CN106674532A - Synthetic method of AyB1-y[Co(CN)6]0.67PBA and AxB1.8-xCo1.2O4 - Google Patents
Synthetic method of AyB1-y[Co(CN)6]0.67PBA and AxB1.8-xCo1.2O4 Download PDFInfo
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- 238000010189 synthetic method Methods 0.000 title claims description 5
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 10
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 8
- 150000003624 transition metals Chemical class 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract 9
- 239000006104 solid solution Substances 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000002077 nanosphere Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- YPSXFMHXRZAGTG-UHFFFAOYSA-N 4-methoxy-2-[2-(5-methoxy-2-nitrosophenyl)ethyl]-1-nitrosobenzene Chemical compound COC1=CC=C(N=O)C(CCC=2C(=CC=C(OC)C=2)N=O)=C1 YPSXFMHXRZAGTG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000006193 liquid solution Substances 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 claims 1
- 230000001052 transient effect Effects 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 239000013256 coordination polymer Substances 0.000 abstract description 3
- 229920001795 coordination polymer Polymers 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229920001485 poly(butyl acrylate) polymer Polymers 0.000 description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000011572 manganese Substances 0.000 description 14
- 238000002156 mixing Methods 0.000 description 6
- 239000012621 metal-organic framework Substances 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 230000032683 aging Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical class [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229960003351 prussian blue Drugs 0.000 description 1
- 239000013225 prussian blue Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical class [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- 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
- C01P2004/30—Particle morphology extending in three dimensions
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention provides a ''copolymer-eutectic morphology'' strategy for accurately regulating and controlling the morphology of an AyB1-y[Co(CN)6]0.67PBA metal organic coordination polymer. In a PVP solution, by preparing a solid solution of two hexacyano-cobaltates (A-Co and B-CoPBA), AyB1-y[Co(CN)6]0.67PBA with a specific morphology can be prepared. In addition, through simple heat treatment, a doped porous transition metal oxide AxB1.8-xCo1.2O4 with a specific morphology can be synthesized. By the morphology controllable synthesis strategy and through simple conversion of a transition metal precursor, MnyFe1-y[Co(CN)6]0.67 and ZnyFe1-y[Co(CN)6]0.67PBA with specific morphology can be easily synthesized. In comparison with other methods in literature, the morphology synthesis strategy has the characteristic of accurate regulation and control of nano-materials' morphology and composition and has strong expansibility.
Description
Technical field
The present invention relates to the use of a kind of morphology controllable mixed type metal organic coordination polymer (AyB1-y[Co(CN)6]0.67PBA method), meanwhile, simple heat treatment, the copolymer can readily be changed into the doping type Porous transition metal oxides (A with specific morphologyxB1.8-xCo1.2O4)。
Background technology
In recent years, metal organic coordination polymer (MOFs) and doping type transition metal oxide (MTMOs) have a wide range of applications in fields such as battery electrode reaction, photocatalysis, Fenton's reaction, magnetic materials.It is well known that the pattern of nano material, composition and specific surface area have a very big impact to the physical and chemical performance of material.Therefore, the morphology controllable of nano material becomes the focus of Recent study functionalization research.Traditional morphology controllable prepares the method for MOFs and MTMOs also to be had a lot, including sol-gal process, coprecipitation and hydro-thermal method etc..But be often subject to that morphology controllable is strong, preparation process is complicated and can the low shortcoming of expanding type restriction, in addition, MOFs the and MTMOs specific surface areas for preparing are generally relatively low.Therefore, the method for preparation process is simple, expansibility is strong morphology controllable synthesis remains unchanged urgent by people's demand.
The Prussian blue similar thing (A-Co PBAs) of cobalt-based is the very abundant metal organic framework compound (MOFs) of the Nomenclature Composition and Structure of Complexes change, and such compound is widely studied because itself having the various excellent physicochemical properties such as absorption, catalysis, photic magnetic.Doping can generally change the pattern of material, therefore, by the transition metal B for adulterating new in A-Co PBAs, then may realize AyB1-y[Co(CN)6]0.67(it is abbreviated as:AyB1-y- Co) PBA copolymers morphology controllable synthesis.Importantly, the A by calcining such doping typeyB1-y- Co PBA copolymers, can be transformed into the Porous transition metal oxides (A with specific morphologyxB1.8-xCo1.2O4).That is, by the strategy of " copolymer-conformal looks ", while realizing AyB1-y- Co PBA and AxB1.8-xCo1.2O4Morphology controllable synthesis.And pass through the A that the synthesis strategy is preparedyB1-y- Co PBA and AxB1.8-xCo1.2O4, also will have great significance in various research fields.
The content of the invention
It is contemplated that a kind of new morphology controllable synthesis strategy of exploitation prepares (AyB1-y- Co PBA), and use it for morphology controllable synthesizing doped type transition metal oxide (AxB1.8-xCo1.2O4)。
A kind of morphology controllable synthesizes AyB1-yThe method of-Co PBA, it is concretely comprised the following steps:
1) by K4[Co(CN)6] settled solution X is made into, its concentration c is 0<c<10mmol/L;
2) by the ACl of required proportioning2And BCl2 、Or A (NO3)2With B (NO3)2It is made into settled solution Y;Wherein transition metal ions A and B molar concentrations sum are K4[Co(CN)6] 1-2 times of solution concentration;A, B are respectively transition metal Zn, Co, Fe, Mn, Ti, Ni, the one kind in Cu, and A and B is differed;
3) to step 2) PVP surfactants, the final concentration of 10-50g/L of its PVP are added in resulting solution;
4) by step 1) resulting solution X adds step 3) resulting solution, solution X and step 3) volume ratio of resulting solution is 1/1, continues to stir 10-60min afterwards;Afterwards centrifuge washing is dried;Generate the A with specific morphologyyB1-y[Co(CN)6]0.67PBA, 0<y<1.
A kind of Porous transition metal oxides AxB1.8-xCo1.2O4(0<x<1.8) synthetic method;It is characterized in that:
Its preparation process is as follows:
By the A described in the claims 1yB1-y[Co(CN)6]0.67PBA is calcined, you can obtain the Porous transition metal oxides A with specific morphologyxB1.8-xCo1.2O4, 0<x<1.8;Its calcining heat is 300-1000 degree.
The invention has the advantages that:
1), by modulation A, the doping ratio of two kinds of transition metal of B can be with accuracy controlling A for the pattern synthesis strategyyB1-y- Co PBA copolymer patterns.
2) synthesis strategy has very strong expansibility, by simple transformation different transition metal A, B, can be easy to prepare the Mn of different-shapeyFe1-y-Co,ZnyFe1-y-Co。
3) A for preparingyB1-y- Co PBA can be changed into the porous doping type transition metal oxide (A with specific morphology through simple thermal treatmentxB1.8-xCo1.2O4)。
4) preparation method is simple.
Description of the drawings
Fig. 1 is to prepare Zn in embodiment 10.5Fe0.5SEM (ESEM) photo of-Co PBA.It can be seen that uniform Zn can be prepared by the strategy0.5Fe0.5- Co PBA nanospheres (500-1000nm).
Fig. 2 is the Mn prepared in embodiment 20.2Fe0.8SEM (ESEM) photo of-Co PBA.It can be seen that uniform Mn can be prepared by the strategy0.2Fe0.8- Co PBA nanometer dices (similar to the pattern of dice, the size in its dice face is 500-1000nm).
Fig. 3 is the Mn prepared in embodiment 30.8Fe0.2SEM (ESEM) photo of-Co PBA.It can be seen that uniform Mn can be prepared by the strategy0.8Fe0.2- Co PBA nanometer dices.In addition, contrast Fig. 3 can be found that this by modulation Mn, the content of Fe can be with the pattern (similar to the pattern of dice, the size in its dice face is 1000-1500nm) of accuracy controlling PBA copolymer.
The Mn that Fig. 4 embodiments 4 are prepared1.4Fe0.4Co1.2O4(ESEM) photo, it can be seen that the doping type transition metal oxide for obtaining, perfectly inherit corresponding presoma Mn0.8Fe0.2The pattern of-Co PBA.Thus the Mn with specific morphology is prepared1.4Fe0.4Co1.2O4Nanometer dice (similar to the pattern of dice, the size in its dice face is 1000-1500nm).
Specific embodiment
Embodiment 1
By 0.0332g K4[Fe(CN)6] be dissolved in 10ml deionized waters and be uniformly mixing to obtain solution A, 0.027g zinc nitrates and the mixing of 0.018g iron chloride are dissolved in into 10ml deionized water obtained solution B, 0.6g PVP are added in solution B and is stirred.Solution A is slowly dropped in B and continues to stir 30min, aging 20h.Afterwards centrifuge washing is dried to obtain Zn0.5Fe0.5- Co PBA nanospheres.
Embodiment 2
By 0.0332g K4[Fe(CN)6] be dissolved in 10ml deionized waters and be uniformly mixing to obtain solution A, 0.025g manganese nitrates and the mixing of 0.057g iron chloride are dissolved in into 10ml deionized water obtained solution B, 0.6g PVP are added in solution B and is stirred.Solution A is slowly dropped in B and continues to stir 30min, aging 20h.Afterwards centrifuge washing is dried to obtain Mn0.2Co0.8- Co PBA nanometer dices.
Embodiment 3
By 0.0332g K4[Fe(CN)6] be dissolved in 10ml deionized waters and be uniformly mixing to obtain solution A, 0.101g manganese nitrates and the mixing of 0.014g iron chloride are dissolved in into 10ml deionized water obtained solution B, 0.6g PVP are added in solution B and is stirred.Solution A is slowly dropped in B and continues to stir 30min, aging 20h.Afterwards centrifuge washing is dried to obtain Mn0.8Co0.2- Co PBA nanometer dices.
Embodiment 4
By Mn obtained above0.8Co0.2- Co PBA nanometers dices can obtain the Porous transition metal doping oxide Mn with identical pattern as 500 degree of calcinings of presoma1.4Fe0.4Co1.2O4Nanometer dice.
The above; one of specific embodiment only of the invention, but protection scope of the present invention do not limit to and this, any those of ordinary skill in the art disclosed herein technical scope in; without the variation and replacement of inventive concept, all should be encompassed within protection domain.Therefore, the protection domain that protection scope of the present invention should be limited by claims is defined.
Claims (3)
1. a kind of AyB1-y[Co(CN)6]0.67The synthetic method of PBA, it is characterised in that:
AyB1-y[Co(CN)6]0.67PBA is obtained by preparing A-Co and B-Co PBA solid solution liquid solutions;By modulation
The doping ratio of two kinds of transition metal of A, B, can be with accuracy controlling AyB1-y- Co PBA copolymer patterns (nanosphere or
Nanometer dice), 0<y<1, concrete preparation process is as follows:
1) by K4[Co(CN)6] settled solution X is made into, its concentration c is 0<c<10mmol/L;
2) by the ACl of required proportioning2And BCl2、Or A (NO3)2With B (NO3)2It is made into settled solution Y;Wherein cross
Metal ion A and B molar concentration sum is crossed for K4[Co(CN)6] 1-2 times of solution concentration;A, B are respectively transition
Metal Zn, Co, Fe, Mn, Ti, Ni, the one kind in Cu, and A and B are differed;
3) to step 2) PVP surfactants, the final concentration of 10-50g/L of its PVP are added in resulting solution;
4) by step 1) resulting solution X adds step 3) resulting solution, solution X and step 3) resulting solution body
Product continues to stir 10-60min than being 1/1, afterwards;Afterwards centrifuge washing is dried;Generate with specific morphology
AyB1-y[Co(CN)6]0.67PBA, 0<y<1.
2. a kind of AxB1.8-xCo1.2O4Synthetic method;It is characterized in that:
Its preparation process is as follows:
By the A described in the claims 1yB1-y[Co(CN)6]0.67PBA is calcined, you can obtained with specific morphology
Porous transition metal oxides AxB1.8-xCo1.2O4, 0<x<1.8;Its calcining heat is 300-1000 degree.
3. according to the synthetic method described in claim 2, it is characterised in that:
By the doping of different transient metal Mns and Fe or Zn and Fe, can synthesize with specific morphology
MnyFe1-yCo1.2O4,ZnyFe1-yCo1.2O4。
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108855159A (en) * | 2018-06-27 | 2018-11-23 | 广东工业大学 | A kind of phosphatization cobalt and its preparation method and application with the synthesis of Prussian blue derivative |
CN109942832A (en) * | 2019-04-18 | 2019-06-28 | 南京邮电大学 | Different-shape π-d is conjugated the preparation of Fe-HHTP metal organic frame and related electrode |
CN111943226A (en) * | 2020-08-30 | 2020-11-17 | 温州大学 | Method for regulating morphology of manganese cobalt Prussian blue crystals by using surfactant |
CN112479317A (en) * | 2020-12-01 | 2021-03-12 | 北京工业大学 | Preparation method and application of composite cathode integrating efficient in-situ hydrogen peroxide electrosynthesis and catalytic performance |
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CN102175728A (en) * | 2011-01-18 | 2011-09-07 | 兰州大学 | Method for preparing nanometer Co-Fe prussian-blue complex-carbon nano tube composite hydrogen peroxide sensor |
CN103441241A (en) * | 2013-04-12 | 2013-12-11 | 中国科学院化学研究所 | Preparation method and application of prussian blue complex/carbon composite material |
CN103768619A (en) * | 2012-10-25 | 2014-05-07 | 常州柯艾医药科技有限公司 | Bismuth-based prussian blue compound nano CT contrast agent and preparation method therefor |
CN104269527A (en) * | 2014-09-23 | 2015-01-07 | 浙江大学 | Preparation method and application of in-situ carbon-compounded prussian blue type compound thin film |
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2015
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CN102175728A (en) * | 2011-01-18 | 2011-09-07 | 兰州大学 | Method for preparing nanometer Co-Fe prussian-blue complex-carbon nano tube composite hydrogen peroxide sensor |
CN103768619A (en) * | 2012-10-25 | 2014-05-07 | 常州柯艾医药科技有限公司 | Bismuth-based prussian blue compound nano CT contrast agent and preparation method therefor |
CN103441241A (en) * | 2013-04-12 | 2013-12-11 | 中国科学院化学研究所 | Preparation method and application of prussian blue complex/carbon composite material |
CN104269527A (en) * | 2014-09-23 | 2015-01-07 | 浙江大学 | Preparation method and application of in-situ carbon-compounded prussian blue type compound thin film |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108855159A (en) * | 2018-06-27 | 2018-11-23 | 广东工业大学 | A kind of phosphatization cobalt and its preparation method and application with the synthesis of Prussian blue derivative |
CN109942832A (en) * | 2019-04-18 | 2019-06-28 | 南京邮电大学 | Different-shape π-d is conjugated the preparation of Fe-HHTP metal organic frame and related electrode |
CN109942832B (en) * | 2019-04-18 | 2021-04-20 | 南京邮电大学 | Preparation of pi-d conjugated Fe-HHTP metal organic framework with different shapes and related electrode |
CN111943226A (en) * | 2020-08-30 | 2020-11-17 | 温州大学 | Method for regulating morphology of manganese cobalt Prussian blue crystals by using surfactant |
CN111943226B (en) * | 2020-08-30 | 2023-08-11 | 温州大学 | Method for regulating and controlling morphology of manganese-cobalt Prussian blue crystal by using surfactant |
CN112479317A (en) * | 2020-12-01 | 2021-03-12 | 北京工业大学 | Preparation method and application of composite cathode integrating efficient in-situ hydrogen peroxide electrosynthesis and catalytic performance |
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