氟氧铋纯相形成;图2是其在扫描电子显微镜(SEM)下的图像,可以看出晶体形貌为片状;图3是其透射电子显微镜(TEM),可以看出片状边长为3-4μm左右;图4是其高分辨透射电镜(HRTEM)表现出明显晶格条纹间距d为0.31,可以索引到(002)面图;图4右上角插图是选区电子衍射(SAED)。
Claims (1)
1.一种片状氟氧铋光催化剂的制备方法,其特征在于:该方法以无水乙醇和水的混合溶液为溶剂,在高压釜内反应生成片状氟氧铋,具体步骤包括:
步骤1,在容器中加入水和无水乙醇,搅拌条件下,加入五水硝酸铋;水和无水乙醇的体积比为14:1,五水硝酸铋对应每毫升无水乙醇的加入量为0.4 g-0.5 g;
步骤2,搅拌20min后加入氟化铵;五水硝酸铋和氟化铵的摩尔比要为1:6;
步骤3,再加入0.1mol/L 氨水;氨水对应每毫升无水乙醇的加入量为15mL;
步骤4,搅拌10min后倒入高压釜,将高压釜密闭放入160oC的烘箱,放置12 h后取出,静置2h冷却;
步骤5,将上层清液倒掉,用纯水将下层固体洗入离心管内,先用纯水离心洗涤2遍,在用无水乙醇离心洗涤2遍,120-160oC烘干2小时。
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CN101664687A (zh) * | 2009-09-29 | 2010-03-10 | 福州大学 | 一种染料敏化的卤氧化铋可见光催化剂的制备及其应用 |
CN102974373A (zh) * | 2012-12-24 | 2013-03-20 | 山东大学 | 一种可见光光催化材料及其制备方法 |
CN103265076A (zh) * | 2013-06-07 | 2013-08-28 | 南京信息工程大学 | 一种片状氯氧铋光催化剂的制备方法 |
CN103769175A (zh) * | 2014-03-04 | 2014-05-07 | 南京信息工程大学 | 一种复合光催化剂的制备方法及其应用 |
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CN101664687A (zh) * | 2009-09-29 | 2010-03-10 | 福州大学 | 一种染料敏化的卤氧化铋可见光催化剂的制备及其应用 |
CN102974373A (zh) * | 2012-12-24 | 2013-03-20 | 山东大学 | 一种可见光光催化材料及其制备方法 |
CN103265076A (zh) * | 2013-06-07 | 2013-08-28 | 南京信息工程大学 | 一种片状氯氧铋光催化剂的制备方法 |
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