CN119160938B - A preparation method and application of antimony trioxide - Google Patents
A preparation method and application of antimony trioxide Download PDFInfo
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- CN119160938B CN119160938B CN202411635028.2A CN202411635028A CN119160938B CN 119160938 B CN119160938 B CN 119160938B CN 202411635028 A CN202411635028 A CN 202411635028A CN 119160938 B CN119160938 B CN 119160938B
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- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000839 emulsion Substances 0.000 claims abstract description 17
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 11
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 239000004519 grease Substances 0.000 claims abstract description 4
- 239000012071 phase Substances 0.000 claims description 35
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- 229920005862 polyol Polymers 0.000 claims description 14
- 150000003077 polyols Chemical class 0.000 claims description 14
- 239000008346 aqueous phase Substances 0.000 claims description 11
- WSXIMVDZMNWNRF-UHFFFAOYSA-N antimony;ethane-1,2-diol Chemical group [Sb].OCCO WSXIMVDZMNWNRF-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical group C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 7
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 7
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 238000009775 high-speed stirring Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 2
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 2
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 2
- 229920001983 poloxamer Polymers 0.000 claims description 2
- 229960000502 poloxamer Drugs 0.000 claims description 2
- 235000011067 sorbitan monolaureate Nutrition 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 10
- 238000005406 washing Methods 0.000 abstract description 7
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 150000005846 sugar alcohols Polymers 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 5
- 235000019799 monosodium phosphate Nutrition 0.000 description 5
- 229920001992 poloxamer 407 Polymers 0.000 description 5
- 229940044476 poloxamer 407 Drugs 0.000 description 5
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
- C01G30/005—Oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the field of inorganic materials, in particular to a preparation method and application of antimonous oxide, which comprises the steps of adding an antimonous oxide precursor and a polyalcohol phase into an oil phase containing a first emulsifying agent and grease, stirring at a high speed to obtain a P/O emulsion, adding the P/O emulsion into a water phase containing a second emulsifying agent and water, stirring at a high speed for 1-30s, stirring at a low speed for reacting for 30-90min, standing, centrifuging, collecting precipitate, washing and drying.
Description
Technical Field
The invention relates to the field of inorganic materials, in particular to a preparation method and application of antimonous oxide.
Background
Antimony trioxide is a traditional chemical raw material, is often used as a white pigment in paint, plastics and synthetic rubber, has unique physical and chemical properties, has a better flame retardant effect, has long-term use as a flame retardant, has higher theoretical capacity as a transition metal oxide, is low in price, rich in reserves and stable in cycle performance, and can be used as an electrode material of a new energy battery and a pseudocapacitor.
At present, the preparation method of the antimonous oxide generally comprises an alcoholysis method, a chemical reduction method, a micro-sol method, a hydrothermal method and the like, and although the prior literature discloses a technical scheme of using an emulsifier TX-50 in the process of preparing the antimonous oxide by the hydrothermal method, no report exists on preparing the nano-micron-level antimonous oxide by the micro-emulsion method.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method and application of antimony trioxide.
The technical scheme adopted is as follows:
A preparation method of antimony trioxide comprises the following steps:
adding an organic antimony precursor and a polyol phase into an oil phase containing a first emulsifier and grease, stirring at a high speed to obtain a P/O emulsion (alcohol-in-oil emulsion), adding the P/O emulsion into an aqueous phase containing a second emulsifier and water, stirring at a high speed for 1-30s, stirring at a low speed for reaction for 30-90min, standing, centrifuging, collecting precipitate, washing and drying.
Further, the organic antimony precursor is ethylene glycol antimony.
Further, the polyol phase is a combination of dipropylene glycol and ethylene glycol in a mass ratio of 1-4:1-4.
Further, the first emulsifier is any one or a combination of more than one of span-20, span-40, span-60 and span-80.
Further, the grease is white oil.
Further, the second emulsifier is a poloxamer.
Further, the pH of the aqueous phase is 3-6.
Further, the aqueous phase is pH adjusted by adding phosphate.
Further, the rotating speed during high-speed stirring is more than or equal to 5000r/min, and the rotating speed during low-speed stirring is less than or equal to 50r/min.
The invention also provides an application of the antimony trioxide prepared by the method in the super capacitor.
The invention has the beneficial effects that:
The application provides a preparation method of antimony trioxide, which utilizes the characteristic that ethylene glycol antimony is dissolved in ethylene glycol and insoluble in white oil, isolates ethylene glycol antimony from weak acid water phase by utilizing oil phase, avoids abnormal enlargement and agglomeration of generated antimony trioxide particles caused by rapid occurrence of hydrolysis reaction, and controls the size of generated antimony trioxide by entering a polyhydric alcohol phase to carry out hydrolysis reaction with ethylene glycol antimony under the action of shearing force in the low-speed stirring reaction process, wherein phosphate is added into the water phase, pH value is regulated, emulsified particles can be mutually repelled after electrification, and the stability of a system is improved.
Drawings
FIG. 1 is an SEM image of antimony trioxide prepared in example 1.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Example 1:
A preparation method of antimony trioxide comprises the following steps:
mixing 2g of dipropylene glycol and 3g of ethylene glycol to obtain a polyol phase;
Adding 0.2g span-80 into 20g white oil and uniformly mixing to obtain an oil phase;
Adding 1g of ethylene glycol antimony into a polyol phase, stirring to dissolve, adding into the oil phase, and stirring at a rotating speed of 10000r/min for 5min to obtain a P/O emulsion;
Adding 2g of poloxamer 407 into 200ml of deionized water, uniformly mixing, and adding sodium dihydrogen phosphate to adjust the pH of the system to 5 to obtain a water phase;
Adding the P/O emulsion into an aqueous phase, stirring at a high speed of 10000r/min for 30s, stirring at a low speed of 50r/min for reaction for 60min, standing for 24h, centrifuging, collecting precipitate, repeatedly washing the product with deionized water and ethanol, and drying to obtain the antimonous oxide with the purity of more than or equal to 99.99%.
The surface morphology of the porous micro-nano particles is tested by adopting a ZEISS (EVO MA 15) scanning electron microscope, the scanning voltage is 20kV, and the porous micro-nano particles are observed to be micro-nano particles with a porous structure, and the specific reference is shown in figure 1;
Mixing antimony trioxide and acetylene black prepared in the embodiment according to the mass ratio of 7:2, fully grinding to obtain a mixture 1, adding polyvinylidene fluoride (the mass of which is 0.5 times of that of the acetylene black) into a proper amount (about 0.5 mL) of N-methylpyrrolidone, fully grinding to obtain a mixture 2, adding the mixture 1 into the mixture 2, fully grinding, smearing the mixture on a foam nickel wafer which is cut in advance, firstly drying 12 h in a blast drying box at 60 ℃, and then immediately transferring the mixture into a vacuum drying box, and drying 12 h at 60 ℃ to serve as a working electrode of a three-electrode system for standby;
The electrochemical performance test is carried out by using an electrochemical workstation, a three-electrode system is adopted, wherein a counter electrode and a reference electrode are respectively selected from platinum sheets and mercury/mercury oxide, a KOH solution with the concentration of 2mol/L is adopted as an electrolyte, cyclic voltammetry and constant current charge-discharge tests are carried out, the voltage window is 0-0.5V, the specific capacity reaches 526F/g under the current density of 2A/g, the multiplying power performance is good, and the capacity retention rate is 95.4% after 2000 cycles under the current density of 2A/g.
Example 2:
A preparation method of antimony trioxide comprises the following steps:
Mixing 1g of dipropylene glycol and 4g of ethylene glycol to obtain a polyol phase;
Adding 0.2g span-80 into 20g white oil and uniformly mixing to obtain an oil phase;
Adding 1g of ethylene glycol antimony into a polyol phase, stirring to dissolve, adding into the oil phase, and stirring at a rotating speed of 10000r/min for 5min to obtain a P/O emulsion;
Adding 2g of poloxamer 407 into 200ml of deionized water, uniformly mixing, and adding sodium dihydrogen phosphate to adjust the pH of the system to 5 to obtain a water phase;
Adding the P/O emulsion into an aqueous phase, stirring at a high speed of 10000r/min for 30s, stirring at a low speed of 50r/min for reaction for 60min, standing for 24h, centrifuging, collecting precipitate, repeatedly washing the product with deionized water and ethanol, and drying to obtain the antimonous oxide with the purity of more than or equal to 99.99%.
The surface morphology of the material is tested by adopting a ZEISS (EVO MA 15) scanning electron microscope, the scanning voltage is 20kV, and the material is observed to be micro-nano particles with porous structures;
The electrochemical performance of the antimony trioxide prepared in this example was tested in the manner of example 1, and the specific capacity reached 505F/g at a current density of 2A/g, indicating that the rate performance was good, and the capacity retention was 94.1% after 2000 cycles at a current density of 2A/g.
Example 3:
A preparation method of antimony trioxide comprises the following steps:
Mixing 2.5g dipropylene glycol and 2.5g ethylene glycol to obtain a polyol phase;
Adding 0.2g span-80 into 20g white oil and uniformly mixing to obtain an oil phase;
Adding 1g of ethylene glycol antimony into a polyol phase, stirring to dissolve, adding into the oil phase, and stirring at a rotating speed of 10000r/min for 5min to obtain a P/O emulsion;
Adding 2g of poloxamer 407 into 200ml of deionized water, uniformly mixing, and adding sodium dihydrogen phosphate to adjust the pH of the system to 5 to obtain a water phase;
Adding the P/O emulsion into an aqueous phase, stirring at a high speed of 10000r/min for 30s, stirring at a low speed of 50r/min for reaction for 60min, standing for 24h, centrifuging, collecting precipitate, repeatedly washing the product with deionized water and ethanol, and drying to obtain the antimonous oxide with the purity of more than or equal to 99.99%.
The surface morphology of the material is tested by adopting a ZEISS (EVO MA 15) scanning electron microscope, the scanning voltage is 20kV, and the material is observed to be micro-nano particles with porous structures;
The electrochemical performance of the antimony trioxide prepared in this example was tested in the manner of example 1, and the specific capacity reached 521F/g at a current density of 2A/g, indicating that the rate performance was good, and the capacity retention was 94.9% after 2000 cycles at a current density of 2A/g.
Example 4:
A preparation method of antimony trioxide comprises the following steps:
3g of dipropylene glycol and 2g of ethylene glycol are mixed to obtain a polyol phase;
Adding 0.2g span-80 into 20g white oil and uniformly mixing to obtain an oil phase;
Adding 1g of ethylene glycol antimony into a polyol phase, stirring to dissolve, adding into the oil phase, and stirring at a rotating speed of 10000r/min for 5min to obtain a P/O emulsion;
Adding 2g of poloxamer 407 into 200ml of deionized water, uniformly mixing, and adding sodium dihydrogen phosphate to adjust the pH of the system to 5 to obtain a water phase;
Adding the P/O emulsion into an aqueous phase, stirring at a high speed of 10000r/min for 30s, stirring at a low speed of 50r/min for reaction for 60min, standing for 24h, centrifuging, collecting precipitate, repeatedly washing the product with deionized water and ethanol, and drying to obtain the antimonous oxide with the purity of more than or equal to 99.99%.
The surface morphology of the material is tested by adopting a ZEISS (EVO MA 15) scanning electron microscope, the scanning voltage is 20kV, and the material is observed to be micro-nano particles with porous structures;
The electrochemical performance of the antimony trioxide prepared in this example was tested in the manner of example 1, and the specific capacity reached 518F/g at a current density of 2A/g, indicating that the rate performance was good, and the capacity retention was 94.3% after 2000 cycles at a current density of 2A/g.
Example 5:
A preparation method of antimony trioxide comprises the following steps:
mixing 4g of dipropylene glycol and 1g of ethylene glycol to obtain a polyol phase;
Adding 0.2g span-80 into 20g white oil and uniformly mixing to obtain an oil phase;
Adding 1g of ethylene glycol antimony into a polyol phase, stirring to dissolve, adding into the oil phase, and stirring at a rotating speed of 10000r/min for 5min to obtain a P/O emulsion;
Adding 2g of poloxamer 407 into 200ml of deionized water, uniformly mixing, and adding sodium dihydrogen phosphate to adjust the pH of the system to 5 to obtain a water phase;
Adding the P/O emulsion into an aqueous phase, stirring at a high speed of 10000r/min for 30s, stirring at a low speed of 50r/min for reaction for 60min, standing for 24h, centrifuging, collecting precipitate, repeatedly washing the product with deionized water and ethanol, and drying to obtain the antimonous oxide with the purity of more than or equal to 99.99%.
The surface morphology of the material is tested by adopting a ZEISS (EVO MA 15) scanning electron microscope, the scanning voltage is 20kV, and the material is observed to be micro-nano particles with porous structures;
The electrochemical performance of the antimony trioxide prepared in this example was tested by the method of example 1, and the specific capacity reached 497F/g at a current density of 2A/g, indicating that the rate performance was good, and the capacity retention was 93.6% after 2000 cycles at a current density of 2A/g.
Comparative example:
commercial antimony trioxide (purity: 99.99% or more, particle size: 1 μm, hebei Ruihuang metal materials Co., ltd.) was used as a sample;
The electrochemical performance of the antimony trioxide prepared in this example was tested in the manner of example 1, with a specific capacity of 419F/g at a current density of 2A/g and a capacity retention of 77.6% after 2000 cycles at a current density of 2A/g.
Characterization of properties:
Taking the antimonous oxide prepared in the embodiments 1-5 of the invention as a sample, dispersing the sample by adopting a circulating dispersion sample injection system, carrying out particle size test on the sample by using a laser particle size distribution instrument, and measuring the change of the particle size of the antimonous oxide by adopting equivalent particle sizes (D10, D50 and D90), wherein D50 refers to a particle size value corresponding to a cumulative distribution percentage of 50%, namely median diameter, wherein particles with the particle size greater than the median diameter account for 50% of the whole sample, and particles with the particle size less than the median diameter account for 50%, and the meanings of D10 and D90 are the same, and the results are shown in the following table 1:
;
as can be seen from Table 1 above, the antimony trioxide prepared by the method of the present invention has a size of micro-nano scale.
The foregoing embodiments are merely for illustrating the technical solution of the present invention, but not for limiting the same, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that modifications may be made to the technical solution described in the foregoing embodiments or equivalents may be substituted for parts of the technical features thereof, and that such modifications or substitutions do not depart from the spirit and scope of the technical solution of the embodiments of the present invention in essence.
Claims (3)
Priority Applications (1)
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| CN102925271A (en) * | 2012-10-19 | 2013-02-13 | 宋小林 | Multiple-effect type semi-synthetic micro-emulsion cutting solution |
| CN114099357A (en) * | 2021-11-30 | 2022-03-01 | 江苏瑞霆生物科技有限公司 | Hydroxytyrosol-containing polyol-in-oil nano emulsion, and preparation method and application thereof |
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| CN116111068A (en) * | 2023-02-24 | 2023-05-12 | 辽宁大学 | Zinc cathode material modified by three-dimensional antimony/antimony oxide composite layer and preparation method and application thereof |
| CN116282150B (en) * | 2023-04-14 | 2024-07-30 | 贵州华星冶金有限公司 | Preparation method of hollow antimonous oxide |
| CN118062890B (en) * | 2024-02-19 | 2024-10-29 | 湖南娄底华星锑业有限公司 | Preparation method of nano antimony trioxide |
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| CN102925271A (en) * | 2012-10-19 | 2013-02-13 | 宋小林 | Multiple-effect type semi-synthetic micro-emulsion cutting solution |
| CN114099357A (en) * | 2021-11-30 | 2022-03-01 | 江苏瑞霆生物科技有限公司 | Hydroxytyrosol-containing polyol-in-oil nano emulsion, and preparation method and application thereof |
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