CN101774630B - 一种水溶性卤化银纳米粒子的制备方法 - Google Patents
一种水溶性卤化银纳米粒子的制备方法 Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 29
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 28
- 239000004332 silver Substances 0.000 title claims abstract description 28
- -1 silver halide Chemical class 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 10
- 150000002367 halogens Chemical class 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 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 8
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical group [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
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- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- GYCHYNMREWYSKH-UHFFFAOYSA-L iron(ii) bromide Chemical compound [Fe+2].[Br-].[Br-] GYCHYNMREWYSKH-UHFFFAOYSA-L 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 claims description 3
- 229910021590 Copper(II) bromide Inorganic materials 0.000 claims description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 3
- 229910021612 Silver iodide Inorganic materials 0.000 claims description 3
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 3
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 3
- 229910001626 barium chloride Inorganic materials 0.000 claims description 3
- 229940045511 barium chloride Drugs 0.000 claims description 3
- 229940045105 silver iodide Drugs 0.000 claims description 3
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 3
- 235000009518 sodium iodide Nutrition 0.000 claims description 3
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- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 2
- 229910021575 Iron(II) bromide Inorganic materials 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 claims description 2
- 229910001622 calcium bromide Inorganic materials 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 229960002713 calcium chloride Drugs 0.000 claims description 2
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 claims description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 2
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 claims description 2
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- 229940045803 cuprous chloride Drugs 0.000 claims description 2
- 229940046149 ferrous bromide Drugs 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229960003284 iron Drugs 0.000 claims description 2
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- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
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- 229960004839 potassium iodide Drugs 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940083599 sodium iodide Drugs 0.000 claims description 2
- 229940102001 zinc bromide Drugs 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 15
- 230000005540 biological transmission Effects 0.000 abstract description 4
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
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Abstract
本发明公开了一种水溶性卤化银纳米粒子的制备方法。方法是将0.1～50g分子量为10000～500000的超支化聚缩水甘油加入到50～1000mL去离子水中，搅拌1min～1hr后，加入0.01～5g的银盐，继续搅拌1min～2hr，然后加入含卤素的酸或盐，含卤素的酸或盐与银盐的摩尔比为0.43～1.05，搅拌1min～1hr，得到水溶性的卤化银纳米粒子。其粒径为2～20纳米，粒子尺寸分布均匀，水溶性好。本发明操作简单，原料易得，适宜大量制备。本发明所制备的水溶性的卤化银颗粒用透射电子显微镜对其粒径进行了观察，用能谱仪测试了其元素组成，用X-射线衍射仪对晶体结构进行了表征。结果表明制得的水溶性卤化银纳米粒子粒径为2～20纳米，结晶好。
Description
技术领域
本发明涉及的是纳米材料领域，具体是一种水溶性卤化银纳米粒子的制备方法
背景技术
水溶性卤化银纳米粒子在涂料、颜料、光敏性材料、影像处理剂、催化等方面有重要的应用。由于卤化银在水中极容易沉淀，所以在水相中通过普通的共沉淀法制备的卤化银颗粒粒径一般都在亚微米(一百纳米到一微米之间)甚至微米级别，难以得到水溶性的卤化银纳米粒子。
发明内容
本发明的目的在于克服现有技术的不足，提供一种水溶性卤化银纳米粒子的制备方法。
水溶性卤化银纳米粒子的制备方法包括以下步骤：
1)将0.1～50g分子量为10000～500000的超支化聚缩水甘油加入到50～1000mL去离子水中，搅拌1min～1hr后，再加入0.01～5g的银盐，继续搅拌1min～2hr，得到含银离子的超支化聚缩水甘油水溶液。
2)将含卤素的酸或盐加入到含银离子的超支化聚缩水甘油水溶液中，含卤素的酸或盐与银盐的摩尔比为0.43～1.05，搅拌1min～2hr，得到水溶性的卤化银纳米粒子。
所述的卤化银纳米粒子为氯化银、溴化银或碘化银。所述的银盐为硝酸银、硫酸银或醋酸银。所述的含卤素的酸为盐酸、溴酸或碘酸；所述的含卤素的盐为氯化铵、氯化钠、氯化钾、氯化钙、氯化钡、氯化镁、氯化铜、氯化亚铜、氯化铁、氯化亚铁、氯化锌、溴化铵、溴化钠、溴化钾、溴化钙、溴化镁、溴化铜、溴化亚铜、溴化铁、溴化亚铁、溴化锌、碘化钠或碘化钾。
本发明操作简单，原料易得，适宜大量制备。本发明所制备的水溶性的卤化银颗粒用透射电子显微镜对其粒径进行了观察，用能谱仪测试了其元素组成，用X-射线衍射仪对晶体结构进行了表征。结果表明制得的水溶性卤化银纳米粒子粒径为2～20纳米，结晶好。
附图说明
图1是水溶性氯化银纳米粒子的透射电子显微镜图；
图2是水溶性氯化银纳米粒子的能谱图；
图3是水溶性溴化银纳米粒子的透射电子显微镜图；
图4是水溶性溴化银纳米粒子的能谱图。
具体实施方式
本发明所述的超支化聚缩水甘油参照文献(Macromolecules 2006，39，7708-7717)制备。在烧瓶中加入0.003～1g三羟甲基丙烷，0.001～1g甲醇钾和5～30mL四氢呋喃，反复抽充氮气三次，在30～90℃搅拌5min～1hr后，在40～100℃真空干燥10min～3hr除去四氢呋喃，再在氮气氛围下加入5～80mL二氧六环，加热到80～130℃，然后滴加1～200mL缩水甘油单体到烧瓶中，滴加时间为1～48hr，滴加完后继续反应30min～24hr，得到分子量为10000～500000的超支化聚缩水甘油。
下面的实施例是对本发明的进一步说明，而不是限制本发明的范围。
实施例1：
步骤1)：将1g分子量为20000的超支化聚缩水甘油加入到装有100mL去离子水的烧瓶中，搅拌30min后，再加入0.2g硝酸银，继续搅拌1hr，得到含银离子的超支化聚缩水甘油水溶液。
步骤2)：将0.07g氯化钠加入到步骤1)所得到的含银离子的超支化聚缩水甘油水溶液中，搅拌1hr，得到水溶性的氯化银纳米粒子。其透射电子显微镜图片如附图1所示，粒径为2～8纳米，粒子分散性好。其能谱分析图如附图2所示，证实了银元素和氯元素的存在。
实施例2：
步骤1)：将10g分子量为80000的超支化聚缩水甘油加入到装有300mL去离子水的烧瓶中，搅拌1hr后，再加入0.5g硝酸银，继续搅拌2hr，得到含银离子的超支化聚缩水甘油水溶液。
步骤2)：将0.36g溴化钾加入到步骤1)所得到的含银离子的超支化聚缩水甘油水溶液中，搅拌1hr，得到水溶性的溴化银纳米粒子。其透射电子显微镜图片如附图3所示，粒径为2～6纳米，粒子分散性好。其能谱分析图如附图4所示，证实了银元素和溴元素的存在。
实施例3：
步骤1)：将2g分子量为10000的超支化聚缩水甘油加入到装有100mL去离子水的烧瓶中，搅拌30min后，再加入0.01g硫酸银，继续搅拌2hr，得到含银离子的超支化聚缩水甘油水溶液。
步骤2)：将0.0047g氯化钾加入到步骤1)所得到的含银离子的超支化聚缩水甘油水溶液中，搅拌15min，得到水溶性的氯化银纳米粒子。
实施例4：
步骤1)：将0.1g分子量为120000的超支化聚缩水甘油加入到装有50mL去离子水的烧瓶中，搅拌1min后，再加入0.02g硝酸银，继续搅拌1hr，得到含银离子的超支化聚缩水甘油水溶液。
步骤2)：将0.013g溴化铜加入到步骤1)所得到的含银离子的超支化聚缩水甘油水溶液中，搅拌1min，得到水溶性的溴化银纳米粒子。
实施例5：
步骤1)：将50g分子量为120000的超支化聚缩水甘油加入到装有1000mL去离子水的烧瓶中，搅拌1hr后，再加入5g硝酸银，继续搅拌2hr，得到含银离子的超支化聚缩水甘油水溶液。
步骤2)：将4.2g碘化钠加入到步骤1)所得到的含银离子的超支化聚缩水甘油水溶液中，搅拌1hr，得到水溶性的碘化银纳米粒子。
实施例6：
步骤1)：将1g分子量为500000的超支化聚缩水甘油加入到装有80mL去离子水的烧瓶中，搅拌30min后，再加入0.15g硝酸银，继续搅拌1hr，得到含银离子的超支化聚缩水甘油水溶液。
步骤2)：将0.09g氯化钡加入到步骤1)所得到的含银离子的超支化聚缩水甘油水溶液中，搅拌1hr，得到水溶性的氯化银纳米粒子。
实施例7：
步骤1)：将10g分子量为120000的超支化聚缩水甘油加入到装有500mL去离子水的烧瓶中，搅拌1hr后，再加入0.25g硝酸银，继续搅拌1hr，得到含银离子的超支化聚缩水甘油水溶液。
步骤2)：将1.5mL 1mol/L的盐酸加入到步骤1)所得到的含银离子的超支化聚缩水甘油水溶液中，搅拌1hr，得到水溶性的氯化银纳米粒子。
Claims (4)
1.一种水溶性卤化银纳米粒子的制备方法，其特征在于包括以下步骤：
1)将0.1～50g分子量为10000～500000的超支化聚缩水甘油加入到50～1000mL去离子水中，搅拌1min～1hr后，再加入0.01～5g的银盐，继续搅拌1min～2hr，得到含银离子的超支化聚缩水甘油水溶液；
2)将含卤素的酸或盐加入到含银离子的超支化聚缩水甘油水溶液中，含卤素的酸或盐与银盐的摩尔比为0.43～1.05，搅拌1min～1hr，得到水溶性的卤化银纳米粒子；
所述的卤化银纳米粒子为氯化银、溴化银或碘化银。
2.根据权利要求1所述的一种水溶性卤化银纳米粒子的制备方法，其特征在于步骤1)中所述的银盐为硝酸银、硫酸银或醋酸银。
3.根据权利要求1所述的一种水溶性卤化银纳米粒子的制备方法，其特征在于所述的含卤素的酸为盐酸、溴酸或碘酸。
4.根据权利要求1所述的一种水溶性卤化银纳米粒子的制备方法，其特征在于所述的含卤素的盐为氯化铵、氯化钠、氯化钾、氯化钙、氯化钡、氯化镁、氯化铜、氯化亚铜、氯化铁、氯化亚铁、氯化锌、溴化铵、溴化钠、溴化钾、溴化钙、溴化镁、溴化铜、溴化亚铜、溴化铁、溴化亚铁、溴化锌、碘化钠或碘化钾。
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