CN108745379A - 一种硫氰化银/多酸纳米复合材料的制备方法 - Google Patents
一种硫氰化银/多酸纳米复合材料的制备方法 Download PDFInfo
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 41
- 239000004332 silver Substances 0.000 title claims abstract description 41
- 238000006365 thiocyanation reaction Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 11
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 238000001914 filtration Methods 0.000 claims abstract description 3
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 5
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound 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=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 3
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- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 2
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 claims description 2
- AYKOTYRPPUMHMT-UHFFFAOYSA-N silver;hydrate Chemical compound O.[Ag] AYKOTYRPPUMHMT-UHFFFAOYSA-N 0.000 claims description 2
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- GKKCIDNWFBPDBW-UHFFFAOYSA-M potassium cyanate Chemical compound [K]OC#N GKKCIDNWFBPDBW-UHFFFAOYSA-M 0.000 claims 1
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 14
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- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 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 description 1
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- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 1
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 description 1
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- 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 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 description 1
- UYDPQDSKEDUNKV-UHFFFAOYSA-N phosphanylidynetungsten Chemical group [W]#P UYDPQDSKEDUNKV-UHFFFAOYSA-N 0.000 description 1
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- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
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Abstract
本发明一种硫氰化银/多酸纳米复合材料的制备方法，属于无机纳米材料制备技术领域，包括以下步骤：将硫氰酸或硫氰酸盐与多酸或多酸盐加入到水中，形成溶液A；将银盐加入到水中形成溶液B；将溶液A与B混合，然后反应0.5‑5小时，过滤得到产物；将产物用水或乙醇洗涤，干燥得到硫氰化银/多酸纳米复合材料。本发明利用简单一步共沉淀制备了硫氰化银/多酸纳米复合材料，组成和粒径均可控，解决了复合材料制备工艺复杂的问题；制备方法及工艺简便，对环境无害，适于大规模工业化生产，应用前景广泛；所制备的硫氰化银/多酸纳米复合材料性能优异，结构稳定性高。
Description
技术领域
本发明属于无机纳米材料制备技术领域，具体涉及一种硫氰化银/多酸纳米复合材料的制备方法。
背景技术
近些年随着人们对于环境保护的要求越来越高和环保力度的增大，如何有效的处理经济发展所带来的环境污染已经是现阶段的研究重点。特别是人类赖以生存的水资源的污染处理，更是迫在眉睫。此外，随着化石燃料的日渐枯竭，如何利用可再生能源处理环境污染也是研究的难点。利用太阳光和廉价的高效光催化剂处理污水是目前最有前景的处理方式。但是绝大多数的光催化剂只能是利用太阳光中的紫外光和可见光。在太阳光下的光催化性能不尽如人意。因此，近些年人们的研发的重点逐渐转向太阳光驱动的光催化剂的研发(例如发明专利201710829833.2；201710448210.0；201810106888.5；201611046738.7；201610078833.9)。
银基光催化剂是一种常用的可见光催化剂，具有高效的光催化性能。但是由于银基光催化剂容易受到光刻蚀，结构稳定性较差。并且银基光催化剂受限于纳米颗粒本身的比表面的影响，对有机污染物的吸附量较小，难以进一步提升银基光催化材料的催化性能。而且，银基光催化材料的制备工艺较为复杂，不利于工业化转化。发展一种制备工艺简单，对环境无害并且可在温和条件下使用的太阳光驱动的光催化材料及其简易的制备方法已经成为目前科学研究和实际应用领域的研究热点和难点。
发明内容
本发明提供了一种硫氰化银/多酸纳米复合材料的制备方法，利用简易的常温一步共沉淀反应制备了纳米复合材料，所制备的硫氰化银/多酸复合材料的组成和粒径可控，催化性能和稳定性变现优异，该制备方法工艺流程简单、成本低及适合规模化生产。
为了实现上述目的，本发明采用的技术方案为：
本发明一种硫氰化银/多酸纳米复合材料的制备方法，包括以下步骤：
1)将硫氰酸或硫氰酸盐与多酸或多酸盐加入到水中，形成溶液A；
2)将银盐加入到水中形成溶液B；
3)将溶液A与B混合，然后反应0.5-5小时，过滤得到产物；
4)将产物用水或乙醇洗涤，干燥得到硫氰化银/多酸纳米复合材料。
步骤1)中硫氰酸或硫氰酸盐、多酸或多酸盐和水的质量比为1：(0.05-1)：(50-500)。
所述多酸为磷钨酸、硅钨酸或磷钼酸中的一种或几种的组合；所述多酸盐为磷钨酸盐、硅钨酸盐或磷钼酸盐中的一种或几种的组合；所述的硫氰酸盐为硫氰酸铵、硫氰酸钠或硫氰酸钾中的一种或几种的组合。
步骤2)中所述的银盐为硝酸银或乙酸银中的一种或二者的组合。
步骤2)中银盐与水的质量比为1：(1-100)。
步骤4)中干燥温度为50-100℃，干燥时间为1-24小时。
本发明的有益效果为：
(1)本发明利用简单一步共沉淀制备了硫氰化银/多酸纳米复合材料，组成和粒径均可控，解决了复合材料制备工艺复杂的问题。
(2)制备方法及工艺简便，对环境无害，适于大规模工业化生产，应用前景广泛。
(3)所制备的硫氰化银/多酸纳米复合材料性能优异，结构稳定性高。
附图说明
图1是实施例1中硫氰化银/多酸的XRD图
图2是实施例1中硫氰化银/多酸的扫描电镜图
图3是实施例1中染料分子降解图
具体实施方式:
下面结合实施例对本发明做进一步说明，但不限于此。降解物为5mg/L的罗丹明B染料溶液。
实施例1
将0.1g硫氰化钠和0.05g磷钼酸加入到30mL水中，溶解后形成溶液A。将0.2g硝酸银加入到10mL水中形成溶液B。将溶液B加入到溶液A中并反应3h。然后将产物用水洗涤3次，在真空干燥箱中80℃干燥12h。
由图1的XRD图谱可知，硫氰化银/多酸纳米复合物的晶体结构主要为硫氰化银。由图2的扫描电镜图可知，其形貌为纳米颗粒。
将0.05g硫氰化银/多酸复合材料加入到100mL罗丹明B溶液或亚甲基蓝溶液中(浓度均为5mg/L)，黑暗中搅拌30min后，加入0.5mL双氧水(浓度为30wt％)进行降解实验。由图3对罗丹明B的降解可知，硫氰化银/多酸复合材料在60分钟内可完全降解罗丹明B。
实施例2
如实施例1所述，所不同的是加入硫氢化铵和磷钨酸。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达100％。
实施例3
如实施例1所述，所不同的是加入硫氰化钾和磷钼酸铵。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达100％。
实施例4
如实施例1所述，所不同的是加入乙酸银。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达100％。
实施例5
如实施例1所述，所不同的加入0.1g磷钼酸。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达95％。
实施例6
如实施例1所述，所不同的是将0.2g硝酸银加入到20mL水中形成溶液B。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达95％。
实施例7
如实施例1所述，所不同的是常温反应0.5h。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达98％。
实施例8
如实施例1所述，所不同的是常温反应5h。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达92％。
实施例9
如实施例1所述，所不同的是加入0.05g硅钨酸。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达90％。。
实施例10
如实施例1所述，所不同的是加入0.1g钨锗酸。所得所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达90％。
实施例11
如实施例1所述，所不同的是在空气气氛下的干燥箱中干燥。所得硫氰化银/多酸复合纳米材料在60min对罗丹明B的降解达100％。
Claims (6)
1.一种硫氰化银/多酸纳米复合材料的制备方法，其特征在于，包括以下步骤：
1)将硫氰酸或硫氰酸盐与多酸或多酸盐加入到水中，形成溶液A；
2)将银盐加入到水中形成溶液B；
3)将溶液A与B混合，然后反应0.5-5小时，过滤得到产物；
4)将产物用水或乙醇洗涤，干燥得到硫氰化银/多酸纳米复合材料。
2.根据权利要求1所述的一种硫氰化银/多酸纳米复合材料的制备方法，其特征在于，步骤1)中硫氰酸或硫氰酸盐、多酸或多酸盐和水的质量比为1：(0.05-1)：(50-500)。
3.根据权利要求1或2所述的一种硫氰化银/多酸纳米复合材料的制备方法，其特征在于，所述多酸为磷钨酸、硅钨酸或磷钼酸中的一种或几种的组合；所述多酸盐为磷钨酸盐、硅钨酸盐或磷钼酸盐中的一种或几种的组合；所述的硫氰酸盐为硫氰酸铵、硫氰酸钠或硫氰酸钾中的一种或几种的组合。
4.根据权利要求1所述的一种硫氰化银/多酸纳米复合材料的制备方法，其特征在于，步骤2)中所述的银盐为硝酸银或乙酸银中的一种或二者的组合。
5.根据权利要求1所述的一种硫氰化银/多酸纳米复合材料的制备方法，其特征在于，步骤2)中银盐与水的质量比为1：(1-100)。
6.根据权利要求1所述的一种硫氰化银/多酸纳米复合材料的制备方法，其特征在于，步骤4)中干燥温度为50-100℃，干燥时间为1-24小时。
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