CN105731539A - Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system - Google Patents
Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system Download PDFInfo
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- CN105731539A CN105731539A CN201610072622.4A CN201610072622A CN105731539A CN 105731539 A CN105731539 A CN 105731539A CN 201610072622 A CN201610072622 A CN 201610072622A CN 105731539 A CN105731539 A CN 105731539A
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- 239000000843 powder Substances 0.000 title claims abstract description 51
- 239000012046 mixed solvent Substances 0.000 title claims abstract description 47
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 43
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910011312 Li3VO4 Inorganic materials 0.000 title claims abstract description 28
- 230000002194 synthesizing effect Effects 0.000 title abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims abstract description 24
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 238000003786 synthesis reaction Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- 230000015572 biosynthetic process Effects 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 14
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 13
- 239000012498 ultrapure water Substances 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 239000006194 liquid suspension Substances 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- PNEFIWYZWIQKEK-UHFFFAOYSA-N carbonic acid;lithium Chemical compound [Li].OC(O)=O PNEFIWYZWIQKEK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000012429 reaction media Substances 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- -1 oxygen-containing inorganic metal compound Chemical class 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- 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
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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)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with a high-temperature and high-pressure mixed solvent thermal system.The method comprises the steps that solid lithium carbonate powder and solid vanadium pentoxide serve as raw materials, a high-temperature and high-pressure mixed solvent serves as a reaction medium, and the lithium vanadate Li3VO4 monocrystal micrometer powder is synthesized with the condition ranges of 2-9 MPa, 200-350 DEG C and 1-4 h.The method has a unique advantage, the lithium vanadate Li3VO4 monocrystal micrometer powder can be quickly, easily and conveniently obtained, the physical phase is pure, the particle size ranges from 1 micrometer to 20 micrometers, and the dispersibility is good.The synthesizing method is easy, convenient and safe to implement, equipment is convenient to use and simple, the reaction process is easy to control, energy conservation and environment protection are achieved, and the method is especially suitable for industrialized mass production.
Description
Technical field
The present invention relates to a kind of can as the preparation method of the compound monocrystal micrometer structure of lithium ion battery negative material, particularly relate to one utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4The method of monocrystalline micron powder.
Background technology
Lithium vanadate Li3VO4It it is a kind of widely used material.Its crystal structure is the non-centrosymmetric structure of pmn21 type, the performances such as its nonlinear optics is had before and studies more widely.Li3VO4Theoretical capacity be 394mAh/g, there is cyclicity good, the features such as the electromotive force of charging and discharging is relatively low.Research finds, lithium vanadate Li3VO4It is likely to be the lithium ion battery negative material of a kind of function admirable.
According to the literature, lithium vanadate Li3VO4The synthetic method of dusty material generally has following several: conventional solid phase synthesis, sol-gal process, light water full-boiled process etc..These methods also exist some problems at present.The powder product granule-morphology that solid phase synthesis obtains is uneven, specific surface area is little, it is serious etc. to reunite, sol-gal process and light water full-boiled process batching step is complicated, process time is longer, technique is relatively complicated.The pattern of material, microcrystal grain distribution of sizes, granule dispersibility etc. be likely to material property produce greatly to affect." green chemistry chemical technology " process advocating energy-conserving and environment-protective also complies with the development trend in the field such as materialogy, chemical engineering.Therefore quick, safe and simple synthetic method is studied to obtain the lithium vanadate Li that thing is mutually pure, granule-morphology is uniformly regular3VO4Dusty material has important scientific research meaning.But, there is presently no through retrieval and utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4The pertinent literature report of monocrystalline micron powder.
Summary of the invention
For deficiency and the drawback of existing synthetic technology, the invention provides a kind of simple and feasible High Temperature High Pressure mixed solvent hot system that utilizes and synthesize lithium vanadate Li3VO4The method of monocrystalline micron powder.
Of the present invention utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4The method of monocrystalline micron powder, step is:
(1) dispensing: will as synthesis target lithium vanadate Li3VO4In raw material components Li, V according to the ratio of atomic ratio Li V=3 1, mix with the form of solid carbonic acid lithium powder and solid vanadium pentoxide powder；
(2) preparation mixed solvent: mixed according to the arbitrary proportion between volume ratio 19 to 91 with ultra-pure water by acetone, prepares mixed solvent；
(3) dispersed material: be scattered in the mixed solvent that step (2) is prepared by step (1) mixed pressed powder, forms solid-liquid suspension body, and wherein the amount of mixed solvent is 50～120 times of powder material volume；
(4) High Temperature High Pressure mixed solvent hot system is utilized to implement isothermal reaction；
(5) cooling: after isothermal reaction, cools down reaction vessel, and container inner pressure is down to normal pressure；
(6) washing: adopt centrifugation or is separated by the solid in reaction vessel by Vacuum filtration device with liquid, with ultra-pure water, ethanol or washing with acetone gained solid precipitation at least 3 times, or the liquid pH=7 after washing to washing stops；
(7) dry: the solid precipitation drying equipment after step (6) being washed is dried, it is thus achieved that product be the lithium vanadate Li of pure phase3VO4Monocrystalline micron powder；
It is characterized in that:
The described method utilizing High Temperature High Pressure mixed solvent hot system to implement isothermal reaction of step (4) is: put in high-temperature high-voltage reaction container by the solid-liquid suspension body that step (3) obtains, after airtight, reaction vessel is put and firing equipment heats to 200～350 DEG C, container inner pressure is 2～9MPa, isothermal reaction 1～4 hour, now the technical characteristic of reaction system is High Temperature High Pressure mixed solvent thermal response system；Wherein, described high-temperature high-voltage reaction container is the high-temperature high-pressure reaction kettle with thermometric, pressure tester；Described firing equipment refers to one of the Muffle furnace of precise control of temperature device, resistance furnace, tube furnace, baking oven；
Step (5) described reaction vessel is cooled to 20～25 DEG C, the mode of cooling is that according to setting speed, heater is cooled to room temperature, or directly cooling in power-off stove, or directly reaction vessel is taken out from heater natural cooling, or is put in frozen water after being taken out from heater by reaction vessel cooling；
The condition that the described centrifugation of step (6) is implemented is: centrifugal rotational speed 1000～2000 revs/min, centrifugation time 10～20 minutes；The filtering membrane of filter that described Vacuum filtration device adopts aperture to be 0.2～0.5 micron；
Step (7) described drying equipment is baking oven, drying baker or infrared lamp, and drying temperature is 50～60 DEG C.
Above-mentioned utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4In the method for monocrystalline micron powder: step (2) described acetone preferably mixes according to the arbitrary proportion between volume ratio 1:2 to 2:1 with ultra-pure water.
Above-mentioned utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4In the method for monocrystalline micron powder: 60～90 times of the amount of step (3) described mixed solvent preferably powder material volume.
Above-mentioned utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4In the method for monocrystalline micron powder: step (4) described heating-up temperature is preferably 250～300 DEG C, container inner pressure is preferably 6～9MPa, preferably 1～2 hour isothermal reaction time；Described firing equipment refers to the Muffle furnace of precise control of temperature device.
Above-mentioned utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4In the method for monocrystalline micron powder: the described centrifugal condition of step (6) is preferably: centrifugal rotational speed 1500 revs/min, centrifugation time 20 minutes.
Above-mentioned utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4In the method for monocrystalline micron powder: step (6) described Vacuum filtration device preferably employs the filtering membrane of filter that aperture is 0.22～0.45 micron.
Provided by the invention utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4The method of monocrystalline micron powder has the advantage of uniqueness, it is possible to obtain lithium vanadate Li by quick, safe and simple method3VO4Monocrystalline micro-powder material, solves in current synthetic process some existing problems, has promoted the development of the sciemtifec and technical sphere such as synthesis and application of Novel cathode material for lithium ion battery.
In the inventive method, be raw material by conventional solid phase inorganic salt and oxide first, using acetone and aqueous mixtures as reaction media, 2～9MPa, 200～350 DEG C temperature range, synthesized lithium vanadate Li in 1～4 little the reaction time3VO4Monocrystalline micropowder powder material.Lithium vanadate Li with the method synthesis3VO4Monocrystalline micropowder powder material, thing is mutually pure, and granule-morphology is more regular, and particle size range is 1～20 micron, and granule is not easily reunited, and dispersibility is relatively good.
The inventive method employs the reactant feed of solid phase, by High Temperature High Pressure mixed solvent hot system as reaction system, simplifying synthesis step, course of reaction is quick, reduce the unsafe factor in building-up process, it is easy to realize the control of building-up process and the control of product grain pattern simultaneously.Because preparation of raw material, consersion unit are fairly simple, course of reaction easily regulates and controls, and the inventive method is particularly suitable for industrialized mass production.
Lithium vanadate Li provided by the invention3VO4The High Temperature High Pressure mixed solvent hot system synthetic method of monocrystalline micropowder powder material applies also for the synthesis of some multivariant oxide monocrystalline micro materials, is the universal method of a kind of synthesizing oxygen-containing inorganic metal compound.
Accompanying drawing explanation
Fig. 1: adopt lithium vanadate Li prepared by High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein: Fig. 1 a is X-ray diffracting spectrum；Fig. 1 b is stereoscan photograph.
Fig. 2: adopt lithium vanadate Li prepared by High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein: Fig. 2 a is X-ray diffracting spectrum；Fig. 2 b is stereoscan photograph.
Fig. 3: adopt lithium vanadate Li prepared by High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein: Fig. 3 a is X-ray diffracting spectrum；Fig. 3 b is stereoscan photograph.
Fig. 4: adopt lithium vanadate Li prepared by High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein: Fig. 4 a is X-ray diffracting spectrum；Fig. 4 b is stereoscan photograph.
Detailed description of the invention
Embodiment 1
1. dispensing:
By 60ml acetone and 40ml ultra-pure water mix homogeneously, it is distributed in above-mentioned mixed solvent after 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride mixing.Be then added to thermometric, pressure tester high-temperature high-pressure reaction kettle (volume is 250 milliliters) in, seal.
2. utilize High Temperature High Pressure mixed solvent hot system to implement isothermal reaction:
The reactor of sealing is put in Muffle furnace, is heated to 280 DEG C (container inner pressure reaches 9MPa), constant 2 hours at this temperature.
3. cooling:
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. washing:
From reactor, take out product, product is filtered by vacuum filter (aperture is 0.45 micron), obtains solid sediment；With ultra-pure water, washing with alcohol gained solid precipitation to the liquid pH=7 after washing only.
5. dry:
By the solid that the obtains baking oven at 50 DEG C～60 DEG C temperature after filtering is dried, obtain lithium vanadate Li3VO4Powder.
X-ray diffraction is it is shown that test the lithium vanadate Li that powder is phase obtained3VO4(Fig. 1 a).Sem observation shows, powder is the Polyhedral Particles (Fig. 1 b) of average-size 1～3 micron.
Embodiment 2
1. dispensing:
By 60ml acetone and 40ml ultra-pure water mix homogeneously, it is distributed in above-mentioned mixed solvent after 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride mixing.Be then added to thermometric, pressure tester high-temperature high-pressure reaction kettle (volume is 250 milliliters) in, seal.
2. utilize High Temperature High Pressure mixed solvent hot system to implement isothermal reaction:
The reactor of sealing is put in Muffle furnace, is heated to 250 DEG C (container inner pressure reaches 6.2MPa), constant 1 hour at this temperature.
3. cooling:
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. washing:
From reactor, take out product, product is filtered by vacuum filter (aperture is 0.45 micron), obtains solid sediment；With ultra-pure water, washing with acetone gained solid precipitation to the liquid pH=7 after washing only.
5. dry:
By the solid that the obtains baking oven at 50 DEG C～60 DEG C temperature after filtering is dried, obtain lithium vanadate Li3VO4Microcrystalline powder.
X-ray diffraction is it is shown that the powder that experiment obtains is lithium vanadate Li3VO4(Fig. 2 a).Sem observation shows, powder is the rod-shpaed particle (Fig. 2 b) of long 3～5 microns of average-size diameter 1 micron.
Embodiment 3
1. dispensing:
By 50ml acetone and 50ml ultra-pure water mix homogeneously, it is distributed in above-mentioned mixed solvent after 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride mixing.Be then added to thermometric, pressure tester high-temperature high-pressure reaction kettle (volume is 250 milliliters) in, seal.
2. utilize High Temperature High Pressure mixed solvent hot system to implement isothermal reaction:
The reactor of sealing is put in Muffle furnace, is heated to 250 DEG C (container inner pressure reaches 6MPa), constant 1 hour at this temperature.
3. cooling:
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. washing:
From reactor, take out product, product is filtered by vacuum filter (aperture is 0.22 micron), obtains solid sediment；With ultra-pure water, washing with alcohol gained solid precipitation to the liquid pH=7 after washing only.
5. dry:
By the solid that the obtains baking oven at 50 DEG C～60 DEG C temperature after filtering is dried, obtain lithium vanadate Li3VO4Microcrystalline powder.
X-ray diffraction is it is shown that the powder that experiment obtains is lithium vanadate Li3VO4(Fig. 3 a).Sem observation shows, powder is the irregularly shaped particles (Fig. 3 b) of average-size 1～2 micron.
Embodiment 4
1. dispensing:
By 60ml acetone and 40ml ultra-pure water mix homogeneously, it is distributed in above-mentioned mixed solvent after 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride mixing.Be then added to thermometric, pressure tester high-temperature high-pressure reaction kettle (volume is 250 milliliters) in, seal.
2. utilize High Temperature High Pressure mixed solvent hot system to implement isothermal reaction:
The reactor of sealing is put in Muffle furnace, is heated to 270 DEG C (container inner pressure reaches 8MPa), constant 1 hour at this temperature.
3. cooling:
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. washing:
From reactor, take out product, product is filtered by vacuum filter (aperture is 0.45 micron), obtains solid sediment；With ultra-pure water, washing with acetone gained solid precipitation to the liquid pH=7 after washing only.
5. dry:
By the solid that the obtains baking oven at 50 DEG C～60 DEG C temperature after filtering is dried, obtain lithium vanadate Li3VO4Microcrystalline powder.
X-ray diffraction is it is shown that the powder that experiment obtains is lithium vanadate Li3VO4(Fig. 4 a).Sem observation shows, major part powder is the rod-shpaed particle (Fig. 4 b) of long 20 microns of diameter 5～10 microns.
Claims (4)
1. one kind utilizes High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4The method of monocrystalline micron powder, step is:
(1) dispensing: will as synthesis target lithium vanadate Li3VO4In raw material components Li, V according to the ratio of atomic ratio Li V=3 1, mix with the form of solid carbonic acid lithium powder and solid vanadium pentoxide powder；
(2) preparation mixed solvent: mixed according to the arbitrary proportion between volume ratio 19 to 91 with ultra-pure water by acetone, prepares mixed solvent；
(3) dispersed material: be scattered in the mixed solvent that step (2) is prepared by step (1) mixed pressed powder, forms solid-liquid suspension body, and wherein the amount of mixed solvent is 50～120 times of powder material volume；
(4) High Temperature High Pressure mixed solvent hot system is utilized to implement isothermal reaction；
(5) cooling: after isothermal reaction, cools down reaction vessel, and container inner pressure is down to normal pressure；
(6) washing: adopt centrifugation or is separated by the solid in reaction vessel by Vacuum filtration device with liquid, with ultra-pure water, ethanol or washing with acetone gained solid precipitation at least 3 times, or the liquid pH=7 after washing to washing stops；
(7) dry: the solid precipitation drying equipment after step (6) being washed is dried, it is thus achieved that product be the lithium vanadate Li of pure phase3VO4Monocrystalline micron powder；
It is characterized in that:
The described method utilizing High Temperature High Pressure mixed solvent hot system to implement isothermal reaction of step (4) is: put in high-temperature high-voltage reaction container by the solid-liquid suspension body that step (3) obtains, after airtight, reaction vessel is put and firing equipment heats to 200～350 DEG C, container inner pressure is 2～9MPa, isothermal reaction 1～4 hour, now the technical characteristic of reaction system is High Temperature High Pressure mixed solvent thermal response system；Wherein, described high-temperature high-voltage reaction container is the high-temperature high-pressure reaction kettle with thermometric, pressure tester；Described firing equipment refers to one of the Muffle furnace of precise control of temperature device, resistance furnace, tube furnace, baking oven；
Step (5) described reaction vessel is cooled to 20～25 DEG C, the mode of cooling is that according to setting speed, heater is cooled to room temperature, or directly cooling in power-off stove, or directly reaction vessel is taken out from heater natural cooling, or is put in frozen water after being taken out from heater by reaction vessel cooling；
The condition that the described centrifugation of step (6) is implemented is: centrifugal rotational speed 1000～2000 revs/min, centrifugation time 10～20 minutes；The filtering membrane of filter that described Vacuum filtration device adopts aperture to be 0.2～0.5 micron；
Step (7) described drying equipment is baking oven, drying baker or infrared lamp, and drying temperature is 50～60 DEG C.
2. utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li as claimed in claim 13VO4The method of monocrystalline micron powder, is characterized in that: step (4) described heating-up temperature is 250～300 DEG C, and container inner pressure is 6～9MPa, isothermal reaction 1～2 hour；Described firing equipment refers to the Muffle furnace of precise control of temperature device.
3. utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li as claimed in claim 13VO4The method of monocrystalline micron powder, is characterized in that: the described centrifugal condition of step (6) is: centrifugal rotational speed 1500 revs/min, centrifugation time 20 minutes.
4. utilize High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li as claimed in claim 13VO4The method of monocrystalline micron powder, is characterized in that: the filtering membrane of filter that the described Vacuum filtration device of step (6) adopts aperture to be 0.22～0.45 micron.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108321373A (en) * | 2018-02-01 | 2018-07-24 | 山东大学 | The method for synthesizing lithium titanate/titanium dioxide compound nano-multicrystal dusty material using high temperature and pressure mixed solvent hot system |
| CN109052471A (en) * | 2018-07-12 | 2018-12-21 | 中国科学院合肥物质科学研究院 | A kind of electrostatic spray prepares the method and application of lithium vanadate porous membrane |
| CN111106335A (en) * | 2019-12-20 | 2020-05-05 | 三峡大学 | Preparation method of lithium ion battery composite negative electrode material |
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| CN1575527A (en) * | 2001-10-25 | 2005-02-02 | 国立科学研究中心 | Lithium and vanadium oxide, a preparation method thereof and the use of same as an active electrode material |
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| CN103474641A (en) * | 2013-09-25 | 2013-12-25 | 三峡大学 | Lithium ion battery anode material Li3VO4 and preparation method thereof |
| CN105133016A (en) * | 2015-10-09 | 2015-12-09 | 新疆大学 | Preparation method and application of lithium vanadate nonlinear optical crystal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108321373A (en) * | 2018-02-01 | 2018-07-24 | 山东大学 | The method for synthesizing lithium titanate/titanium dioxide compound nano-multicrystal dusty material using high temperature and pressure mixed solvent hot system |
| CN108321373B (en) * | 2018-02-01 | 2020-07-07 | 山东大学 | Method for synthesizing lithium titanate/titanium dioxide composite nano polycrystalline powder material by utilizing high-temperature high-pressure mixed solvent thermal system |
| CN109052471A (en) * | 2018-07-12 | 2018-12-21 | 中国科学院合肥物质科学研究院 | A kind of electrostatic spray prepares the method and application of lithium vanadate porous membrane |
| CN111106335A (en) * | 2019-12-20 | 2020-05-05 | 三峡大学 | Preparation method of lithium ion battery composite negative electrode material |
| CN111106335B (en) * | 2019-12-20 | 2022-05-03 | 三峡大学 | Preparation method of lithium ion battery composite negative electrode material |
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| CN105731539B (en) | 2017-03-22 |
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