CN106044840A - 一种十四面体溴化银晶体的制备方法 - Google Patents
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- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 title claims abstract description 42
- 239000013078 crystal Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 108010010803 Gelatin Proteins 0.000 claims abstract description 27
- 229920000159 gelatin Polymers 0.000 claims abstract description 27
- 239000008273 gelatin Substances 0.000 claims abstract description 27
- 235000019322 gelatine Nutrition 0.000 claims abstract description 27
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 17
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 10
- 239000003223 protective agent Substances 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 10
- 238000013019 agitation Methods 0.000 claims description 9
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 230000005070 ripening Effects 0.000 claims description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 abstract description 9
- 230000035800 maturation Effects 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 4
- 238000009775 high-speed stirring Methods 0.000 abstract 1
- 229940006460 bromide ion Drugs 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- -1 Silver halide Chemical class 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 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 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G5/00—Compounds of silver
- C01G5/02—Halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
本发明涉及一种十四面体溴化银晶体的制备方法,所述十四面体溴化银晶体包含{100}和{111}暴露面,其制备方法包括以下步骤:在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到含有明胶溶液的反应锅中,控制反应锅内温度为60−90℃,溴离子浓度为2.8×10‑3−4×10‑3,反应结束后,进行20分钟物理成熟,再用温热水洗涤除去明胶保护剂和无机盐,得到包含{100}和{111}暴露面的十四面体溴化银晶体。本方法具有工艺简单、环保、易大批量制备的特点。
Description
技术领域
本发明涉及一种可应用于水中污染物降解以及光解水光催化材料的制备方法,属于光催化技术领域。
背景技术
进入21世纪,全球范围的环境污染和能源危机变得更加突出,已严重威胁到人类的生存和发展,更成为制约世界各国可持续发展的瓶颈。如何降解日益严重的环境污染和能源污染,已成各国政府普遍关注和亟待解决的头等大事。
自20世纪70年代Fujishima和Honda发现在n型半导体二氧化钛电极上光解水制氢以来,半导体光催化技术受到了广大研究者的广泛关注,并有望在解决日益严重的环境污染和能源危机中发挥关键作用。在环境污染物治理方面,半导体光催化材料可以利用太阳光将水体和大气中的绝大对数有机污染物降解为无毒无害的水和二氧化碳;在解决能源危机方面,半导体光催化材料可以利用太阳光光解水制备氢气,作为不产生污染的清洁能源,满足人类的各种能源需求。此外,半导体材料还可以用于太阳能电池材料,将光能转化为电能。
卤化银半导体材料具有优异光电和光催化特性,在环境污染物治理、光解水制氢制氧、二氧化碳还原等领域具有广阔的应用前景。基于卤化银的半导体材料在这些领域中的应用性能与其形貌结构、晶面以及氧化还原能级等因素密切相关。本发明公开了一种含有{100}和{111}暴露面的十四面体溴化银晶体的制备方法,该制备方法具有工艺简单、环保、易大批量制备等优点。
发明内容
本发明所述十四面体溴化银晶体的制备方法包括以下步骤:
在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到含有明胶溶液的反应锅中,反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,得到包含{100}和{111}暴露面的十四面体溴化银晶体。
上述十四面体溴化银晶体的制备方法,反应温度为60−90℃,反应锅内溴离子浓度为2.8×10-3−4×10-3 mol/L。
附图说明
图1为实施例1得到十四面体溴化银晶体的X射线衍射图;
图2为实施例1得到十四面体溴化银晶体的扫描电镜图;
图3为实施例1得到的十四面体溴化银晶体在可见光下降解甲基橙曲线。
具体实施方式
以下结合实例对本发明进行进一步的详述。
实施例1
首先,将反应锅内的明胶水溶液上升到85℃,并维持在该温度不变。在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到上述明胶水溶液中,控制蠕动泵的流速,使反应锅内的溴离子浓度始终保持在(3.2 ± 0.1)×10-3 mol/L。反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,即得到包含{100}和{111}暴露面的十四面体溴化银晶体。
图1为实施例1得到十四面体溴化银晶体的X射线衍射图,衍射峰的出峰位置与溴化银的标准谱图((JCPDS文件: 06-438)一致,确认了制备样品的确为溴化银。
图2为实施例1得到十四面体溴化银晶体的扫描电镜图,根据晶体的集合构型,可以判定所制备溴化银为包含{100}和{111}暴露面的十四面体。
图3为实施例1得到十四面体溴化银晶体在可见光下光催化降解甲基橙曲线,从图中可以看出,十四面体溴化银具有比立方体和八面体溴化银更高的光催化活性。
实施例2
首先,将反应锅内的明胶水溶液上升到60℃,并维持在该温度不变。在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到上述明胶水溶液中,控制蠕动泵的流速,使反应锅内的溴离子浓度始终保持在(3.2 ± 0.1)×10-3 mol/L。反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,即得到包含{100}和{111}暴露面的十四面体溴化银晶体。
实施例3
首先,将反应锅内的明胶水溶液上升到75℃,并维持在该温度不变。在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到上述明胶水溶液中,控制蠕动泵的流速,使反应锅内的溴离子浓度始终保持在(3.2 ± 0.1)×10-3 mol/L。反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,即得到包含{100}和{111}暴露面的十四面体溴化银晶体。
实施例3
首先,将反应锅内的明胶水溶液上升到90℃,并维持在该温度不变。在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到上述明胶水溶液中,控制蠕动泵的流速,使反应锅内的溴离子浓度始终保持在(3.2 ± 0.1)×10-3 mol/L。反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,即得到包含{100}和{111}暴露面的十四面体溴化银晶体。
实施例4
首先,将反应锅内的明胶水溶液上升到85℃,并维持在该温度不变。在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到上述明胶水溶液中,控制蠕动泵的流速,使反应锅内的溴离子浓度始终保持在(2.8 ± 0.1)×10-3 mol/L。反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,即得到包含{100}和{111}暴露面的十四面体溴化银晶体。
实施例5
首先,将反应锅内的明胶水溶液上升到85℃,并维持在该温度不变。在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到上述明胶水溶液中,控制蠕动泵的流速,使反应锅内的溴离子浓度始终保持在(3.6 ± 0.1)×10-3 mol/L。反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,即得到包含{100}和{111}暴露面的十四面体溴化银晶体。
实施例6
首先,将反应锅内的明胶水溶液上升到85℃,并维持在该温度不变。在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到上述明胶水溶液中,控制蠕动泵的流速,使反应锅内的溴离子浓度始终保持在(4.0 ± 0.1)×10-3 mol/L。反应结束后,进行20分钟物理成熟。然后,用温热水洗涤除去明胶保护剂和无机盐,即得到包含{100}和{111}暴露面的十四面体溴化银晶体。
Claims (3)
1.一种十四面体溴化银晶体的制备方法,其特征在于,所述十四面体溴化银晶体包含{100}和{111}暴露面,其制备过程包括以下步骤:
在高速搅拌下,用蠕动泵将硝酸银溶液和溴化银溶液同时注入到含有明胶溶液的反应锅中,反应结束后,进行20分钟物理成熟,再用温热水洗涤除去明胶保护剂和无机盐,得到包含{100}和{111}暴露面的十四面体溴化银晶体。
2.根据权利要求1所述的十四面体溴化银晶体的制备方法,其特征在于,反应温度为60−90℃。
3.根据权利要求1所述的十四面体溴化银晶体的制备方法,其特征在于,反应锅内溴离子浓度为2.8×10-3−4×10-3 mol/L。
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GB2038792A (en) * | 1978-12-26 | 1980-07-30 | Du Pont | Novel silver halide crystals with two surface types |
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GB2038792A (en) * | 1978-12-26 | 1980-07-30 | Du Pont | Novel silver halide crystals with two surface types |
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陈朝等: "溴化银晶体生长的影响因素", 《影像技术》 * |
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Application publication date: 20161026 |