CN107311135A - A kind of preparation method of polypody shape phosphoric acid ag material - Google Patents
A kind of preparation method of polypody shape phosphoric acid ag material Download PDFInfo
- Publication number
- CN107311135A CN107311135A CN201710574201.6A CN201710574201A CN107311135A CN 107311135 A CN107311135 A CN 107311135A CN 201710574201 A CN201710574201 A CN 201710574201A CN 107311135 A CN107311135 A CN 107311135A
- Authority
- CN
- China
- Prior art keywords
- solution
- phosphoric acid
- preparation
- ionic liquid
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims description 20
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims description 10
- 241000592274 Polypodium vulgare Species 0.000 title claims 10
- 239000000243 solution Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002608 ionic liquid Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims 2
- 235000021317 phosphate Nutrition 0.000 claims 2
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical class CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 claims 1
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims 1
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- AYKOTYRPPUMHMT-UHFFFAOYSA-N silver;hydrate Chemical compound O.[Ag] AYKOTYRPPUMHMT-UHFFFAOYSA-N 0.000 claims 1
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 abstract description 22
- 229940019931 silver phosphate Drugs 0.000 abstract description 22
- 229910000161 silver phosphate Inorganic materials 0.000 abstract description 22
- DGLRDKLJZLEJCY-UHFFFAOYSA-L disodium hydrogenphosphate dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].OP([O-])([O-])=O DGLRDKLJZLEJCY-UHFFFAOYSA-L 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002244 precipitate Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- JIWPXWWZICHKEO-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;dihydrogen phosphate Chemical compound OP(O)([O-])=O.CCCC[N+]=1C=CN(C)C=1 JIWPXWWZICHKEO-UHFFFAOYSA-M 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- AJAACDDASFNKSC-UHFFFAOYSA-N dihydrogen phosphate;2-ethyl-3-methyl-1h-imidazol-3-ium Chemical compound OP(O)([O-])=O.CCC=1NC=C[N+]=1C AJAACDDASFNKSC-UHFFFAOYSA-N 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- RXFYJLHIPHJRCS-UHFFFAOYSA-M dihydrogen phosphate;1-ethyl-3-methylimidazol-3-ium Chemical compound OP(O)([O-])=O.CCN1C=C[N+](C)=C1 RXFYJLHIPHJRCS-UHFFFAOYSA-M 0.000 description 1
- KDQPSPMLNJTZAL-UHFFFAOYSA-L disodium hydrogenphosphate dihydrate Chemical compound O.O.[Na+].[Na+].OP([O-])([O-])=O KDQPSPMLNJTZAL-UHFFFAOYSA-L 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910001958 silver carbonate Inorganic materials 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
本发明公开了一种多足状磷酸银材料的制备方法。该制备方法包括以下步骤：1)将硝酸银溶解在水中，搅拌，得到溶液A；2)将十二水磷酸氢二钠溶解在离子液体和水组成的混合溶液中，搅拌，超声分散，得到溶液B；3)将溶液A滴加到溶液B中，搅拌，得到悬浊液C；4)将悬浊液C进行水热反应，冷却，分离沉淀，洗涤，干燥，得到多足状磷酸银粉末。本发明以硝酸银、十二水磷酸氢二钠为原料，以离子液体为溶剂、分散剂和模板剂，采用“共沉淀—水热法”制得微米级多足状Ag3PO4。该方法原料易得，离子液体可重复使用，工艺简单，合成温度低。The invention discloses a method for preparing a multipod silver phosphate material. The preparation method comprises the following steps: 1) dissolving silver nitrate in water and stirring to obtain solution A; 2) dissolving disodium hydrogen phosphate dodecahydrate in a mixed solution composed of ionic liquid and water, stirring and ultrasonically dispersing to obtain Solution B; 3) Add solution A dropwise to solution B and stir to obtain suspension C; 4) Perform hydrothermal reaction on suspension C, cool, separate and precipitate, wash, and dry to obtain multipod silver phosphate powder. The invention uses silver nitrate and disodium hydrogen phosphate dodecahydrate as raw materials, ionic liquid as solvent, dispersant and template agent, and adopts "co-precipitation-hydrothermal method" to prepare micron-sized multipod Ag 3 PO 4 . The method has easy-to-obtain raw materials, reusable ionic liquid, simple process and low synthesis temperature.
Description
技术领域technical field
本发明涉及一种多足状磷酸银材料的制备方法。The invention relates to a preparation method of a multipod silver phosphate material.
背景技术Background technique
磷酸银的形貌对其性质有较大的影响。通过加入模板或添加剂可辅助调控磷酸银的生长速率，制备不同形貌的磷酸银。如采用聚碳酸酯模板经化学沉积制备出纳米棒状磷酸银；通过碳酸银和磷酸间的酸蚀，阴离子交换反应制备多孔磷酸银；通过聚乙二醇调控合成3D花状磷酸银；通过水热法制备菱形十二面体磷酸银；以Au@Ag纳米棒为起始材料，基于异质外延生长出凹二十四面体磷酸银；利用柠檬酸钠辅助制备层状结构的多孔微立方体磷酸银。The morphology of silver phosphate has a great influence on its properties. By adding templates or additives, the growth rate of silver phosphate can be assisted to regulate the growth rate of silver phosphate, and silver phosphate with different shapes can be prepared. For example, nano-rod silver phosphate is prepared by chemical deposition using polycarbonate template; porous silver phosphate is prepared by acid etching and anion exchange reaction between silver carbonate and phosphoric acid; 3D flower-shaped silver phosphate is synthesized by polyethylene glycol regulation; hydrothermal rhombic dodecahedral silver phosphate was prepared by the method; using Au@Ag nanorods as the starting material, concave tetrahedral silver phosphate was grown based on heteroepitaxial growth; the porous microcube silver phosphate with layered structure was assisted by sodium citrate .
发明内容Contents of the invention
本发明的目的在于提供一种多足状磷酸银材料的制备方法。The object of the present invention is to provide a method for preparing a multipod silver phosphate material.
本发明所采取的技术方案是：The technical scheme that the present invention takes is:
一种多足状磷酸银材料的制备方法，包括以下步骤：A preparation method of a multipod silver phosphate material, comprising the following steps:
1)将硝酸银溶解在水中，搅拌，得到溶液A；1) Dissolving silver nitrate in water and stirring to obtain solution A;
2)将十二水磷酸氢二钠溶解在离子液体和水组成的混合溶液中，搅拌，超声分散，得到溶液B；离子液体为1-丁基-3-甲基咪唑磷酸二氢盐或1-乙基-3-甲基咪唑磷酸二氢盐中的至少一种；2) Dissolve disodium hydrogen phosphate dodecahydrate in a mixed solution composed of ionic liquid and water, stir, and disperse ultrasonically to obtain solution B; the ionic liquid is 1-butyl-3-methylimidazolium dihydrogen phosphate or 1 - at least one of ethyl-3-methylimidazole dihydrogen phosphate;
3)将溶液A滴加到溶液B中，搅拌，得到悬浊液C；3) Add solution A dropwise to solution B and stir to obtain suspension C;
4)将悬浊液C进行水热反应，冷却，分离沉淀，洗涤，干燥，得到多足状磷酸银粉末。4) Suspension C is subjected to hydrothermal reaction, cooled, separated and precipitated, washed and dried to obtain multipod silver phosphate powder.
步骤1)中，硝酸银与水的用量比为1g：(15～25)mL。In step 1), the dosage ratio of silver nitrate to water is 1 g: (15-25) mL.
步骤2)中，十二水磷酸氢二钠、离子液体和水的用量比为1g：(8～20)mL：(2～5)mL。In step 2), the dosage ratio of disodium hydrogen phosphate dodecahydrate, ionic liquid and water is 1 g: (8-20) mL: (2-5) mL.
步骤3)中，溶液A的滴加速度为每1滴2～4秒。In step 3), the dropping speed of solution A is 2-4 seconds per 1 drop.
步骤4)中，水热反应的反应温度为140～200℃，反应时间为15～25h。In step 4), the reaction temperature of the hydrothermal reaction is 140-200° C., and the reaction time is 15-25 hours.
步骤4)中，干燥为真空干燥，干燥温度为40～70℃。In step 4), the drying is vacuum drying, and the drying temperature is 40-70°C.
多足状磷酸银粉末的粒径为10～50μm。The particle size of the multipod silver phosphate powder is 10-50 μm.
本发明的有益效果是：The beneficial effects of the present invention are:
本发明以硝酸银、十二水磷酸氢二钠为原料，以离子液体为溶剂、分散剂和模板剂，采用“共沉淀—水热法”制得微米级多足状Ag3PO4。该方法原料易得，离子液体可重复使用，工艺简单，合成温度低。The invention uses silver nitrate and disodium hydrogen phosphate dodecahydrate as raw materials, ionic liquid as solvent, dispersant and template agent, and adopts "co-precipitation-hydrothermal method" to prepare micron-sized multipod Ag 3 PO 4 . The method has easy-to-obtain raw materials, reusable ionic liquid, simple process and low synthesis temperature.
附图说明Description of drawings
图1为实施例制备的多足状Ag3PO4的XRD射线衍射图谱；Fig. 1 is the XRD ray diffraction pattern of the many-legged Ag 3 PO 4 that embodiment prepares;
图2为实施例制备的多足状Ag3PO4在放大倍数为400的SEM图谱；Fig. 2 is the SEM spectrum of the multipod-shaped Ag 3 PO 4 prepared in the embodiment at a magnification of 400;
图3为实施例制备的多足状Ag3PO4在放大倍数为8000的SEM图谱。Fig. 3 is the SEM spectrum of the multipod-shaped Ag 3 PO 4 prepared in the embodiment at a magnification of 8000.
具体实施方式detailed description
一种多足状磷酸银材料的制备方法，包括以下步骤：A preparation method of a multipod silver phosphate material, comprising the following steps:
1)将硝酸银溶解在水中，搅拌，得到溶液A；1) Dissolving silver nitrate in water and stirring to obtain solution A;
2)将十二水磷酸氢二钠溶解在离子液体和水组成的混合溶液中，搅拌，超声分散，得到溶液B；离子液体为1-丁基-3-甲基咪唑磷酸二氢盐或1-乙基-3-甲基咪唑磷酸二氢盐中的至少一种；2) Dissolve disodium hydrogen phosphate dodecahydrate in a mixed solution composed of ionic liquid and water, stir, and disperse ultrasonically to obtain solution B; the ionic liquid is 1-butyl-3-methylimidazolium dihydrogen phosphate or 1 - at least one of ethyl-3-methylimidazole dihydrogen phosphate;
3)将溶液A滴加到溶液B中，搅拌，得到悬浊液C；3) Add solution A dropwise to solution B and stir to obtain suspension C;
4)将悬浊液C进行水热反应，冷却，分离沉淀，洗涤，干燥，得到多足状磷酸银粉末。4) Suspension C is subjected to hydrothermal reaction, cooled, separated and precipitated, washed and dried to obtain multipod silver phosphate powder.
优选的，一种多足状磷酸银材料的制备方法，包括以下步骤：Preferably, a kind of preparation method of multipod shape silver phosphate material, comprises the following steps:
1)将硝酸银溶解在水中，在暗处均匀搅拌20-30min，得到溶液A；1) Dissolve silver nitrate in water, and stir evenly in the dark for 20-30min to obtain solution A;
2)将十二水磷酸氢二钠溶解在含有离子液体和水的混合溶液中，持续搅拌30-60min，再持续超声2-3h，得到溶液B；离子液体为1-丁基-3-甲基咪唑磷酸二氢盐或1-乙基-3-甲基咪唑磷酸二氢盐；2) Dissolve disodium hydrogen phosphate dodecahydrate in a mixed solution containing ionic liquid and water, continue to stir for 30-60 minutes, and then continue to sonicate for 2-3 hours to obtain solution B; the ionic liquid is 1-butyl-3-methyl imidazolium dihydrogen phosphate or 1-ethyl-3-methylimidazolium dihydrogen phosphate;
3)将溶液A逐滴滴加到溶液B中，然后在暗处搅拌30-60min，得到悬浊液C；3) Add solution A dropwise to solution B, then stir in the dark for 30-60min to obtain suspension C;
4)将悬浊液C转入反应釜中，进行水热反应，冷却后，分离沉淀，经洗涤干燥，得到多足状磷酸银粉末。4) Transfer the suspension C into a reaction kettle for hydrothermal reaction, after cooling, separate the precipitate, wash and dry to obtain the multipod silver phosphate powder.
优选的，步骤1)中，硝酸银与水的用量比为1g：(15～25)mL。Preferably, in step 1), the dosage ratio of silver nitrate to water is 1 g: (15-25) mL.
优选的，步骤2)中，十二水磷酸氢二钠、离子液体和水的用量比为1g：(8～20)mL：(2～5)mL；进一步优选的，步骤2)中，十二水磷酸氢二钠、离子液体和水的用量比为1g：(8～12)mL：(2～3)mL。Preferably, in step 2), the dosage ratio of disodium hydrogen phosphate dodecahydrate, ionic liquid and water is 1 g: (8-20) mL: (2-5) mL; further preferably, in step 2), ten The dosage ratio of disodium hydrogen phosphate dihydrate, ionic liquid and water is 1 g: (8-12) mL: (2-3) mL.
优选的，步骤1)或步骤2)中的水为去离子水、超纯水、蒸馏水中的其中一种；进一步优选的，步骤1)或步骤2)中的水为去离子水。Preferably, the water in step 1) or step 2) is one of deionized water, ultrapure water, and distilled water; further preferably, the water in step 1) or step 2) is deionized water.
优选的，步骤3)中，溶液A的滴加速度为每1滴2～4秒。Preferably, in step 3), the dropping speed of solution A is 2-4 seconds per drop.
优选的，步骤4)中，水热反应的反应温度为140～200℃，反应时间为15～25h。Preferably, in step 4), the reaction temperature of the hydrothermal reaction is 140-200° C., and the reaction time is 15-25 hours.
优选的，步骤4)中，干燥为真空干燥，干燥温度为40～70℃。Preferably, in step 4), the drying is vacuum drying, and the drying temperature is 40-70°C.
进一步的，多足状磷酸银粉末的粒径为10～50μm。Further, the particle size of the multipod silver phosphate powder is 10-50 μm.
以下通过具体的实施例对本发明的内容作进一步详细的说明。The content of the present invention will be described in further detail below through specific examples.
实施例：Example:
1)将1.482g硝酸银固体溶解在30mL去离子水中，不断搅拌使之形成澄清的溶液，得到溶液A；1) Dissolve 1.482g of silver nitrate solid in 30mL of deionized water, and keep stirring to form a clear solution to obtain solution A;
2)将2.312g十二水磷酸氢二钠溶解在含有25mL的1-丁基-3-甲基咪唑磷酸二氢盐离子液体和5mL去离子水的混合溶液中，持续搅拌30-60min，再持续超声2-3h，得到溶液B；2) Dissolve 2.312g of disodium hydrogen phosphate dodecahydrate in a mixed solution containing 25mL of 1-butyl-3-methylimidazolium dihydrogen phosphate ionic liquid and 5mL of deionized water, keep stirring for 30-60min, and then Continue to sonicate for 2-3 hours to obtain solution B;
3)将步骤1)制备的溶液A逐滴滴加到步骤2)制备的溶液B中，再加入适量的去离子水，然后在暗处搅拌30-60min，得到悬浊液C；3) Add solution A prepared in step 1) dropwise to solution B prepared in step 2), then add an appropriate amount of deionized water, and then stir in the dark for 30-60min to obtain suspension C;
4)将含有Ag3PO4晶核的悬浊液倒入的聚四氟乙烯反应釜内，置于恒温箱内于160℃水热晶化18h；4) Pour the suspension containing Ag 3 PO 4 crystal nuclei into a polytetrafluoroethylene reactor, and place it in a constant temperature box for hydrothermal crystallization at 160°C for 18 hours;
5)待反应釜自然冷却后倒出溶液，将倒出的溶液在高速离心机内离心收集沉淀，用去离子水和无水乙醇洗涤数次后，在真空恒温箱中50℃下干燥得到灰黑色Ag3PO4粉体。5) Pour out the solution after the reaction kettle is naturally cooled, centrifuge the poured out solution in a high-speed centrifuge to collect the precipitate, wash it with deionized water and absolute ethanol several times, and dry it in a vacuum thermostat at 50°C to obtain ash Black Ag 3 PO 4 powder.
将实施例制备的材料进行X射线衍射分析，XRD射线衍射图谱如附图1所示。从X射线衍射分析得知，实施例制备所得的材料为Ag3PO4。SEM分析图谱如附图2(放大倍数400)和附图3(放大倍数8000)所示。从图2和图3的SEM图谱可见，本发明制备得到的Ag3PO4材料呈现微米级多足状结构，颗粒表面凹凸不平，粒径为10～50μm。The materials prepared in the examples were analyzed by X-ray diffraction, and the XRD ray diffraction pattern is shown in Figure 1. According to X-ray diffraction analysis, the material prepared in the example is Ag 3 PO 4 . The SEM analysis spectrum is shown in accompanying drawing 2 (magnification factor 400) and accompanying drawing 3 (magnification factor 8000). It can be seen from the SEM spectra of Fig. 2 and Fig. 3 that the Ag 3 PO 4 material prepared by the present invention presents a micron-sized multi-pod structure, the surface of the particles is uneven, and the particle size is 10-50 μm.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710574201.6A CN107311135B (en) | 2017-07-14 | 2017-07-14 | A kind of preparation method of polypody shape phosphoric acid ag material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710574201.6A CN107311135B (en) | 2017-07-14 | 2017-07-14 | A kind of preparation method of polypody shape phosphoric acid ag material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107311135A true CN107311135A (en) | 2017-11-03 |
| CN107311135B CN107311135B (en) | 2019-04-05 |
Family
ID=60178796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710574201.6A Expired - Fee Related CN107311135B (en) | 2017-07-14 | 2017-07-14 | A kind of preparation method of polypody shape phosphoric acid ag material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107311135B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940937A (en) * | 2010-10-21 | 2011-01-12 | 武汉理工大学 | High-efficiency visible light catalyst silver phosphate and preparation method thereof |
| CN102698782A (en) * | 2012-06-25 | 2012-10-03 | 武汉理工大学 | Dendrite silver phosphate visible light catalyst and preparation method thereof |
| CN103252246A (en) * | 2013-06-07 | 2013-08-21 | 南京信息工程大学 | Shuttle-type silver phosphate photocatalyst and preparation method thereof |
| CN103626146A (en) * | 2013-12-13 | 2014-03-12 | 扬州大学 | Preparation method of polyhedral silver phosphate |
| CN104085869A (en) * | 2014-07-16 | 2014-10-08 | 辽宁石油化工大学 | Method for synthesizing spindly bismuth phosphate by adopting imidazole dihydric phosphate type ionic liquid |
| WO2017042624A1 (en) * | 2015-09-11 | 2017-03-16 | Uniwersytet Warszawski | Methods for obtaining salts of silver(ii) and hydrates thereof, products obtained by the methods and use of the same |
-
2017
- 2017-07-14 CN CN201710574201.6A patent/CN107311135B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940937A (en) * | 2010-10-21 | 2011-01-12 | 武汉理工大学 | High-efficiency visible light catalyst silver phosphate and preparation method thereof |
| CN102698782A (en) * | 2012-06-25 | 2012-10-03 | 武汉理工大学 | Dendrite silver phosphate visible light catalyst and preparation method thereof |
| CN103252246A (en) * | 2013-06-07 | 2013-08-21 | 南京信息工程大学 | Shuttle-type silver phosphate photocatalyst and preparation method thereof |
| CN103626146A (en) * | 2013-12-13 | 2014-03-12 | 扬州大学 | Preparation method of polyhedral silver phosphate |
| CN104085869A (en) * | 2014-07-16 | 2014-10-08 | 辽宁石油化工大学 | Method for synthesizing spindly bismuth phosphate by adopting imidazole dihydric phosphate type ionic liquid |
| WO2017042624A1 (en) * | 2015-09-11 | 2017-03-16 | Uniwersytet Warszawski | Methods for obtaining salts of silver(ii) and hydrates thereof, products obtained by the methods and use of the same |
Non-Patent Citations (2)
| Title |
|---|
| AIPING WU ET AL.: "morphology -controlled synthesis of Ag3PO4 nano/microcrystals and their antibaterial properties", 《MATERIALS RESEARCH BULLETIN》 * |
| PRASHANTH W.MENEZES ET AL.: "morphology-dependent activaties of silver phosphates:visible-light water oxidation and dye degradation", 《CHEMPLUSCHEM》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107311135B (en) | 2019-04-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| AU2023446716B2 (en) | Method for continuously preparing mixed hydroxide precipitate from laterite nickel ore by hydrometallurgy | |
| CN110054196B (en) | A method for preparing high-purity spherical instant boric acid induced by organic molecules | |
| WO2017121280A1 (en) | Method for continuously producing battery-grade lithium carbonate | |
| CN105523543A (en) | Method for preparing graphene quantum dots with grading increase | |
| CN105586028B (en) | A kind of preparation method of CdSe@CdS core core-shell structure quantum dots | |
| CN102786098B (en) | Preparation method of pyrite-type ferrous disulfide micro/nanocrystalline material with controllable morphology | |
| CN104843661B (en) | A kind of preparation method without templated synthesis phosphoric acid antimony microballoon | |
| CN104117372A (en) | A hydrothermal preparation method of a supported nickel phosphide catalyst with nanometer red phosphorus as a phosphorus source | |
| CN103663530B (en) | A kind of preparation method of calcium carbonate powder | |
| Wang et al. | Hydrothermal synthesis of ZnSe hollow micropheres | |
| CN102842716B (en) | A kind of preparation method of nanoscale lithium iron phosphate | |
| CN104402065B (en) | The preparation method of the spherical cobalt disulfide nano-powder of one kind | |
| CN106946236B (en) | Amorphous nanometer spherical activity phosphoric acid molten iron closes object and its preparation method and application | |
| CN110540255B (en) | Process for preparing nano nickel oxide by water-soluble salt isolation method | |
| WO2024139112A1 (en) | Process and system for preparing iron phosphate by using out-of-kettle circulating mixing and stirring | |
| CN108610489B (en) | Preparation method of nano material based on metal organic framework material and with different dimensions | |
| CN108516578A (en) | A kind of sub-micron indium oxide raw powder's production technology | |
| CN101367541A (en) | A kind of synthetic method of nano copper sulfide | |
| CN104944399B (en) | The preparation method of hydroxyapatite micro-sphere | |
| CN107311135A (en) | A kind of preparation method of polypody shape phosphoric acid ag material | |
| CN103896323A (en) | Method for preparing nanometer zinc oxide with micro-emulsion | |
| CN102603008B (en) | Method for synthesizing nanoscale copper pyrites | |
| CN110510592B (en) | Method for regulating and preparing hydroxyapatite with excellent cell compatibility | |
| CN104607218A (en) | Composite silver bromide-bismuth phosphate heterojunction photocatalytic material and preparation method thereof | |
| CN101269837A (en) | Process for producing Bi2S3 nano-powder body |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190405 |