CN106186008A - A kind of lithium battery diaphragm coating boehmite and hydrothermal preparing process thereof - Google Patents
A kind of lithium battery diaphragm coating boehmite and hydrothermal preparing process thereof Download PDFInfo
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- CN106186008A CN106186008A CN201610512184.9A CN201610512184A CN106186008A CN 106186008 A CN106186008 A CN 106186008A CN 201610512184 A CN201610512184 A CN 201610512184A CN 106186008 A CN106186008 A CN 106186008A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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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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- 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
- C01P2006/12—Surface area
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- 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
- C01P2006/80—Compositional purity
Abstract
The present invention provides a kind of lithium battery diaphragm ceramic coating boehmite and hydrothermal preparing process thereof, under quick stirring, precipitant solution is quickly added dropwise to Al3+Saline solution be hydrolyzed after, ageing, filter pressing, the indefinite form aluminum presoma obtained is put into reactor carries out hydro-thermal reaction, obtain single dispersing, high-purity boehmite powder.The boehmite particles dispersibility of synthesis is high, and narrow diameter distribution, specific surface is 2～15m2/ g, mean diameter 500～800nm, high purity 99.95%.The method inorganic combustion inhibitor of the present invention, organic catalyst, sewage treating material etc., prepared boehmite purity is high, and dispersion high-crystallinity is good, narrow diameter distribution.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, particularly to a kind of lithium battery diaphragm coating boehmite and
Its hydrothermal preparing process.
Background technology
Boehmite (Boehmite), also known as boehmite, boehmite, molecular formula is γ-AlOOH, AlO (OH) (hydration
Aluminium oxide), it is a kind of to crystallize hydrated alumina incomplete, containing a water of crystallization, belongs to rhombic system, there is stratiform
Structure.In these are laminar structured, an aluminium ion (A13+) and 6 oxonium ion (O of surrounding2-) define the eight of a deformation
Face body, the total octahedra border of oxonium ion is connected by double-deck zigzag hydrogen bond and forms.The structure of this uniqueness makes it
At preparation α-Al2O3Important persursor material, inorganic combustion inhibitor, organic catalyst, adsorbent, the field such as sewage treating material
There is the biggest application future.
Due to boehmite excellent physical, chemical property, it is also widely used in the field of some new developments.As at battery
Barrier film coating material this respect, boehmite has also been employed that, market is even exclusively used for battery diaphragm coating material aspect
Boehmite product.After barrier film is coated with last layer boehmite coating, can effectively play and be similar to α-Al2O3Effect: avoid electricity
Short circuit between pole, improves the safety that lithium battery uses, and can promote the guarantor's fluidity of the imbibition to electrolyte.And due to synthesized
Boehmite price far below α-Al2O3Price, use boehmite replace α-Al2O3As barrier film coated ceramic material, can pole
The earth reduces coating barrier film production cost, and reduces when the abrasion of nick roller, barrier film during coating are cut greatly by aluminium oxide hardness pair
The abrasion of blade.
In recent years, boehmite material technology of preparing has obtained developing faster, occurs in that many new synthetic methods, such as gas
Xiang Fa, solvent-thermal process method (hydrothermal synthesis method), sol-gel process, the sedimentation method, ionic liquid method, hard template method etc..Chinese patent
Publication number CN 103663519 A, its boehmite material prepared employs meta-aluminate as aluminum source, and carbamide is precipitant,
Under thermal and hydric environment, at a temperature of 130-200 DEG C, prepare diameter 2-5 micron under the conditions of reacting 2-24 hour and there is micro-nano
The boehmite of hierarchy.China Patent Publication No. CN 103011215 A employs sodium aluminate, carbamide is raw material, high at high temperature
It is heated to 140-180 DEG C in pressure reactor, is incubated 8-15 hour, obtains Boehmite micro-nano structure sphere shape powder body material.China is specially
It is raw material that profit publication number CN 102815733 A uses boehmite, mineral acid or inorganic base, water in autoclave
Thermal response, obtains nanoscale boehmite.China Patent Publication No. CN 102701244 A, by aluminum salt solution, precipitant, is mixed in
In hydrothermal reaction kettle, under hydrothermal conditions, temperature controls at 120～200 DEG C, reacts and obtains boehmite micropowder in 6～24 hours
Body.
It is an object of the invention to provide a kind of granule to be uniformly dispersed, high-purity, the vigorous nurse of tabular of the rhombus of narrow diameter distribution
Preparation Method made of stones.Synthesized boehmite can solve the problem that the deficiency on aluminium oxide used by barrier film coating processes now, greatly drops
Low cost, and reduce when the abrasion of nick roller, barrier film during coating are cut greatly by aluminium oxide hardness the abrasion to blade.
Summary of the invention
It is an object of the invention to provide a kind of particle dispersion high, narrow diameter distribution, what purity was high prepares the side of boehmite
Method, the method can solve the problem that the deficiency on existing industrial manufacture process, and Simplified flowsheet, reduction cost, prepared boehmite is pure
Degree height, dispersion high-crystallinity is good, narrow diameter distribution.
The present invention provides the preparation method of a kind of water heat transfer boehmite, comprises the following steps:
A pure water solution is warming up to 30 DEG C～100 DEG C by ()；
B Al salt is dissolved in pure water by (), prepare Al saline solution after stirring；
C precipitant solution is added dropwise to Al saline solution and is stirred hydrolysis by ()；
D () quickly regulates above-mentioned solution pH value is 3.5～5.5, is then aged 1～10 hour by solution constant temperature；
After (e) ageing, remove the moisture in solidliquid mixture；
F the indefinite form aluminum presoma obtained and precipitant solution are put in (large-scale) high-temperature high-pressure reaction kettle and are reacted by (),
Compactedness is 60～80%；
G reactor under quick stirring, is warming up to 150～250 DEG C by (), Temperature fall, obtains γ-AlOOH slurry
Material；
H (), by after the γ-AlOOH slurry washing 1 obtained～7 times, is spray-dried, prepare boehmite powder.
Preferably, in described step (c), temperature during hydrolysis is 40～70 DEG C, preferable temperature 50～65 DEG C, mixing speed
It is 200～1000rpm.
Preferably, the time regulating above-mentioned solution pH value in described step (d) is 0.01～6min, and governing speed is 0.01
～effect is more preferable during 3min, described pH value controls 3.5～5.5, and pH value is more favorably to react when 4.0～5.0；Constant temperature ageing 1
～10 hours, constant temperature is aged preferably 3～7 hours.
Preferably, in described step (g), heating rate controls between 0.5～4.0 DEG C/min, and heating rate reaches 1.0
～during 3.0 DEG C/min, effect is more excellent；Reactor mixing speed 200～1000rpm, preferably 400～800rpm.
Preferably, after reactor is warming up to 150～250 DEG C by described step (g), preferably 160～220 DEG C；Need elder generation
It is incubated 2～10 hours, preferably 2～7 hours, Temperature fall the most again.
Preferably, in described step (f) in reactor in mixed liquor the concentration of aluminum presoma be 0.1～2.0mol L-1,
It is further 0.4～1.0mol L-1。
Preferably, in described step (b), Al salt is selected from Al (NO3)3·9H2O or AlCl3·6H2O, preferably Al
(NO3)3·9H2O。
Preferably, described precipitant solution is selected from carbamide, or NH3·H2O, or carbamide and NH3·H2The mixture of O,
It is preferably carbamide and NH3·H2Both O mixed solution.
Preferably, the moisture mode removing solidliquid mixture in described step (e) takes off selected from filtration, filter pressing or dewaterer
Water.
The method according to the invention synthesis prepares boehmite powder, and boehmite powder is the tabular monodisperse particles of rhombus,
Degree of crystallinity is high, and specific surface is 2～15m2/ g, mean diameter is 500～800nm, and purity is more than 99.95%.
Unique distinction of the present invention is to use hydro-thermal method, by controlling the experiment parameter of whole flow process (such as aluminum source, temperature, PH
Value, precipitant etc.) control to synthesize the pattern of boehmite.The boehmite particles dispersibility of synthesis is high, narrow diameter distribution, specific surface
It is 2～15m2/ g, mean diameter 500～800nm, high purity 99.95%, can apply to lithium battery diaphragm coated ceramic
Material, preparation α-Al2O3Important persursor material, inorganic combustion inhibitor, organic catalyst, sewage treating material etc..The present invention's
Purpose is to provide a kind of granule and is uniformly dispersed, high-purity, the tabular boehmite preparation method of the rhombus of narrow diameter distribution.Synthesized
Boehmite can solve the problem that the deficiency on aluminium oxide used by barrier film coating processes now, greatly reduce cost, and reduce oxidation
Abrasion to blade when the abrasion of nick roller, barrier film during coating are cut greatly by aluminum hardness.Prepared boehmite purity is high, dispersion
Degree high-crystallinity is good, narrow diameter distribution.
Accompanying drawing explanation
Fig. 1 present invention process flow chart
The scanning electron microscope (SEM) photograph of the boehmite product of Fig. 2 present invention synthesis
The boehmite product of Fig. 3 present invention synthesis is coated in the scanning electron microscope (SEM) photograph on lithium battery diaphragm surface
Detailed description of the invention
Below in conjunction with specific embodiment and accompanying drawing, present disclosure is further illustrated, but the protection of the present invention
Scope is not limited only to the content described by embodiment.
Embodiment 1
(1) pure water solution is warming up to 100 DEG C；
(2) according to stoichiometric proportion precise AlCl3·6H2O, is dissolved in pure water, with the mixing speed of 200rpm
Stirring prepares saline solution；
(3) raising mixing speed is to 350rpm, controls solution temperature, at 70 DEG C, then quickly to be instilled by precipitant carbamide
To Al3+Saline solution be hydrolyzed；
(4) in 6min, rapid titration to solution pH value is 5.5, then keeps the mixing speed of 350rpm, 70 DEG C of constant temperature
It is aged 1 hour；
(5) after constant temperature ageing, obtaining the solidliquid mixture containing precipitation, the moisture of solidliquid mixture is removed in filter pressing, will
To indefinite form aluminum presoma and precipitant carbamide put in (large-scale) high-temperature high-pressure reaction kettle, add to the 80% of compactedness,
The concentration controlling aluminum presoma is 2.0mol L-1；
(6) by reactor under 200rpm stirs speed stirring, it is heated to 250 DEG C with 4.0 DEG C/min heating rate, temperature retention time
Control after 2 hours, Temperature fall, obtain γ-AlOOH slurry；
(7) it is spray-dried after the γ-AlOOH slurry washing that obtains 7 times with ultra-pure water, obtains single dispersing, high-purity
Boehmite powder.The boehmite particles dispersibility of synthesis is high, and narrow diameter distribution, specific surface is 2.2m2/ g, mean diameter exists
530nm, high purity 99.95%.
Embodiment 2
(1) pure water solution is warming up to 75 DEG C；
(2) according to stoichiometric proportion precise Al (NO3)3·9H2O, is dissolved in pure water, with the stirring of 400rpm
Speed stirring prepares saline solution；
(3) raising mixing speed is to 500rpm, is controlled by solution temperature at 60 DEG C, by NH3·H2O solution is quickly added dropwise to
Al3+Saline solution be hydrolyzed；
(4) in 4min, rapid titration to solution pH value is 4.8, then keeps the mixing speed of 500rpm, 60 DEG C of constant temperature
It is aged 3 hours；
(5) after constant temperature ageing, obtaining the solidliquid mixture containing precipitation, the moisture of solidliquid mixture is removed in dehydration, will
The indefinite form aluminum presoma arrived and NH3·H2O solution is put in (large-scale) high-temperature high-pressure reaction kettle, adds to the 80% of compactedness,
The concentration controlling aluminum presoma is 1.2mol L-1；
(6) by reactor under 450rpm stirs speed stirring, it is heated to 210 DEG C with 2.8 DEG C/min heating rate, temperature retention time
Control after 3.5 hr, Temperature fall, obtain γ-AlOOH slurry；
(7) it is spray-dried after the γ-AlOOH slurry washing that obtains 5 times with ultra-pure water, obtains single dispersing, high-purity
Boehmite powder.The boehmite particles dispersibility of synthesis is high, and narrow diameter distribution, specific surface is 5.6m2/ g, mean diameter exists
780nm, high purity 99.95%.
Embodiment 3
(1) pure water solution is warming up to 50 DEG C；
(2) according to stoichiometric proportion precise Al (NO3)3·9H2O, is dissolved in pure water, with the stirring of 650rpm
Saline solution is prepared after speed stirring；
(3) it is kept stirring for speed 650rpm, solution temperature is controlled at 50 DEG C, by precipitant carbamide and NH3·H2Both O
Mixture solution is quickly added dropwise to Al3+Saline solution be hydrolyzed；
(4) in 2.0min, rapid titration to solution pH value is 4.2, then 50 DEG C of constant temperature under the mixing speed of 650rpm
It is aged 6 hours；
(5), after constant temperature ageing, obtain the solidliquid mixture containing precipitation, filter the moisture removing solidliquid mixture, will
The indefinite form aluminum presoma arrived and precipitant carbamide and NH3·H2Both O mixture solution puts into (large-scale) high-temperature high-pressure reaction kettle
In, adding to the 80% of compactedness, the concentration controlling aluminum presoma is 0.62mol L-1；
(6) by reactor under 750rpm stirs speed stirring, it is heated to 185 DEG C with 1.6 DEG C/min heating rate, temperature retention time
Control after 6 hours, Temperature fall, obtain γ-AlOOH slurry；
(7) it is spray-dried after the γ-AlOOH slurry washing that obtains 4 times with ultra-pure water, obtains single dispersing, high-purity
Boehmite powder.The boehmite particles dispersibility of synthesis is high, and narrow diameter distribution, specific surface is 8.9m2/ g, mean diameter exists
680nm, high purity 99.95%.
Embodiment 4
(1) pure water solution is warming up to 30 DEG C；
(2) according to stoichiometric proportion precise Al (NO3)3·9H2O, is dissolved in pure water, with the stirring of 1000rpm
Saline solution is prepared after speed stirring；
(3) under the stirring of 1000rpm, solution temperature is controlled at 40 DEG C, by precipitant carbamide and NH3·H2O two
Person's mixture solution is quickly added dropwise to Al3+Saline solution be hydrolyzed；
(4) in 0.5min, rapid titration to solution pH value is 3.5, then 40 DEG C of perseverances under the mixing speed of 1000rpm
Temperature ageing 10 hours；
(5) after constant temperature ageing, obtaining the solidliquid mixture containing precipitation, the moisture of solidliquid mixture is removed in filter pressing, will
The indefinite form aluminum presoma arrived and precipitant carbamide and NH3·H2Both O mixture solution puts into (large-scale) high-temperature high-pressure reaction kettle
In, adding to the 80% of compactedness, the concentration controlling aluminum presoma is 0.1mol L-1；
(6) by reactor under 1000rpm stirs speed stirring, it is heated to 150 DEG C, during insulation with 0.5 DEG C/min heating rate
Between control after 10 hours, Temperature fall, obtain γ-AlOOH slurry；
(7) it is spray-dried after the γ-AlOOH slurry washing that obtains 3 times with ultra-pure water, obtains single dispersing, high-purity
Boehmite powder.The boehmite particles dispersibility of synthesis is high, and narrow diameter distribution, specific surface is 15m2/ g, mean diameter exists
690nm, high purity 99.95%.
It is above the present invention has been carried out concrete elaboration, is adapted to assist in and understands the present invention, but embodiments of the present invention
And be not restricted to the described embodiments, any without departing from the change made under the principle of the invention, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. a hydrothermal preparing process for lithium battery diaphragm ceramic coating boehmite, mainly comprises the steps that
A pure water solution is warming up to 30 DEG C～100 DEG C by ()；
B Al salt is dissolved in pure water by (), prepare Al saline solution after stirring；
C precipitant solution is added dropwise to Al saline solution and is stirred hydrolysis by ()；
D () quickly regulates above-mentioned solution pH value is 3.5～5.5, is then aged 1～10 hour by solution constant temperature；
After (e) ageing, remove the moisture in solidliquid mixture；
F the indefinite form aluminum presoma obtained and precipitant solution are put in (large-scale) high-temperature high-pressure reaction kettle and are reacted by (), fill
Degree is 60～80%；
G reactor under stirring, is warming up to 150～250 DEG C by (), Temperature fall obtains γ-AlOOH slurry；
H (), by after the γ-AlOOH slurry washing 1 obtained～7 times, is spray-dried, prepare boehmite powder.
Preparation method the most according to claim 1, it is characterised in that in described step (c) temperature during hydrolysis be 40～
70 DEG C, preferable temperature 50～65 DEG C, mixing speed is 200～1000rpm.
Preparation method the most according to claim 1, it is characterised in that regulate above-mentioned solution pH value in described step (d)
Time is 0.01～6min, preferably 0.01～3min；Described pH value is preferably 4.0～5.0, and the ageing preferably 3～7 of described constant temperature is little
Time.
Preparation method the most according to claim 1, it is characterised in that in described step (g) heating rate control 0.5～
Between 4.0 DEG C/min, preferably heating rate is at 1.0～3.0 DEG C/min；Reactor mixing speed is 200～1000rpm, preferably
It is 400～800rpm.
5. according to the preparation method described in claim 1 or 4, it is characterised in that reactor is warming up to by described step (g)
After 150～250 DEG C, need first to be incubated 2～10 hours, preferably 3～7 hours, lower the temperature the most again.
Preparation method the most according to claim 1, it is characterised in that aluminum in mixed liquor in reactor in described step (f)
The concentration of presoma is 0.1～2.0mol L-1, preferably 0.5～1.3mol L-1。
Preparation method the most according to claim 1, it is characterised in that in described step (b), Al salt is selected from Al (NO3)3·
9H2O or AlCl3·6H2O。
Preparation method the most according to claim 1, it is characterised in that described precipitant solution is selected from carbamide or NH3·H2O,
Or the mixture for both.
Preparation method the most according to claim 1, it is characterised in that remove the water of solidliquid mixture in described step (e)
The mode of dividing is selected from filtration, filter pressing or dewaterer dehydration.
10. being prepared a lithium battery diaphragm coating boehmite by the arbitrary described preparation method of claim 1-9, its feature exists
In, boehmite powder is the tabular monodisperse particles of rhombus, and degree of crystallinity is high, and specific surface is 2～15m2/ g, mean diameter is 500
～800nm, purity is more than 99.95%.
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| CN201610512184.9A CN106186008B (en) | 2016-06-30 | 2016-06-30 | Boehmite for lithium battery diaphragm coating and hydrothermal preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107946521A (en) * | 2017-11-29 | 2018-04-20 | 山东聊城瑞利金属材料有限公司 | A kind of lithium battery diaphragm aluminium oxide manufacture method of boehmite coating |
| CN109534376A (en) * | 2019-01-17 | 2019-03-29 | 滨州市金毅设备有限公司 | A kind of high purification preparation method of boehmite |
| CN110197886A (en) * | 2018-02-26 | 2019-09-03 | 宁德新能源科技有限公司 | A kind of isolation film and electrochemical appliance |
| CN110357135A (en) * | 2019-06-19 | 2019-10-22 | 苏州盛曼特新材料有限公司 | A kind of preparation method of high-purity lithium battery diaphragm special-alumina |
| CN110451538A (en) * | 2019-08-20 | 2019-11-15 | 中铝山东有限公司 | A kind of preparation method of high-purity boehmite and high purity aluminium oxide |
| CN111341982A (en) * | 2020-03-18 | 2020-06-26 | 江苏厚生新能源科技有限公司 | Coated diaphragm, preparation method, doped boehmite, ceramic slurry and lithium battery |
| CN111792660A (en) * | 2020-07-15 | 2020-10-20 | 东北大学 | Method for producing boehmite micro-nano powder by using aluminum chloride |
| CN113860342A (en) * | 2021-11-05 | 2021-12-31 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepipedal boehmite and high-purity parallelepipedal boehmite |
| CN114538488A (en) * | 2022-02-23 | 2022-05-27 | 山东诚祥新能源股份有限公司 | Preparation method of high-purity boehmite for lithium battery diaphragm |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107946521A (en) * | 2017-11-29 | 2018-04-20 | 山东聊城瑞利金属材料有限公司 | A kind of lithium battery diaphragm aluminium oxide manufacture method of boehmite coating |
| CN110197886A (en) * | 2018-02-26 | 2019-09-03 | 宁德新能源科技有限公司 | A kind of isolation film and electrochemical appliance |
| CN109534376A (en) * | 2019-01-17 | 2019-03-29 | 滨州市金毅设备有限公司 | A kind of high purification preparation method of boehmite |
| CN110357135A (en) * | 2019-06-19 | 2019-10-22 | 苏州盛曼特新材料有限公司 | A kind of preparation method of high-purity lithium battery diaphragm special-alumina |
| CN110357135B (en) * | 2019-06-19 | 2020-11-24 | 苏州盛曼特新材料有限公司 | Preparation method of special alumina for high-purity lithium battery diaphragm |
| CN110451538A (en) * | 2019-08-20 | 2019-11-15 | 中铝山东有限公司 | A kind of preparation method of high-purity boehmite and high purity aluminium oxide |
| CN111341982A (en) * | 2020-03-18 | 2020-06-26 | 江苏厚生新能源科技有限公司 | Coated diaphragm, preparation method, doped boehmite, ceramic slurry and lithium battery |
| CN111341982B (en) * | 2020-03-18 | 2022-11-25 | 江苏厚生新能源科技有限公司 | Coated diaphragm, preparation method, doped boehmite, ceramic slurry and lithium battery |
| CN111792660A (en) * | 2020-07-15 | 2020-10-20 | 东北大学 | Method for producing boehmite micro-nano powder by using aluminum chloride |
| CN113860342A (en) * | 2021-11-05 | 2021-12-31 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepipedal boehmite and high-purity parallelepipedal boehmite |
| CN113860342B (en) * | 2021-11-05 | 2023-08-08 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepiped boehmite and high-purity parallelepiped boehmite |
| CN114538488A (en) * | 2022-02-23 | 2022-05-27 | 山东诚祥新能源股份有限公司 | Preparation method of high-purity boehmite for lithium battery diaphragm |
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