CN105753459A - Preparation method and products of organic metal complex and aluminum oxide compound - Google Patents
Preparation method and products of organic metal complex and aluminum oxide compound Download PDFInfo
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- CN105753459A CN105753459A CN201610129144.6A CN201610129144A CN105753459A CN 105753459 A CN105753459 A CN 105753459A CN 201610129144 A CN201610129144 A CN 201610129144A CN 105753459 A CN105753459 A CN 105753459A
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- Prior art keywords
- aluminium
- hydroxyquinoline
- oxide
- organometallic complex
- sintering
- Prior art date
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- -1 aluminum oxide compound Chemical class 0.000 title claims abstract description 13
- 150000004696 coordination complex Chemical class 0.000 title claims abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 62
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 62
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract description 7
- 239000004411 aluminium Substances 0.000 claims description 56
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 47
- 238000005245 sintering Methods 0.000 claims description 36
- 125000002524 organometallic group Chemical group 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 31
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 30
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 28
- 229960003540 oxyquinoline Drugs 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 20
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- 150000007522 mineralic acids Chemical class 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001942 caesium oxide Inorganic materials 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- NBYLBWHHTUWMER-UHFFFAOYSA-N 2-Methylquinolin-8-ol Chemical class C1=CC=C(O)C2=NC(C)=CC=C21 NBYLBWHHTUWMER-UHFFFAOYSA-N 0.000 claims 1
- 150000002927 oxygen compounds Chemical class 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 13
- 238000000576 coating method Methods 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 abstract 4
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 15
- 229910052744 lithium Inorganic materials 0.000 description 15
- 230000004888 barrier function Effects 0.000 description 12
- 239000011247 coating layer Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000012467 final product Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000007711 solidification Methods 0.000 description 6
- 230000008023 solidification Effects 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000000320 mechanical mixture Substances 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005213 imbibition Methods 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001399 aluminium compounds Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000001907 polarising light microscopy Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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Abstract
The invention provides organic metal complex.The organic metal complex is prepared by mixing bis(2-methyl-8-oxyquinoline-N1, O8)-(1, 1'-biphenyl-4-hydroxyl)aluminum and 8-oxychinolin aluminum, wherein the weight ratio of the bis(2-methyl-8-oxyquinoline-N1, O8)-(1, 1'-biphenyl-4-hydroxyl)aluminum and 8-oxychinolin aluminum to the 8-oxychinolin aluminum is 2-5:5-8.Atmosphere generated during high-temperature decomposition can have embedding and co-growth of certain degree, so that the growth orientation of crystals can be changed, the atomic structure on the surface of microcosmic particles can be improved, and functional material crystal structure design is achieved.When aluminum oxide compound obtained from the organic metal complex is prepared into a coating membrane, the coating membrane is outstanding in water absorption performance, and the self-discharge performance, voltage drop performance and normal-temperature circulation performance of the coating membrane are evidently better than those of a common aluminum oxide coating membrane.The preparation method of the organic metal complex is simple, practical, evident in effect, and capable of satisfying the requirements of large-scale industrial production.
Description
Technical field
The present invention relates to dynamic lithium battery and manufacture field, especially a kind of organometallic complex and oxidation
The preparation method of aluminium compound and product.
Background technology
Along with an urgent demand of new energy technology development, lithium-ion-power cell is high by specific energy density,
The characteristic such as memory-less effect and relative environmental protection become new energy technology first selection, but common lithium
Ion battery there is also certain potential safety hazard, is mainly manifested in thermal failure, external impacts and
When falling, there is on fire or blast due to reasons such as barrier film breakages in battery.In recent years, the whole world is right
Safety improvement means in lithium battery, especially dynamic lithium battery are mainly by pottery, are also with regard to alfa
The methods such as phase alumina coating improve barrier film material deformation effect in the case of external force and thermal shock, to reach
Purpose to safety improvement.
Common alumina material mainly has following several respects defect for power lithium battery:
1. grain structure is mainly random form is main, formed 2-4 micron thickness coating after, particle it
Between there is obvious spatial joint clearance, it is impossible to preferably stop Li dendrite metal deposit growth because
Reduce the effect improving lithium battery self discharge of ceramic-coated separator.
2., due to lithium battery diaphragm coating needs very thin thickness, typically within 5 micron thickness, therefore want
Ask the primary granule particle diameter of aluminum oxide coating layer typically between 100-400nm.The negative issue thus brought is
Submicron material has stronger water imbibition, and moisture can occur with the lithium salts in electrolyte after bringing lithium battery into
Chemical reaction, the ionic conduction ability destroying lithium salts has formed HF, causes battery to produce more serious knot
Structure destroys.
3. power lithium battery needs to ensure the durability of more than 10 years, therefore it is required that ceramic particle and bonding
Must keep good and lasting cohesive between agent, current common alumina surface active site is relatively low,
Typically significantly lost efficacy in 400-500 rear appearance of circulation, it is impossible to meet the primary demand of power lithium battery.
Therefore meet lithium battery, alfa phase alumina material that especially dynamic lithium battery security performance needs and
Its preparation the most just becomes technological difficulties in the industry.
Summary of the invention
The technical problem to be solved is to provide a kind of organometallic complex.
Another technical problem to be solved by this invention is to provide applies above-mentioned organometallic complex to prepare
The method of alumina compound.
Another technical problem to be solved by this invention is the product providing above-mentioned preparation method to be obtained
Alumina compound.
For solving above-mentioned technical problem, the technical scheme is that
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl)
Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3)
Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline
The mixture weight ratio of aluminium is 2-5:5-8.
Preferably, above-mentioned organometallic complex, described double (2-methyl-8-hydroxyquinoline-N1, O8)-
(1,1'-biphenyl-4-hydroxyl) aluminium is 2:8 with the mixture weight ratio of 8-hydroxyquinoline aluminium.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount
It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with
8-hydroxyquinoline aluminium mixes, and to obtain final product.
The application in terms of preparing alumina compound of the above-mentioned organometallic complex, can change the life of crystal
Long orientation.
According to defect (hole) mechanism of the crystal structure that practice draws, above-mentioned organic by adding in crystal
Metal complex, the atmosphere that its pyrolysis process produces can occur a certain degree of in hexagonal
Embed and symbiosis is long, thus change the orientation of growth of crystal, and improve the atomic structure on microscopic particles surface
Composition, thus reach the purpose of functional material crystal structure design.
Preferably, the method that above-mentioned organometallic complex prepares alumina compound, concrete steps are applied
For:
(1) by high-purity aluminium hydroxide micro powder by dry powder blender, with inorganic oxide additive and upper
State organometallic complex be blended prepare aluminium hydroxide compound, described inorganic oxide additive for oxidation
Barium, magnesia, yittrium oxide, chromium oxide, iron oxide, cesium oxide, titanium oxide, manganese oxide, silica
With the one in calcium oxide or any combination, described aluminium hydroxide micro powder and inorganic oxide additive and have
The consumption number of machine metal complex is aluminium hydroxide micro powder 920-970 part, inorganic oxide additive 30-60
Part, organometallic complex 10-30 part；
(2) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push-plate type and burns
Knot kiln, carries out high temperature sintering, wherein, sintering temperature 1100-1300 DEG C, and single group crucible material is at sintering oven
The middle time of staying is 4-8 hour, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing concentration
Hot-air for 10-25% (volume ratio) carbon dioxide.
Preferably, the preparation method of above-mentioned alumina compound, in described step (1), dry powder blender is double spiral shells
Rotation conical mixer.
Preferably, the preparation method of above-mentioned alumina compound, in described step (1), inorganic oxide adds
Add the grain diameter of agent to be chosen at 0.8-4.0 micron grain size scope there is preferable sintering effect.
Preferably, the preparation method of above-mentioned alumina compound, in described step (1), inorganic oxide adds
Add before agent uses and carry out Chemical Pretreatment, concretely comprise the following steps and inorganic oxide additive is placed on solidification bed
In reactor, being passed through the steam that inorganic acid mixes with air, wherein inorganic acid is nitric acid, hydrochloric acid or sulfuric acid,
The content of inorganic acid is 2.0-6.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 2.0-10.0kg/m2
Left and right, the process time in steam is 30-80min, and steam temperature is 20-50 DEG C.
The alumina compound obtained by above-mentioned preparation method, for laminated structure, radius-thickness ratio is at 8-30:1.
Described radius-thickness ratio uses crystal optics method to be measured, and the method is with spindle stage and polarized light microscopy
Mirror measures radius-thickness ratio: be first bonded on the needle point of spindle stage by sheet-like particle powder, then by rotary needle
Platform is fixed on petrographic microscope objective table；Subsequently rotate needle handle to be set level by particle, first measure horizontal
Particle diameter under state；Finally rotate needle handle 90 degree, measure grain thickness.Thus obtain particle diameter and thickness,
Finally calculate radius-thickness ratio.
The invention has the beneficial effects as follows:
Above-mentioned organometallic complex, the atmosphere produced in pyrolysis process can be sent out in hexagonal
Raw a certain degree of embedding and symbiosis are long, thus change the orientation of growth of crystal, and improve microscopic particles table
The atomic structure composition in face, thus reach the purpose of functional material crystal structure design, organic by this
After the alumina compound that metal complex is obtained makes coating, barrier film water absorbing properties highlights, and is certainly putting
Electricity aspect, voltage drop and normal-temperature circulating performance aspect are substantially better than common aluminum oxide coating layer barrier film, its system
Preparation Method is simple and practical, and effect is notable, is suitable for the needs that large-scale industrial produces.
Accompanying drawing explanation
Fig. 1 is the alumina powder pattern SEM contrast after shaping；
Fig. 2 is the coated separator made by alumina compound of the present invention, and common commercialization pottery
The water imbibition contrast of barrier film (common aluminum oxide coating layer), wherein, A is alumina composite of the present invention
Thing coating, B is commercial alumina coating；
Fig. 3 is the capacity attenuation test comparison figure after alumina compound prepares battery；
Fig. 4 is the self discharge test comparison figure after alumina compound prepares battery.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl)
Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3)
Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline
The mixture weight ratio of aluminium is 2:8.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount
It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with
8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 2
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl)
Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3)
Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline
The mixture weight ratio of aluminium is 5:5.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount
It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with
8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 3
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl)
Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3)
Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline
The mixture weight ratio of aluminium is 2:5.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount
It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with
8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 4
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl)
Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3)
Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline
The mixture weight ratio of aluminium is 5:8.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount
It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with
8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 5
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl)
Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3)
Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline
The mixture weight ratio of aluminium is 3:7.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount
It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with
8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 6
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the magnesia of 4:4:1:1, calcium oxide, yittrium oxide, cesium oxide, logical
Crossing machinery powder mixing apparatus to carry out being simply mixed uniformly, wherein, the grain diameter of each inorganic oxide exists
In the range of 1-3 micron grain size；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide
Powder is placed in fixed bedreactor, is passed through the steam that nitric acid mixes with air, wherein the containing of nitric acid
Amount is 3.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 3.0-4.0kg/m2, in steam
The process time is 60min, between steam temperature about 40 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 950 is taken by weight
Organometallic complex described in part, the inorganic oxide mixture 35 parts of step (2) gained, embodiment 1
15 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal
Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1200 DEG C, and single group crucible material is at sintering
In kiln, the time of staying is 6 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense
Degree is the hot-air of 20% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will
Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack,
Make finished product.
Utilizing laser fineness gage to detect finished product, result is as it is shown in figure 1, in bimodal distribution.
Embodiment 7
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the barium monoxide of 5:3:2, chromium oxide, iron oxide, by machinery powder
Mixing apparatus carries out being simply mixed uniformly, and wherein, the grain diameter of each inorganic oxide is at 0.8-4.0 micron
In particle size range；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide
Powder is placed in fixed bedreactor, is passed through the steam that hydrochloric acid mixes with air, wherein the containing of hydrochloric acid
Amount is 6.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 2.0-5.0kg/m2, in steam
The process time is 30min, between steam temperature about 50 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 920 is taken by weight
Organometallic complex described in part, the inorganic oxide mixture 60 parts of step (2) gained, embodiment 1
30 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal
Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1100 DEG C, and single group crucible material is at sintering
In kiln, the time of staying is 8 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense
Degree is the hot-air of 10% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will
Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack,
Make finished product.
Embodiment 8
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the magnesia of 4:2:1, titanium oxide, silica, by machinery powder
Mixing apparatus carries out being simply mixed uniformly, and wherein, the grain diameter of each inorganic oxide is at 2-4 micron grain size
In the range of；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide
Powder is placed in fixed bedreactor, is passed through the steam that sulfuric acid mixes with air, wherein the containing of sulfuric acid
Amount is 2.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 7.0-10.0kg/m2, in steam
The process time is 80min, between steam temperature about 20 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 970 is taken by weight
Organometallic complex described in part, the inorganic oxide mixture 30 parts of step (2) gained, embodiment 1
10 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal
Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1300 DEG C, and single group crucible material is at sintering
In kiln, the time of staying is 4 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense
Degree is the hot-air of 25% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will
Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack,
Make finished product.
Embodiment 9
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the magnesia of 7:3, manganese oxide, is carried out by machinery powder mixing apparatus
Being simply mixed uniformly, wherein, the grain diameter of each inorganic oxide is in the range of 2-3 micron grain size；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide
Powder is placed in fixed bedreactor, is passed through the steam that nitric acid mixes with air, wherein the containing of nitric acid
Amount is 4.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 4.0-7.0kg/m2, in steam
The process time is 70min, between steam temperature about 35 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 940 is taken by weight
Organometallic complex described in part, the inorganic oxide mixture 45 parts of step (2) gained, embodiment 1
20 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal
Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1200 DEG C, and single group crucible material is at sintering
In kiln, the time of staying is 6 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense
Degree is the hot-air of 15% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will
Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack,
Make finished product.
Below in conjunction with concrete test example, the present invention is described in detail.
Aluminum oxide coating layer prepares power lithium battery application test
Select alumina compound, water, polyacrylate (adhesive), polycarboxylic acids described in embodiment 6
(dispersant) and analyze pure propyl alcohol (wetting agent), described alumina compound, water, polyacrylic acid
The weight ratio of the pure propyl alcohol of ester, polycarboxylic acids and analysis is 40:50:4:1:0.5, by the way of high speed dispersion, and system
Becoming the aluminum oxide glue of 50% solid content, viscosity is at 50-80CP, by the coating of micro-gravure coater one side
Mode, applies twice at Asahi Chemical Industry's PE12um matrix surface, forms the aluminum oxide coating layer of each 4um in two sides,
Barrier film gross thickness 20um；
Choosing the most extremely ternary material, negative pole is the 30AH standard lithium battery of modified graphite, uses above-mentioned
The double-surface ceramics barrier film (12um matrix, two sides each 4um coating) of coated separator and common commercial is carried out
Contrast test.
Test shows:
As in figure 2 it is shown, alumina composite material prepared by the present invention, after making coating, hence it is evident that micro-
See and be different from commercially available common alumina material (double-surface ceramics barrier film), after measured, averagely in architectural feature
Radius-thickness ratio is 16:1, and common commercial alumina is irregularly shaped, and radius-thickness ratio is between 1:1-2.4:1.
And as can be seen from Table 1, coated separator water imbibition is substantially better than common aluminum oxide coating layer；
It addition, at ternary material (nickel cobalt manganese molar ratio 5:2:3) as positive pole, modifying natural graphite material
Battery evaluation is carried out as (energy density is 480wh/L) in the 30Ah square aluminum housing battery of negative pole. such as figure
Shown in 3 and Fig. 4, after making dynamic lithium battery, in terms of self discharge, use barrier film of the present invention every
In regulation ageing time, (7 days) voltage reduces to 6.02 millivolts to film battery, and control cell is at 9.32 millivolts,
Keeping battery voltage performance made by this patent is substantially better than common aluminum oxide coating layer barrier film；Final battery is normal
Temperature cycle performance is also significantly better than the battery of common aluminum oxide coating layer barrier film, made by barrier film of the present invention
Circulating battery 600 times, capability retention about 87%, control cell capacity then less than 80%,
And rapid corruptions occurs.
Table 1 moisture entrapment content balance
Described test specimen refers to alumina composite material of the present invention；Reference sample refers to commercially available common
Alumina material.
Above-mentioned with reference to embodiment to this for the alumina compound applying dynamic lithium battery and preparation method thereof
The detailed description carried out, is illustrative rather than determinate, if can according to restriction scope list
Dry embodiment, therefore changing and modifications under without departing from present general inventive concept, should belong to the present invention's
Within protection domain.
Claims (7)
1. an organometallic complex, it is characterised in that: by double (2-methyl-8-hydroxyquinoline-N1, O8)-
(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline aluminium composition, described double (2-methyl-8-hydroxyquinolines
-N1, O8) the mixture weight ratio of-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline aluminium is 2-5:5-8.
Organometallic complex the most according to claim 1, it is characterised in that: described double (2-
Methyl-8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline aluminium
For 2:8.
3. the application in terms of preparing alumina compound of the organometallic complex described in claim 1,
The orientation of growth of crystal can be changed.
4., by the application of organometallic complex described in claim 3, prepare the side of alumina compound
Method, it is characterised in that: concretely comprise the following steps:
(1) by high-purity aluminium hydroxide micro powder by dry powder blender, with inorganic oxide additive and upper
State organometallic complex be blended prepare aluminium hydroxide compound, described inorganic oxide additive for oxidation
Barium, magnesia, yittrium oxide, chromium oxide, iron oxide, cesium oxide, titanium oxide, manganese oxide, silica
With the one in calcium oxide or any combination, described aluminium hydroxide micro powder and inorganic oxide additive and have
The consumption number of machine metal complex is aluminium hydroxide micro powder 920-970 part, inorganic oxide additive 30-60
Part, organometallic complex 10-30 part；
(2) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push-plate type and burns
Knot kiln, carries out high temperature sintering, wherein, sintering temperature 1100-1300 DEG C, and single group crucible material is at sintering oven
The middle time of staying is 4-8 hour, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing concentration
Hot-air for 10-25% (v/v) carbon dioxide.
The preparation method of alumina compound the most according to claim 4, it is characterised in that: described
In step (1), the grain diameter of inorganic oxide additive is chosen at 0.8-4.0 micron grain size scope and has relatively
Good sintering effect.
The preparation method of alumina compound the most according to claim 4, it is characterised in that: described
In step (1), inorganic oxide additive carries out Chemical Pretreatment before using, and concretely comprises the following steps inorganic oxygen
Compound additive is placed in fixed bedreactor, is passed through the steam that inorganic acid mixes, Qi Zhongwu with air
Machine acid is nitric acid, hydrochloric acid or sulfuric acid, and the content of inorganic acid is 2.0-6.0% (wt), solidifies the inorganic of bed surface
Oxide placement amount is at 2.0-10.0kg/m2Left and right, the process time in steam is 30-80min, steam temperature
Degree is for 20-50 DEG C.
7. the alumina compound obtained by the described preparation method of one of claim 4-6, it is characterised in that:
In the form of sheets, radius-thickness ratio is between 8-30:1.
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| CN111192992A (en) * | 2020-01-20 | 2020-05-22 | 武汉中兴创新材料技术有限公司 | Preparation method and device of ultrathin coating diaphragm |
| CN115445304A (en) * | 2022-07-29 | 2022-12-09 | 扬州中天利新材料股份有限公司 | High-purity magnesium oxide production is with electric pressure release all-in-one of straining |
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| CN115445304A (en) * | 2022-07-29 | 2022-12-09 | 扬州中天利新材料股份有限公司 | High-purity magnesium oxide production is with electric pressure release all-in-one of straining |
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