CN106185856B - A kind of method and its product and purposes using ionic liquid liquid phase support membranous system preparation phosphorylation rare earth nano material - Google Patents
A kind of method and its product and purposes using ionic liquid liquid phase support membranous system preparation phosphorylation rare earth nano material Download PDFInfo
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- CN106185856B CN106185856B CN201610495007.4A CN201610495007A CN106185856B CN 106185856 B CN106185856 B CN 106185856B CN 201610495007 A CN201610495007 A CN 201610495007A CN 106185856 B CN106185856 B CN 106185856B
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 102
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 68
- 230000026731 phosphorylation Effects 0.000 title claims abstract description 58
- 238000006366 phosphorylation reaction Methods 0.000 title claims abstract description 58
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 58
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 55
- 239000007791 liquid phase Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- -1 rare earth ion Chemical class 0.000 claims abstract description 64
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 46
- 239000010452 phosphate Substances 0.000 claims abstract description 46
- 239000012071 phase Substances 0.000 claims abstract description 44
- 239000012528 membrane Substances 0.000 claims abstract description 34
- 230000005291 magnetic effect Effects 0.000 claims abstract description 10
- 238000013019 agitation Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 9
- 239000002033 PVDF binder Substances 0.000 claims description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 150000002460 imidazoles Chemical class 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229910010272 inorganic material Inorganic materials 0.000 claims description 4
- 239000011147 inorganic material Substances 0.000 claims description 4
- 239000011368 organic material Substances 0.000 claims description 4
- 239000004964 aerogel Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- WXMVWUBWIHZLMQ-UHFFFAOYSA-N 3-methyl-1-octylimidazolium Chemical compound CCCCCCCCN1C=C[N+](C)=C1 WXMVWUBWIHZLMQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 229940079593 drug Drugs 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims 1
- 230000007797 corrosion Effects 0.000 claims 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical group OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims 1
- 230000005855 radiation Effects 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 23
- 239000011521 glass Substances 0.000 description 22
- 235000011007 phosphoric acid Nutrition 0.000 description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 20
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 6
- 241000209094 Oryza Species 0.000 description 6
- 235000007164 Oryza sativa Nutrition 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
- 239000004519 grease Substances 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 230000000873 masking effect Effects 0.000 description 6
- 229910017604 nitric acid Inorganic materials 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 239000004568 cement Substances 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 210000001124 body fluid Anatomy 0.000 description 2
- 239000010839 body fluid Substances 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/5115—Inorganic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0036—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions by adsorption or absorption
-
- 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1804—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with rare earths or actinides
-
- B01J35/40—
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- B01J35/51—
-
- B01J35/61—
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- 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
- C01P2004/32—Spheres
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- 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
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
Abstract
The present invention relates to a kind of method using ionic liquid liquid phase support membranous system preparation phosphorylation rare earth nano material and its product and purposes, and described method includes following steps：1) liquid phase support membrane is impregnated with ionic liquid, obtains ionic liquid liquid phase support membrane；2) prepare rare earth ion supply respectively mutually and phosphate anion supplies phase；3) assembling ionic liquid liquid phase supports membranous system；4) it is reacted under magnetic agitation, obtains the phosphorylation rare earth nano material of the present invention.The preparation method simple and effective, can implement under room temperature, environmental pressure, and preparation condition is mild, in addition, not being related to template in the method, reduce the puzzlement of environmental pollution, be easy to implement industrialization, can greatly reduce production cost.
Description
Technical field
The invention belongs to field of nanometer material technology, more particularly to a kind of the preparation method and its system of phosphorylation rare earth nano material
Product and purposes.
Background technology
So-called rare earth element refers to that lanthanide series adds the scandium Sc and yttrium Y for belonging to III B races, totally 17 kinds of elements.These yuan
Element has electronic structure identical, and electronic configuration similar in internal layer 4f electron energy levels, electricity price are high, radius is big, polarization force is strong, change
Learn property it is active and can hydrolyze etc. properties thus there is good light, electricity, magnetic performance, therefore its apply it is very extensive.It is especially existing
For the development and application of some new type functional materials, rare earth element has become indispensable raw material.China is rare earth resources
Big country, the development and application of rare earth nano material are the new ways opened up rare earth resources and efficiently used, and are found easy, efficient
Preparation method is also at active demand.
Nano material refers to the material that at least one-dimensional geometric dimension reaches nano-scale dimension in space three-dimensional.Material nano
Change will assign material many be different from macroscopic view characteristic, nano-particle have skin effect, bulk effect, quantum size effect and
Macroscopical tunnel-effect makes particle while keeping original physics and chemical property, electricity, magnetics, optics, mechanics, calorifics,
Chemistry etc. shows peculiar performance.
Rare earth phosphate nanometer material is due to good chemical stability and thermostabilization, being mainly used in high performance
Optical device, catalysis, biological tracer mark and converting photons, laser etc..In addition to this, the rare earth phosphoric acid with special appearance
Salt is nanocrystalline to have potential application prospect in magnetic material, electronic material and optical material etc..Different preparation methods
Microscopic appearance, particle size and the photoluminescence performance that luminescent material can be influenced with reaction condition, to influence its application.With
The continuous development of nano material preparation technology and perfect, people oneself through being prepared with many different physical methods and chemical method
The nano luminescent material of different sizes, different structure and different compositions, and its characteristics of luminescence is studied.Traditional preparation
Method mainly has hydro-thermal method, ultrasonic method, chemical precipitation method etc., since various technologies respectively have advantage and disadvantage, various preparation methods are excellent
Change combination, maximize favourable factors and minimize unfavourable ones, while positive discussion nano material novel preparation method, also will be synthesis Nano-scale Rare-earth Luminescent Materials hair
Exhibition trend.
Liquid phase supports membranous system as one of most efficient piece-rate system, is by two parts supply phase, liquid film phase three parts
Composition, when the supply phase on liquid phase film both sides, reception are identical, coupling linkage carries out respectively for extraction and the back extraction of metal.Liquid film phase is then
Containing a kind of carrier of selective binding target metal ions, metal can be injected to the hole of microporous membrane.Liquid phase support membrane
The key that system can efficiently separate not only has higher requirements to carrier, also requires liquid film good stabilization in longtime running
Property.However, among practical application, using conventional organic solvents as liquid film phase, maintaining a long-term stability property has certain difficulty.
In recent years ionic liquid due to its unique property start instead of effect of the organic solvent in liquid-liquid extraction and liquid film separation it is convex
It is aobvious.Ionic liquid at room temperature (room temperature ionic liquids, RTILs) is by positively charged and negative electricity ion structure
At being in a liquid state under room temperature or lower temperature.Ionic liquid is referred to as " green " solvent, and compared with conventional solvent, it has very
Low vapour pressure, hypotoxicity, incombustibility, wide potential windows, very wide liquid range, high ionic conductivity and preferably heat is steady
It is qualitative, not only academicly there is good researching value, is also having broad application prospects in industrial production.
Invention content
Of low cost, high flux, safety and environmental protection are prepared the object of the present invention is to provide a kind of, convenient for the system of industrialized production
The method of the phosphorylation nano material of standby rare earth and other metals.
It is a further object to provide phosphorylation nano materials and application thereof prepared by the above method.
The invention is realized in this way a kind of utilizing ionic liquid liquid phase support membranous system separation-nanosizing reaction coupling
The method that linkage prepares phosphorylation rare earth nano material comprising following steps：
1) porous membrane material is impregnated with ionic liquid, to obtain required ionic liquid liquid phase support membrane；
2) prepare rare earth ion supply respectively mutually and phosphate anion supplies phase；
3) assembling ionic liquid liquid phase supports membranous system comprising is located at rare earth made from the step 2) of carrying respectively of both sides
Ion supply is mutually and phosphate anion supplies ionic liquid body fluid made from the container of phase and the step 1) between two containers
Phase support membrane；Rare earth ion supply made from above-mentioned step 2) is mutually mutually injected separately into above-mentioned appearance with phosphate anion supply
In device, the container of the both sides is communicated by the ionic liquid liquid phase support membrane between container；
4) two containers are stirred respectively, and are reacted and obtained the phosphorylation rare earth nano material.
According to the present invention, the ionic liquid in step 1) is selected from imidazoles system ionic liquid.The imidazoles system ionic liquid example
As being [Cnmim] [Tf2N], [Cnmim] [PF6], [Cnmim] [BF4], n=2-16, it is further preferred that n=4-10.Preferably, institute
It is, for example, [Bmim] [Tf to state imidazoles system ionic liquid2N]、[Omim][Tf2N]、[Bmim][PF6]、[Bmim][BF4] etc.,
In, n is that n is 8 in 4, Omim in Bmim.
According to the present invention, the porous membrane material in step 1), for example, HVHP dewatering microporous films, PVDF dewatering microporous films or core
Pore membrane.The aperture of the porous membrane material is 200-500nm.
According to the present invention, in step 1), per 10cm2Porous membrane material using 100 μ l or more ionic liquid impregnate.It is described
The time of immersion is 0.1-24 hours, preferably 1-10 hours.
According to the present invention, in step 2), rare earth ion supply is mutually the solution containing rare earth ion, preferably contains rare earth ion
Aqueous solution；The suitable concentration of its Rare Earth Ion is 20ppm-10000ppm.
According to the present invention, in step 2), phosphate anion supply is mutually the solution of phosphorus-containing acid ion；Wherein phosphate radical from
The suitable concentration of son is 0.1M-5M.
Further include the pH for adjusting rare earth ion supply phase after injection rare earth ion supply phase in step 3) according to the present invention
The step of (preferably, adjust pH be 1~6), and/or, in rare earth ion supplies phase other anionic radicals are added is received with controlling
The pattern of rice material.
According to the present invention, in step 4), magnetic stir bar is preferably placed respectively in two containers, it is anti-under magnetic agitation
It answers, obtains the phosphorylation rare earth nano material of the present invention.
It in step 4), is stirred to react and is carried out under room temperature, normal pressure, the reaction time is 1~30min.
According to the present invention, the rare earth in the phosphorylation rare earth nano material is not particularly limited, any rare earth.It is excellent
Choosing, the phosphorylation rare earth nano material includes that the long rodlike phosphorylation rare earth nano material of nanometer, nanometer tufted phosphorylation are dilute
The membranaceous phosphorylation rare earth nano material of native nano material, flat porous or the spherical phosphorylation rare earth nano material of nanometer.It is also more excellent
Selection of land, the membranaceous phosphorylation rare earth nano material of flat porous have the feature structure of whisker interpenetrating networks.
The above-mentioned preparation method of the present invention is equally applicable to the preparation of the phosphate nano material of other metal ions.
The present invention further provides the phosphorylation nano materials being prepared by the above method.
Preferably, the phosphorylation nano material is phosphorylation rare earth nano material.It is further preferred that the phosphorylation
Rare earth nano material includes the long rodlike phosphorylation rare earth nano material of nanometer, nanometer tufted phosphorylation rare earth nano material, plane
Porous membranaceous phosphorylation rare earth nano material or the spherical phosphorylation rare earth nano material of nanometer.It is more preferred still that the plane is more
The membranaceous phosphorylation rare earth nano material in hole has the feature structure of whisker interpenetrating networks.
Membranaceous (feature structure with the whisker interpenetrating networks) phosphorylation rare earth nano material (rare earth of above-mentioned flat porous
Film, rare earth containing zeolite) can be used for environmental improvement, be mainly used for the filtering of high radioactivity human nuclide in nuclear power efflux wastewater with
And aerogel substance is harmful in atmosphere, such as PM2.5 and radioactive dust etc. filtering and absorption.
The spherical phosphorylation rare earth nano material of above-mentioned nanometer (having high-specific surface area) can be widely applied to catalyst
Carrier and drug conveying carrier.
The phosphorylation rare earth nano material of above-mentioned preparation can be used as functional additive, itself and organic/inorganic materials are mixed
It is molten, to improve the fire resistance, wearability and acid-alkali-corrosive-resisting of the organic/inorganic materials.
The beneficial effects of the invention are as follows：
Phosphorylation rare earth nano material preparation method provided by the invention, method is simple, and preparation condition is mild, in room temperature and
It is obtained within the scope of wider pH, pattern is easy regulation and control.This preparation method is cheap using equipment under room temperature, environmental pressure, prepares
Flux is high, and simple and efficient, it is not necessary that template is added, safety and environmental protection is pollution-free, can greatly reduce production cost, be easy to implement
Industrialized production.
Description of the drawings
Fig. 1 is the SEM figures of the long rod-shaped nanometer cerous phosphate of nanometer of high dispersive made from the embodiment of the present invention 1
Fig. 2 is the XRD diagram of the long rod-shaped nanometer cerous phosphate of nanometer of high dispersive made from the embodiment of the present invention 1
Fig. 3 is the SEM figures of the nanometer cerous phosphate of nanometer tufted (flower-shaped) made from the embodiment of the present invention 2
Fig. 4 is the XRD diagram of the nanometer cerous phosphate of nanometer tufted (flower-shaped) made from the embodiment of the present invention 2
Fig. 5 is receiving for flat porous made from the embodiment of the present invention 3 membranaceous (feature structure with whisker interpenetrating networks)
The SEM figures of rice cerous phosphate
Fig. 6 is receiving for flat porous made from the embodiment of the present invention 3 membranaceous (feature structure with whisker interpenetrating networks)
The XRD diagram of rice cerous phosphate
Fig. 7 is receiving for flat porous made from the embodiment of the present invention 4 membranaceous (feature structure with whisker interpenetrating networks)
The SEM figures of rice cerous phosphate
Fig. 8 is receiving for flat porous made from the embodiment of the present invention 4 membranaceous (feature structure with whisker interpenetrating networks)
The XRD diagram of rice cerous phosphate
Fig. 9 is the SEM figures of the spherical nanometer cerous phosphate of nanometer made from the embodiment of the present invention 5
Figure 10 is the XRD diagram of the spherical nanometer cerous phosphate of nanometer made from the embodiment of the present invention 5
Figure 11 equipment therefor schematic diagrames of the present invention
Specific implementation mode
In order to make the purpose of the present invention, technical solution and advantage definitely, with reference to the accompanying drawings and embodiments, to this hair
It is bright to be further elaborated.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used in
Limit the present invention.
As previously mentioned, reacting coupling using ionic liquid liquid phase support membranous system separation-nanosizing the invention discloses a kind of
Close the method that linkage prepares phosphorylation rare earth nano material comprising following steps：
1) porous membrane material is impregnated with ionic liquid, to obtain required ionic liquid liquid phase support membrane；
2) prepare rare earth ion supply respectively mutually and phosphate anion supplies phase；
3) assembling ionic liquid liquid phase supports membranous system comprising is located at rare earth made from the step 2) of carrying respectively of both sides
Ion supply is mutually and phosphate anion supplies ionic liquid body fluid made from the container of phase and the step 1) between two containers
Phase support membrane；Rare earth ion supply made from above-mentioned step 2) is mutually mutually injected separately into above-mentioned appearance with phosphate anion supply
In device；
4) it places magnetic stir bar respectively in two containers, is reacted under magnetic agitation, the phosphorylation for obtaining the present invention is dilute
Native nano material.
In a preferred embodiment of the present invention, in step 2), rare earth ion supply is mutually containing the molten of rare earth ion
Liquid, for example, rare-earth salt solution obtain specifically using soluble rare-earth salt commonly used in the art as solute by solvent configuration of water
Rare-earth salt solution.For example, which can be divided into rare earth nitrades, and Rare Earths salt also includes by rare earth
Oxide reacts the soluble rare-earth salt of (such as nitric acid) generation with acid.
In a preferred embodiment of the present invention, in step 2), phosphate anion supply is mutually phosphorus-containing acid ion
Solution, be using orthophosphoric acid commonly used in the art, soluble phosphoric acid dihydric salt or soluble orthophosphates as solute, be molten with water
The solution (pH is preferably adjusted to make it below rare earth ion supply phase) of phosphorus-containing acid ion obtained by agent configuration.The soluble phosphoric acid
Dihydric salt is, for example, potassium dihydrogen phosphate, sodium dihydrogen phosphate etc.；The solubility orthophosphates is, for example, ammonium phosphate etc..It is produced to improve
Object precision, it is preferably commercially available to analyze pure grade soluble rare-earth salt and orthophosphoric acid, soluble phosphoric acid dihydric salt or soluble orthophosphates,
Preferred solvent is deionized water.
In the present invention, the preparation of the supply phase can carry out in any open-top receptacle such as conical flask and beaker.
In a preferred embodiment of the present invention, step 3) includes assembling ionic liquid liquid phase support membranous system.
The structural schematic diagram of the liquid phase support membranous system is shown in Figure 11, and as shown in figure 11, the system comprises carrying rare earth ion supplies
The glass apparatus of phase, the glass apparatus and ionic liquid liquid phase support membrane of carrying phosphate anion supply phase, two glass apparatus
Staggered relatively, the ionic liquid liquid phase support membrane is placed on the position that two glass apparatus are connected.In advance in two glass
One piece of magneton is respectively added in instrument, wipes vacuum silicon grease on the interface of the opposite connection of two glass apparatus, the support membrane is put
It is placed in the centre of two glass apparatus, cement and is clamped with iron clamp, both sides are injected separately into rare earth ion supply phase and (contain rare earth ion
Solution) and phosphate anion supply phase (solution of phosphorus-containing acid ion), ensure without supply mutually overflows.
In a preferred embodiment of the present invention, further include adjusting after injection rare earth ion supply phase in step 3)
The step of pH (it is 1~6 preferably, to adjust pH) of solution, and/or, other anionic radicals are added in rare earth ion supplies phase
To control the pattern of nano material.Wherein, the sodium hydroxide that various concentration may be used in pH, nitric acid are adjusted, hydrochloric acid etc. is adjusted
Section, other described anionic radicals are added in the form of the salt containing the anion, and the concentration of salt can influence the shape of nano-particle
Looks.The present invention is had found by comparative study, within the pH value adjustable range, rare earth ion and phosphate anion it is mole dense
The change of ratio is spent, the influence of essence will not be generated to the pattern of rare-earth nanometer particles, and the concentration of acid ion is then to particle
There are large effects for size.From the point of view of adjusting in 1~6 range of pH value, the nano material crystallinity that is obtained in comparatively strong acidity
It is good, and the nano material size obtained when relatively low acidity is big.
In a preferred embodiment of the present invention, in step 4), under room temperature, normal pressure system is placed on magnetic force stirs
It mixes on device, keeps rotating speed 300-1800rpm/min (such as 1000rpm/min), reaction 1-30min that can have white precipitate life
At, after the completion of reaction, precipitation is centrifuged from waste liquid and is come out, respectively with deionized water and absolute ethyl alcohol wash three times, in
A conventional oven or vacuum drying may be selected in 70 DEG C of drying, the drying.In order to keep nano-particle well dispersed, it is easy to observe its shape
Looks can also disperse particle in ethanol, to take supernatant liquor to be distributed on masking foil and dried again.
Phosphorylation rare earth nano material preparation method provided by the invention use simple, cheap equipment, simple and effective,
Room temperature can be implemented under environmental pressure, and preparation condition is mild, as long as simple control ph and the concentration of salt can be obtained crystallinity
Good nano material.The invention is not related to template also, reduces the puzzlement of environmental pollution, is easy to implement industrialization, can
Greatly reduce production cost.
Illustrate the preparation method of above-mentioned rare earth phosphate nanometer material below by way of the embodiment of specific preparation method.
Embodiment 1
With ionic liquid [Bmim] [Tf2N] impregnate PVDF dewatering microporous films (0.45 μm thick, diameter 47mm) 2 hours, it obtains
Ionic liquid liquid phase support membrane.
Weigh the cerous nitrate [Ce (NO of certain mass3)3·6H2O] it is dissolved in 55ml deionized waters, it is configured to 2000ppm's
Cerous nitrate aqueous solution is used in combination nitric acid tune pH value to 1, obtains rare earth ion supply phase.The concentrated phosphoric acid for taking certain volume, is diluted with water
At the phosphoric acid solution 55ml of 2mol/l, phosphate anion supply phase is obtained.Liquid phase support membranous system as shown in figure 11 is assembled, in advance
One piece of magneton is respectively first added in two glass apparatus, vacuum silicon grease is wiped on the interface that two glass apparatus are connected, it will be upper
The centre that ionic liquid liquid phase support membrane is positioned over two glass apparatus is stated, cements and is clamped with iron clamp, both sides are injected separately into
The cerous nitrate aqueous solution and phosphoric acid solution stated, system is placed on magnetic stirring apparatus, maintains the rotating speed of 1000rpm/min.Instead
It after answering half an hour, centrifuges, obtains white precipitate, washed three times with deionized water and absolute ethyl alcohol respectively, by product point
It dissipates in ethanol, supernatant liquor is taken to be dispersed on masking foil in 70 DEG C of drying.SEM phenograms visible phosphoric acid obtained (see Fig. 1)
Cerium is that nanometer is long rodlike；XRD characterization figure shows that obtained nanometer cerous phosphate is hexagonal phase (see Fig. 2).
Embodiment 2
With ionic liquid [Bmim] [Tf2N] impregnate PVDF dewatering microporous films (0.45 μm thick, diameter 47mm) 2 hours, it obtains
Ionic liquid liquid phase support membrane.
Weigh the cerous nitrate [Ce (NO of certain mass3)3·6H2O] it is dissolved in 55ml deionized waters, it is configured to 2000ppm's
Cerous nitrate aqueous solution is used in combination nitric acid tune pH value to 2, obtains rare earth ion supply phase.The concentrated phosphoric acid for taking certain volume, is diluted with water
At the phosphoric acid solution 55ml of 2mol/l, phosphate anion supply phase is obtained.Liquid phase support membranous system as shown in figure 11 is assembled, in advance
One piece of magneton is respectively first added in two glass apparatus, vacuum silicon grease is wiped on the interface that two glass apparatus are connected, it will be upper
The centre that the PVDF filter membranes that ionic liquid impregnated are positioned over two glass apparatus is stated, cements and is clamped with iron clamp, both sides point
Above-mentioned cerous nitrate aqueous solution and phosphoric acid solution are not injected, and system is placed on magnetic stirring apparatus, maintains 1000rpm/min's
Rotating speed.It after reacting half an hour, centrifuges, obtains white precipitate, washed three times with deionized water and absolute ethyl alcohol respectively, it will
Product disperses in ethanol, supernatant liquor to be taken to be dispersed on masking foil in 70 DEG C of drying.SEM phenograms are visible (see Fig. 3) to be made
Cerous phosphate be nanometer tufted (flower-shaped)；XRD characterization figure shows that obtained nanometer cerous phosphate is hexagonal phase (see Fig. 4).
Embodiment 3
With ionic liquid [Bmim] [Tf2N] impregnate PVDF dewatering microporous films (0.45 μm thick, diameter 47mm) 2 hours, it obtains
Ionic liquid liquid phase support membrane.
Weigh the cerous nitrate [Ce (NO of certain mass3)3·6H2O] it is dissolved in 55ml deionized waters, it is configured to 2000ppm's
Cerous nitrate aqueous solution is used in combination nitric acid tune pH value to 3, obtains rare earth ion supply phase.The concentrated phosphoric acid for taking certain volume, is diluted with water
At the phosphoric acid solution 55ml of 2mol/l, phosphate anion supply phase is obtained.Liquid phase support membranous system as shown in figure 11 is assembled, in advance
One piece of magneton is respectively first added in two glass apparatus, vacuum silicon grease is wiped on the interface that two glass apparatus are connected, it will be upper
The centre that ionic liquid liquid phase support membrane is positioned over two glass apparatus is stated, cements and is clamped with iron clamp, both sides are injected separately into
The cerous nitrate aqueous solution and phosphoric acid solution stated, system is placed on magnetic stirring apparatus, maintains the rotating speed of 1000rpm/min.Instead
It after answering half an hour, centrifuges, obtains white precipitate, washed three times with deionized water and absolute ethyl alcohol respectively, by product point
It dissipates in ethanol, supernatant liquor is taken to be dispersed on masking foil in 70 DEG C of drying.SEM phenograms visible nanometer obtained (see Fig. 5)
Cerous phosphate is that flat porous is membranaceous (with the feature structure with whisker interpenetrating networks)；XRD characterization figure shows made (see Fig. 6)
The nanometer cerous phosphate obtained is hexagonal phase.
Embodiment 4
With ionic liquid [Bmim] [Tf2N] impregnate PVDF dewatering microporous films (0.45 μm thick, diameter 47mm) 2 hours, it obtains
Ionic liquid liquid phase support membrane.
Weigh the cerous nitrate [Ce (NO of certain mass3)3·6H2O] it is dissolved in 55ml deionized waters, it is configured to 2000ppm's
Cerous nitrate aqueous solution is used in combination nitric acid tune pH value to 4, obtains rare earth ion supply phase.The concentrated phosphoric acid for taking certain volume, is diluted with water
At the phosphoric acid solution 55ml of 2mol/l, phosphate anion supply phase is obtained.Liquid phase support membranous system as shown in figure 11 is assembled, in advance
One piece of magneton is respectively first added in two glass apparatus, vacuum silicon grease is wiped on the interface that two glass apparatus are connected, it will be upper
The centre that ionic liquid liquid phase support membrane is positioned over two glass apparatus is stated, cements and is clamped with iron clamp, both sides are injected separately into nitre
Sour cerium aqueous solution and phosphoric acid solution, system is placed on magnetic stirring apparatus, maintains the rotating speed of 1000rpm/min.Half of reaction
After hour, centrifuges, obtain white precipitate, washed three times with deionized water and absolute ethyl alcohol respectively, product is dispersed in second
In alcohol, supernatant liquor is taken to be dispersed on masking foil in 70 DEG C of drying.SEM phenograms visible nanometer cerous phosphate obtained (see Fig. 7)
It is membranaceous (with the feature structure with whisker interpenetrating networks) for flat porous；XRD characterization figure shows obtained receive (see Fig. 8)
Rice cerous phosphate is hexagonal phase.
Embodiment 5
With ionic liquid [Bmim] [Tf2N] impregnate PVDF dewatering microporous films (0.45 μm thick, diameter 47mm) 2 hours, it obtains
Ionic liquid liquid phase support membrane.
Weigh the cerous nitrate [Ce (NO of certain mass3)3·6H2O] it is dissolved in 55ml deionized waters, it is configured to 2000ppm's
Cerous nitrate aqueous solution, and the ammonium sulfate of certain mass is added thereto, a concentration of 0.1mol/L obtains rare earth ion supply phase.
The concentrated phosphoric acid for taking certain volume is diluted with water into the phosphoric acid solution 55ml of 2mol/l, obtains phosphate anion supply phase.Assembling is such as
Liquid phase shown in Figure 11 supports membranous system, one piece of magneton is respectively added in two glass apparatus in advance, in two glass apparatus phases
Vacuum silicon grease is wiped on the interface of connection, above-mentioned ionic liquid liquid phase support membrane is positioned over to the centre of two glass apparatus, is cemented
It is used in combination iron clamp to clamp, both sides are injected separately into cerous nitrate aqueous solution and phosphoric acid solution, and system is placed on magnetic stirring apparatus, maintain
The rotating speed of 1000rpm/min.It after reacting half an hour, centrifuges, obtains white precipitate, use deionized water and anhydrous respectively
Ethyl alcohol is washed three times, in ethanol by product dispersion, supernatant liquor is taken to be dispersed on masking foil in 70 DEG C of drying.SEM phenograms (see
Fig. 9) visible cerous phosphate obtained is that nanometer is spherical；XRD characterization figure shows that obtained nanometer cerous phosphate is six sides (see Figure 10)
Crystalline phase.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to the above embodiments.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the present invention
Within the scope of shield.
Claims (26)
1. a kind of preparing phosphorylation rare earth nano using ionic liquid liquid phase support membranous system separation-nanosizing reaction coupling linkage
The method of material, which is characterized in that described method includes following steps：
1) porous membrane material is impregnated with ionic liquid, to obtain required ionic liquid liquid phase support membrane；
2) prepare rare earth ion supply respectively mutually and phosphate anion supplies phase；
3) assembling ionic liquid liquid phase supports membranous system comprising is located at rare earth ion made from the step 2) of carrying respectively of both sides
Supply is mutually and phosphate anion supplies ionic liquid liquid phase branch made from the container of phase and the step 1) between two containers
Support film；Rare earth ion supply made from above-mentioned step 2) is mutually mutually injected separately into above-mentioned container with phosphate anion supply
In；The container of the both sides is communicated by the ionic liquid liquid phase support membrane between container；
4) two containers are stirred respectively, and are reacted and obtained the phosphorylation rare earth nano material.
2. according to the method described in claim 1, it is characterized in that, the ionic liquid in step 1) is selected from imidazoles system ionic liquid
Body.
3. according to the method described in claim 2, it is characterized in that, imidazoles system ionic liquid is [Cnmim] [Tf2N],
[Cnmim][PF6] or [Cnmim] [BF4], n=2-16.
4. according to the method described in claim 3, it is characterized in that, n=4-10.
5. according to the method described in claim 2, it is characterized in that, imidazoles system ionic liquid is [Bmim] [Tf2N]、
[Omim][Tf2N]、[Bmim][PF6] or [Bmim] [BF4]。
6. according to the method described in claim 1, it is characterized in that, porous membrane material in step 1) be HVHP dewatering microporous films,
PVDF dewatering microporous films or nucleopore membranes.
7. according to the method described in claim 1, it is characterized in that, the aperture of the porous membrane material is 200-500nm.
8. according to the method described in claim 1, it is characterized in that, in step 1), per 10cm2Porous membrane material use 100 μ l with
On ionic liquid impregnate.
9. according to the method described in claim 8, it is characterized in that, the time of the immersion is 0.1-24 hours.
10. according to the method described in claim 9, it is characterized in that, the time of the immersion is 1-10 hours.
11. according to the method described in claim 1, it is characterized in that, in step 2), rare earth ion supply is mutually containing rare earth ion
Solution；A concentration of 20ppm-10000ppm of its Rare Earth Ion.
12. according to the method for claim 11, which is characterized in that the rare earth ion supply is mutually the water containing rare earth ion
Solution.
13. according to the method described in claim 1, it is characterized in that, in step 2), phosphate anion supply is mutually phosphorous acid group
The solution of ion；The wherein a concentration of 0.1M-5M of phosphate anion.
14. according to the method described in claim 1, it is characterized in that, in step 3), after injection rare earth ion supply phase, also wrap
The step of including the pH for adjusting rare earth ion supply phase, and/or, other anionic radicals are added to control in rare earth ion supplies phase
The pattern of nano material.
15. according to the method for claim 14, which is characterized in that it is 1~6 to adjust pH.
16. according to the method described in claim 1, it is characterized in that, in step 4), in two containers magnetic force is placed respectively and stirred
Son is mixed, is reacted under magnetic agitation, the phosphorylation rare earth nano material is obtained.
17. according to the method for claim 16, which is characterized in that in step 4), be stirred to react under room temperature, normal pressure into
Row, reaction time are 1~30min.
18. according to the method for claim 14, which is characterized in that the phosphorylation rare earth nano material includes the long stick of nanometer
Shape phosphorylation rare earth nano material, nanometer tufted phosphorylation rare earth nano material, the membranaceous phosphorylation rare earth nano material of flat porous
Material or the spherical phosphorylation rare earth nano material of nanometer.
19. according to the method for claim 18, which is characterized in that the membranaceous phosphorylation rare earth nano material of flat porous
Feature structure with whisker interpenetrating networks.
20. according to claim 1-19 any one of them methods, which is characterized in that above-mentioned preparation method is equally applicable to other
The preparation of the phosphate nano material of metal ion.
21. a kind of phosphorylation nano material, which is characterized in that the material is by any one of claim 1-20 the method systems
；
The phosphorylation nano material is phosphorylation rare earth nano material；
The phosphorylation rare earth nano material includes that nanometer tufted phosphorylation rare earth nano material, the membranaceous phosphorylation of flat porous are dilute
Native nano material or the spherical phosphorylation rare earth nano material of nanometer.
22. phosphorylation nano material according to claim 21, which is characterized in that the membranaceous phosphorylation of flat porous is dilute
Native nano material has the feature structure of whisker interpenetrating networks.
23. the purposes of the phosphorylation nano material described in claim 21, which is characterized in that the phosphorylation nano material is tool
There is the membranaceous phosphorylation rare earth nano material of the flat porous of the feature structure of whisker interpenetrating networks, the material outside nuclear power for arranging
The filtering and absorption of aerogel substance are harmful in waste water in the filtering of high radioactivity human nuclide and atmosphere.
24. purposes according to claim 23, which is characterized in that harmful aerogel substance is PM2.5 and radiation
Property dust.
25. the purposes of the phosphorylation nano material described in claim 21, which is characterized in that the phosphorylation nano material is tool
There are the spherical phosphorylation rare earth nano material of the nanometer of high-specific surface area, carrier and drug conveying of the material for catalyst to carry
Body.
26. the purposes of the phosphorylation nano material described in claim 21, which is characterized in that the material is added as function
Agent, by itself and organic/inorganic materials consolute, to which the fire resistance, wearability and acid and alkali-resistance that improve the organic/inorganic materials are rotten
Corrosion.
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| CN1456714A (en) * | 2003-05-22 | 2003-11-19 | 北京大学 | Method for preparing phosphoric acid rare earth monocrystalline nano-thread |
| CN101704543A (en) * | 2009-11-25 | 2010-05-12 | 深圳大学 | Method for preparing cerous phosphate nano wire |
| CN102849706A (en) * | 2012-08-29 | 2013-01-02 | 深圳大学 | Preparation method of cerium phosphate nano-wires |
| CN105347422A (en) * | 2015-11-16 | 2016-02-24 | 西安建筑科技大学 | Method for removing cyanide in cyanogen-containing waste water by ionic liquid supported liquid membrane technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456714A (en) * | 2003-05-22 | 2003-11-19 | 北京大学 | Method for preparing phosphoric acid rare earth monocrystalline nano-thread |
| CN101704543A (en) * | 2009-11-25 | 2010-05-12 | 深圳大学 | Method for preparing cerous phosphate nano wire |
| CN102849706A (en) * | 2012-08-29 | 2013-01-02 | 深圳大学 | Preparation method of cerium phosphate nano-wires |
| CN105347422A (en) * | 2015-11-16 | 2016-02-24 | 西安建筑科技大学 | Method for removing cyanide in cyanogen-containing waste water by ionic liquid supported liquid membrane technology |
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