CN107115859A - 三氧化钨纳米晶光催化剂的制备方法 - Google Patents
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 title claims description 7
- 239000003054 catalyst Substances 0.000 title abstract description 10
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- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 150000003657 tungsten Chemical class 0.000 claims description 14
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000007848 Bronsted acid Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- RWZYAGGXGHYGMB-UHFFFAOYSA-N anthranilic acid Chemical compound NC1=CC=CC=C1C(O)=O RWZYAGGXGHYGMB-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 229960004050 aminobenzoic acid Drugs 0.000 claims description 6
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- 238000010438 heat treatment Methods 0.000 claims description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 4
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims description 2
- AAQNGTNRWPXMPB-UHFFFAOYSA-N dipotassium;dioxido(dioxo)tungsten Chemical compound [K+].[K+].[O-][W]([O-])(=O)=O AAQNGTNRWPXMPB-UHFFFAOYSA-N 0.000 claims description 2
- -1 m-aminophenyl Chemical group 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims 1
- 229910052721 tungsten Inorganic materials 0.000 claims 1
- 239000010937 tungsten Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 3
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 7
- 229910001930 tungsten oxide Inorganic materials 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 5
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
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- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical group [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
本发明公开了一种单斜晶系三氧化钨纳米晶光催化剂的制备方法。其以水热法制备出的W18O49为前驱体,对其进行进一步的焙烧,从而合成出单斜相三氧化钨纳米晶。本发明通过调节形貌保护剂用量、焙烧温度等显著提高了制备得到的光催化剂的催化吸附降解性能,制备工艺简单,催化剂比表面积大。
Description
技术领域
本发明涉及一种单斜晶系三氧化钨纳米晶光催化剂的制备方法,属于无机非金属材料制备技术领域。
背景技术
氧化钨由于原料来源广泛、价格低、绿色无污染以及光稳定等特点被认为是最有希望的光催化剂之一,已在清除水和大气污染物的实验中得到了成功应用。虽然氧化钨有着广泛的应用,但氧化钨在光催化方面还存在一些缺陷。主要是由于:其导带的位置较低,这使得其具有较高氧化能力的价带所产生的光生空穴在光氧化过程中受到了抑制作用。研究如何使氧化钨光催化剂能够有效利用太阳光并具有较高的光生载流子利用效率具有重要的理论和实践意义。因此,需要开发不同的合成及改性方法以提高氧化钨基光催化剂的光催化活性。
发明内容
本发明的目的在于提供一种单斜晶系三氧化钨纳米晶光催化剂的制备方法,通过对晶体结构的调控提高催化剂吸附降解染料性能。
本发明实现过程如下:
一种三氧化钨纳米晶的制备方法,其以可溶性钨盐为原料,加入形貌控制保护剂和水,将体系置于150~200 oC下密闭水热反应得到前驱体W18O49,再将前驱体W18O49在300~600oC下煅烧得到JCPDS卡片号为72-0677的单斜晶系三氧化钨纳米晶,所述形貌控制保护剂选自对氨基苯甲酸、邻氨基苯甲酸或间氨基苯甲酸,可溶性钨盐与形貌控制保护剂的质量比为(0.5~4.5):(1~6);
上述可溶性钨盐选自钨酸钠、钨酸钾、偏钨酸铵或仲钨酸铵。
上述可溶性钨盐先分散在摩尔浓度为0.5~3.5 M的质子酸中,可溶性钨盐与质子酸的质量体积比为(5~15):(10~20)g/ml,经冷冻干燥后使用,所述质子酸选自盐酸、硝酸、硫酸。
上述前驱体W18O49在350~420 oC下煅烧得到JCPDS卡片号为72-0677的单斜晶系三氧化钨纳米晶。
具体地说,本发明三氧化钨纳米晶的制备方法包括以下步骤:
(1)将5~15 g可溶性钨盐分散在10~20 mL的质子酸盐酸、硝酸或硫酸中,酸摩尔浓度为0.5~3.5M,冷冻干燥;
(2)将0.5~4.5 g 干燥后产物与1~6 g对氨基苯甲酸、邻氨基苯甲酸或者间氨基苯甲酸中的一种或者几种溶解在50~100 mL水中,再将体系转移入四氟乙烯釜内衬,反应釜在150~200 oC下水热12~48 h;
(3)待体系冷却后先用水离心洗涤,再用无水乙醇洗涤,产物在50~80 oC下烘干2~8h得到W18O49前驱体;
(4)将W18O49前驱体在300~600 oC下保温10~60 min,升温速率:0.5~3.5 oC min-1,最后得到单斜晶系三氧化钨纳米晶。
本发明有益效果:本发明提出了一种工艺简单、成本低廉,水热、焙烧相结合的方法,通过加入形貌控制保护剂合成出化学稳定性和结构稳定性优异的氧化钨纳米晶,其高比表面积可以暴露出更多活性位点,提高了对光的利用率,对染料废水的处理具有优异效果,在工业上有广泛应用前景。
附图说明
图1为三氧化钨的透射电镜图;
图2为三氧化钨的X射线粉末衍射图;
图3为不同焙烧温度下三氧化钨的的吸附性能图。
具体实施方式
实施例1
将6 g可溶性钨盐分散在15 mL的质子酸盐酸中,酸浓度为1.5 M,冷冻干燥;将0.6 g干燥后产物与5 g对氨基苯甲酸溶解在80 mL水中,再将体系转移入四氟乙烯釜胆,反应釜在160 oC下水热24 h;待体系冷却后先用水离心洗涤,再用无水乙醇洗涤,产物在60 oC下烘干6 h到W18O49前驱体。将5 g W18O49前驱体在400 oC下保温20 min(升温速率:1 oC min-1),最后得到单斜晶系三氧化钨纳米晶。得到的三氧化钨的透射电镜图(图1)显示产物为纳米棒状, X射线粉末衍射图(图2)结果为单斜晶系三氧化钨,JCPDS卡片号为72-0677;其光催化降解亚甲基蓝的性能较好(图3)。
实施例2
将6 g可溶性钨盐分散在15 mL的质子酸盐酸中,酸摩尔浓度为1.5 M,冷冻干燥;将0.6g 干燥后产物与5 g对氨基苯甲酸溶解在80 mL水中,再将体系转移入四氟乙烯釜胆,反应釜在160 oC下水热24 h;待体系冷却后先用水离心洗涤,再用无水乙醇洗涤,产物在60 oC下烘干6 h到W18O49前驱体。将5 g W18O49前驱体在500 oC下保温20 min(升温速率:1 oC min-1),最后得到单斜晶系三氧化钨纳米晶,其光催化降解亚甲基蓝的性能如图3所示。
本发明通过控制制备工艺的水热时间、水热温度、焙烧温度等因素,成功获得了单斜相三氧化钨纳米晶光催化剂,并提高了其光催化降解亚甲基蓝的性能。
Claims (6)
1.一种三氧化钨纳米晶的制备方法,其特征在于:以可溶性钨盐为原料,加入形貌控制保护剂和水,将体系置于150~200 oC下密闭水热反应得到前驱体W18O49,再将前驱体W18O49在300~600 oC下煅烧得到JCPDS卡片号为72-0677的单斜晶系三氧化钨纳米晶,所述形貌控制保护剂选自对氨基苯甲酸、邻氨基苯甲酸或间氨基苯甲酸,可溶性钨盐与形貌控制保护剂的质量比为(0.5~4.5):(1~6)。
2.根据权利要求1所述的三氧化钨纳米晶的制备方法,其特征在于:可溶性钨盐选自钨酸钠、钨酸钾、偏钨酸铵或仲钨酸铵。
3.根据权利要求1所述的三氧化钨纳米晶的制备方法,其特征在于:所述可溶性钨盐先分散在摩尔浓度为0.5~3.5 M的质子酸中,可溶性钨盐与质子酸的质量体积比为(5~15):(10~20)g/ml,经冷冻干燥后使用。
4.根据权利要求3所述的三氧化钨纳米晶的制备方法,其特征在于:所述质子酸选自盐酸、硝酸、硫酸。
5.根据权利要求1所述的三氧化钨纳米晶的制备方法,其特征在于:前驱体W18O49在350~420 oC下进行煅烧。
6.根据权利要求1所述的三氧化钨纳米晶的制备方法,其特征在于包括以下步骤:
(1)将5~15 g可溶性钨盐分散在10~20 mL的质子酸盐酸、硝酸或硫酸中,酸摩尔浓度为0.5~3.5M,冷冻干燥;
(2)将0.5~4.5 g 干燥后产物与1~6 g对氨基苯甲酸、邻氨基苯甲酸或者间氨基苯甲酸中的一种或者几种溶解在50~100 mL水中,再将体系转移入四氟乙烯釜内衬,反应釜在150~200 oC下水热12~48 h;
(3)待体系冷却后先用水离心洗涤,再用无水乙醇洗涤,产物在50~80 oC下烘干2~8 h得到W18O49前驱体;
(4)将W18O49前驱体在300~600 oC下保温10~60 min,升温速率:0.5~3.5 oC min-1,最后得到单斜晶系三氧化钨纳米晶。
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Cited By (6)
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CN107597155A (zh) * | 2017-09-27 | 2018-01-19 | 大连民族大学 | 一种一锅法合成具有可见光响应的光催化剂BiPO4/WO3纳米片的制备方法 |
CN110624534A (zh) * | 2019-10-21 | 2019-12-31 | 吉林建筑大学 | 一种生物遗态的wo3光催化剂及其制备方法和应用 |
CN111774051A (zh) * | 2020-06-02 | 2020-10-16 | 贵州理工学院 | 光热催化醇类脱水制乙烯和有机产物的催化剂及制备方法 |
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