CN110054208A - A kind of porous flake boehmite and its prepare the purposes that lithium ion battery applies cloth diaphragm - Google Patents
A kind of porous flake boehmite and its prepare the purposes that lithium ion battery applies cloth diaphragm Download PDFInfo
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- CN110054208A CN110054208A CN201910334009.9A CN201910334009A CN110054208A CN 110054208 A CN110054208 A CN 110054208A CN 201910334009 A CN201910334009 A CN 201910334009A CN 110054208 A CN110054208 A CN 110054208A
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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
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to technical field of inorganic nanometer material, and in particular to a kind of porous flake boehmite, and preparation method and its purposes for preparing lithium ion battery painting cloth diaphragm are further disclosed.Flake porous boehmite of the present invention, by adding suitable pore creating material and Adjunct humectants, is prepared, the boehmite is the sheet boehmite material with porous structure using aluminium salt as raw material through high temperature hydrothermal process.The porous structure of the flake porous boehmite is suitable for lithium battery diaphragm coating and uses, and can effectively improve aperture and the porosity of battery diaphragm, and can reduce resistance and improve ionic conductivity, helps to improve the permeability and lithium ion battery passability of battery diaphragm.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, and in particular to a kind of porous flake boehmite, and it is further public
It opens preparation method and it prepares the purposes that lithium ion battery applies cloth diaphragm.
Background technique
Lithium ion battery due to specific energy is big, operating voltage is high, service life cycle is long, memory-less effect, self discharge are small,
Pollution free green environment protection, the advantages that having extended cycle life, have been widely used in Portable mobile electronic device, and be listed in electronic
Automobile, space flight, military affairs and large-scale energy storage device candidate power supply.Capacity, resistance to height with the development of lithium ion battery, to battery
Cryogenic property and cycle life etc. require higher and higher, and lithium ion battery is a kind of to use extensive secondary cell at present.
Lithium ion battery is mainly made of the four big materials including positive electrode, negative electrode material, diaphragm, electrolyte.
The component part one of important as its, diaphragm play the role of its performance considerable.Diaphragm (battery
Separator) refer to one layer of diaphragm material between the anode and cathode of battery, be usually referred to as with battery diaphragm, it is main
Effect is isolation positive and negative electrode and prevents the electronics in battery from passing freely through, while allowing the ion in electrolyte in positive and negative anodes
Between pass freely through.
In the prior art, boehmite is the main material for preparing lithium ion battery separator.Boehmite (Boehmite) is also known as
Boehmite or boehmite, chemical formula are γ-Al2O3·H2O or γ-AlOOH.γ-AlOOH is by many AlO6Octahedral
What body was constituted, Al is in octahedra center, and O is on octahedra vertex, and octahedron is by coplanar formation double-strand, then vertex forms three-dimensional altogether
Skeleton structure.γ-AlOOH belong to rhombic system layer structure, and with its unique mechanics, chemistry, optical property ceramic material,
Optical material, semiconductor material, composite material, catalyst and carrier material and paint field are used widely, and are especially existed
Field of lithium ion battery has been widely used.
In the prior art, the preparation method of boehmite is relatively more, mainly includes the precipitation method (acid, alkali precipitation), carbonizatin method, alcohol
Aluminum water solution, hydro-thermal method, sol-gel method, ionic liquid method, hard template method etc..Especially to use aluminium salt and urea etc. for raw material,
Being most widely used for ultra-fine boehmite powder is prepared using hydrothermal process.But the above method is typically only capable to obtain ultra-fine grain diameter
Sheet boehmite will affect the conductivity of ion when preparing lithium ion battery separator, and further influence the permeability of diaphragm
With lithium ion battery passability, it is unfavorable for the raising of performance of lithium ion battery.
Summary of the invention
For this purpose, being suitable for preparing coating of lithium-ion battery diaphragm technical problem to be solved by the present invention lies in one kind is provided
Porous flake boehmite；
Second technical problem to be solved by this invention is to provide the preparation method of above-mentioned porous flake boehmite.
In order to solve the above technical problems, a kind of preparation method of porous flake boehmite of the present invention, including it is as follows
Step:
(1) aluminium salt material is taken to prepare to obtain aluminum salt solution, it is spare；
(2) Adjunct humectants are added in Xiang Suoshu aluminum salt solution, mix；
(3) continue that pore creating material is added into the aluminum salt solution, mix；
(4) continue to be added auxiliary agent into the aluminum salt solution to adjust material liquid pH to alkalinity, obtain presoma feed liquid；
(5) by gained presoma feed liquid in 150-250 DEG C of progress hydrothermal synthesis reaction；
(6) after the completion of hydro-thermal reaction, gained slurry is settled and is discharged supernatant, through spraying dry after settled slurry is washed
Dry processing is to get required porous flake boehmite powder.
Specifically, in the preparation method of the porous flake boehmite, in the step (1):
The aluminium salt material includes at least one of aluminium chloride, aluminum nitrate, aluminum sulfate；
In the aluminum salt solution, Al is controlled3+Concentration is 0.2-0.6mol/L.
Specifically, in the preparation method of the porous flake boehmite, in the step (2):
The Adjunct humectants include polyvinylpyrrolidone, N- ethyl pyrrolidone, n-vinyl pyrrolidone or N-
At least one of octylpyrrolidone；
In the aluminum salt solution, the addition concentration for controlling the Adjunct humectants is 0.2-0.5g/L.
Specifically, in the preparation method of the porous flake boehmite, in the step (3):
The pore creating material include polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO-PEO) triblock copolymer and/
Or polyoxyethylene polyoxypropylene block copolymer；
In the aluminum salt solution, the pore creating material and the Al are controlled3+Molar concentration rate be 0.01-0.05:100.
Specifically, in the preparation method of the porous flake boehmite, in the step (4):
The auxiliary agent includes at least one of urea, ammonium hydroxide or aluminium hydroxide.
In the step (4), the pH value for adjusting the presoma feed liquid is 7-11.
In the step (4), further include the steps that the presoma feed liquid, which is heated to 60-80 DEG C, to be mixed.
In the step (5), the heating rate for controlling the hydrothermal synthesis step is 1-5 DEG C/min.
In the step (6), the washing step is to add water washing, and preferably repeatedly washed.
The invention also discloses the porous flake boehmites being prepared by the method.
Flake porous boehmite of the present invention is to pass through addition using aluminium salts such as aluminium chloride, aluminum nitrate, aluminum sulfate as raw material
Polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO-PEO) triblock copolymer and/or polyoxyethylene polyoxypropylene block
Copolymer adds polyvinylpyrrolidone, N- ethyl pyrrolidone, n-vinyl pyrrolidone and/or N- as pore creating material
Octylpyrrolidone is prepared as Adjunct humectants through high temperature hydrothermal process, and the boehmite is with porous structure
Sheet boehmite material.The porous structure of the flake porous boehmite is suitable for lithium battery diaphragm coating and uses, and can effectively mention
The aperture of high battery diaphragm and porosity, and resistance can be reduced and improve ionic conductivity, help to improve the logical of battery diaphragm
Permeability and lithium ion battery passability.
The preparation method of flake porous boehmite of the present invention, by screening and adding pore creating material and wetting agent,
Porous flake boehmite is formed under 150-250 DEG C of hydrothermal condition, entire preparation process is simple and easy, and raw material is easy to get, and molten
Agent system is uniformly dispersed, and helps to improve the through performance of lithium ion battery separator.Flake porous boehmite of the present invention
It, can be in favor of the shape of the evenly dispersed and pore structure of pore creating material by preparing boehmite presoma at 60-80 DEG C in preparation method
At, cause gathering and being segregated for pore creating material so as to avoid temperature difference, can effectively in presoma pore creating material dispersion.
Detailed description of the invention
In order to make the content of the present invention more clearly understood, it below according to specific embodiments of the present invention and combines
Attached drawing, the present invention is described in further detail, wherein
Fig. 1 is the scanning electron microscope (SEM) photograph that boehmite powder S-1 is made in embodiment 1；
Fig. 2 is the X-ray diffractogram that boehmite powder S-1 is made in embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph that boehmite powder S-2 is made in embodiment 2；
Fig. 4 is the X-ray diffractogram that boehmite powder S-2 is made in embodiment 2；
Fig. 5 is the scanning electron microscope (SEM) photograph that boehmite powder S-3 is made in embodiment 3；
Fig. 6 is the X-ray diffractogram that boehmite powder S-3 is made in embodiment 3；
Fig. 7 is the scanning electron microscope (SEM) photograph that boehmite powder S-4 is made in embodiment 4；
Fig. 8 is the X-ray diffractogram that boehmite powder S-4 is made in embodiment 4.
Specific embodiment
Embodiment 1
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 66.64g aluminum sulfate and (analyzes pure, Al2(SO4)3·18H2O it) is added in 1000g deionized water, and
Aluminum salt solution is made in heating stirring, spare；
(2) polyvinylpyrrolidone (K 30) 0.25g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO- is added
PEO) triblock copolymer (molecular weight 3000-10000) 0.2g is mixed；
(4) it continues up to state and appropriate aluminium hydroxide is added in aluminum salt solution obtained to adjust the pH value 8.5 of solution, and
In adition process, heating is opened, controls 65 DEG C of solution temperature, speed of agitator 60r/min is stirred 30min, obtains presoma
Feed liquid；
(5) the presoma feed liquid obtained is transferred in autoclave, control compactedness is 60%, control reaction
Kettle heating rate is 2 DEG C/min, until holding temperature is 180 DEG C of progress hydrothermal synthesis reactions, soaking time 10h, water-heat process
Open stirring, mixing speed 60r/min；
(6) after the completion of the hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed
It washs, control amount of water is 10 times for settling weight of material, and after continuous washing 2 times, sedimentation material is carried out spray drying treatment, can
It obtains for the flake porous boehmite powder S-1 of lithium battery diaphragm coating.
The scanning electron microscope (SEM) photograph that the boehmite powder S-1 is made in the present embodiment is as shown in Fig. 1, the boehmite powder S-
1 X-ray diffractogram is as shown in Figure 2.
Embodiment 2
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 72.5g aluminium chloride and (analyzes pure, AlCl3·6H2O it) is added in 1000g deionized water, and heats and stir
It mixes, aluminum salt solution is made, it is spare；
(2) polyvinylpyrrolidone (K 30) 0.45g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO- is added
PEO) triblock copolymer (molecular weight 3000-10000) 0.25g is mixed；
(4) it continues up to state in aluminum salt solution obtained and appropriate aluminium hydroxide is added to adjust solution ph as 10, and
In adition process, heating is opened, controls 80 DEG C of solution temperature, speed of agitator 120r/min, 20min is stirred, obtains presoma material
Liquid；
(5) gained presoma feed liquid is transferred in autoclave, control compactedness is 60%, reaction kettle heating rate
For 2 DEG C/min, until reaching holding temperature for 220 DEG C of progress hydrothermal synthesis reactions, soaking time 20h, water-heat process unlatching is stirred
It mixes, mixing speed 120r/min；
(6) after the completion of hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed,
10 times that amount of water is example weight are controlled, after continuously washing 3 times, material spray drying treatment will be settled, can obtain being used for lithium
The flake porous boehmite powder S-2 of battery diaphragm coating.
The scanning electron microscope (SEM) photograph that the boehmite powder S-2 is made in the present embodiment is as shown in Fig. 3, the boehmite powder S-
2 X-ray diffractogram is as shown in Figure 4.
Embodiment 3
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 187.5g aluminum nitrate and (analyzes pure, Al (NO4)3·9H2O it) is added in 1000g deionized water, and adds
Aluminum salt solution is made in thermal agitation, spare；
(2) addition polyvinylpyrrolidone (K 30) 0.5g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO- is added
PEO) triblock copolymer (molecular weight 3000-10000) 0.3g is mixed；
(4) it continues up to state in aluminum salt solution obtained and appropriate aluminium hydroxide is added to adjust solution ph as 8.5, and
In adition process, heating is opened, controls 80 DEG C of solution temperature, speed of agitator 60r/min, 30min is stirred, obtains presoma material
Liquid；
(5) the obtained presoma feed liquid is transferred in autoclave, control compactedness is 80%, heating rate
For 5 DEG C/min, until reaching Europe holding temperature for 220 DEG C of progress hydrothermal synthesis reactions, soaking time 20h, water-heat process is opened
Stirring, mixing speed 60r/min；
(6) after to hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed,
10 times that amount of water is example weight are controlled, after continuously washing 5 times, material spray drying treatment will be settled, can obtain being used for lithium
The flake porous boehmite powder S-3 of battery diaphragm coating.
The scanning electron microscope (SEM) photograph that the boehmite powder S-3 is made in the present embodiment is as shown in Fig. 5, the boehmite powder S-
3 X-ray diffractogram is as shown in Figure 6.
Embodiment 4
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 66.64g aluminum sulfate and (analyzes pure, Al2(SO4)3·18H2O) and 24.2g aluminium chloride (analysis it is pure,
AlCl3·6H2O it) is mixed to join in 1000g deionized water, and heating stirring, aluminum salt solution is made, it is spare；
(2) polyvinylpyrrolidone (K 30) 0.25g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO- is added
PEO) triblock copolymer (molecular weight 3000-10000) 0.2g is mixed；
(4) it continues up to state in aluminum salt solution obtained and appropriate aluminium hydroxide is added to adjust solution ph as 11, and
In adition process, heating is opened, controls 70 DEG C of solution temperature, speed of agitator 60r/min, 30min is stirred, obtains presoma material
Liquid；
(5) obtained presoma feed liquid is transferred in autoclave, control compactedness is 60%, reaction kettle heating speed
Degree is 2 DEG C/min, until reaching holding temperature is 180 DEG C, carries out hydrothermal synthesis reaction, soaking time 10h, water-heat process is opened
Stirring, mixing speed 60r/min；
(6) after to hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed,
10 times that amount of water is example weight are controlled, after continuously washing 2 times, sediment slurry material spray drying treatment can be used
In the flake porous boehmite powder S-4 of lithium battery diaphragm coating.
The scanning electron microscope (SEM) photograph that the boehmite powder S-4 is made in the present embodiment is as shown in Fig. 7, the boehmite powder S-
4 X-ray diffractogram is as shown in Figure 8.
Embodiment 5
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 72.5g aluminium chloride and (analyzes pure, AlCl3·6H2O it) is added in 1000g deionized water, and heats and stir
It mixes, aluminum salt solution is made, it is spare；
(2) N- ethyl pyrrolidone 0.45g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO- is added
PEO) triblock copolymer (molecular weight 3000-10000) 0.25g is mixed；
(4) it continues up to state in aluminum salt solution obtained and appropriate aluminium hydroxide is added to adjust solution ph as 10, and
In adition process, heating is opened, controls 80 DEG C of solution temperature, speed of agitator 120r/min, 20min is stirred, obtains presoma material
Liquid；
(5) gained presoma feed liquid is transferred in autoclave, control compactedness is 60%, reaction kettle heating rate
For 2 DEG C/min, until reaching holding temperature for 150 DEG C of progress hydrothermal synthesis reactions, soaking time 20h, water-heat process unlatching is stirred
It mixes, mixing speed 120r/min；
(6) after the completion of hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed,
10 times that amount of water is example weight are controlled, after continuously washing 3 times, material spray drying treatment will be settled, can obtain being used for lithium
Battery diaphragm is coated with flake porous boehmite powder.
Embodiment 6
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 72.5g aluminium chloride and (analyzes pure, AlCl3·6H2O it) is added in 1000g deionized water, and heats and stir
It mixes, aluminum salt solution is made, it is spare；
(2) n-vinyl pyrrolidone 0.45g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO- is added
PEO) triblock copolymer (molecular weight 3000-10000) 0.25g is mixed；
(4) it continues up to state in aluminum salt solution obtained and appropriate aluminium hydroxide is added to adjust solution ph as 10, and
In adition process, heating is opened, controls 80 DEG C of solution temperature, speed of agitator 120r/min, 20min is stirred, obtains presoma material
Liquid；
(5) gained presoma feed liquid is transferred in autoclave, control compactedness is 60%, reaction kettle heating rate
For 2 DEG C/min, until reaching holding temperature for 250 DEG C of progress hydrothermal synthesis reactions, soaking time 20h, water-heat process unlatching is stirred
It mixes, mixing speed 120r/min；
(6) after the completion of hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed,
10 times that amount of water is example weight are controlled, after continuously washing 3 times, material spray drying treatment will be settled, can obtain being used for lithium
Battery diaphragm is coated with flake porous boehmite powder.
Embodiment 7
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 72.5g aluminium chloride and (analyzes pure, AlCl3·6H2O it) is added in 1000g deionized water, and heats and stir
It mixes, aluminum salt solution is made, it is spare；
(2) n-octylpyrrolidone 0.45g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO- is added
PEO) triblock copolymer (molecular weight 3000-10000) 0.25g is mixed；
(4) it continues up to state in aluminum salt solution obtained and appropriate aluminium hydroxide is added to adjust solution ph as 10, and
In adition process, heating is opened, controls 80 DEG C of solution temperature, speed of agitator 120r/min, 20min is stirred, obtains presoma material
Liquid；
(5) gained presoma feed liquid is transferred in autoclave, control compactedness is 60%, reaction kettle heating rate
For 2 DEG C/min, until reaching holding temperature for 220 DEG C of progress hydrothermal synthesis reactions, soaking time 20h, water-heat process unlatching is stirred
It mixes, mixing speed 120r/min；
(6) after the completion of hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed,
10 times that amount of water is example weight are controlled, after continuously washing 3 times, material spray drying treatment will be settled, can obtain being used for lithium
Battery diaphragm is coated with flake porous boehmite powder.
Embodiment 8
The preparation method of porous flake boehmite, includes the following steps: described in the present embodiment
(1) it weighs 72.5g aluminium chloride and (analyzes pure, AlCl3·6H2O it) is added in 1000g deionized water, and heats and stir
It mixes, aluminum salt solution is made, it is spare；
(2) n-octylpyrrolidone 0.45g is added into aluminum salt solution obtained above, mixes；
(3) it continues up to state in aluminum salt solution obtained and polyoxyethylene polyoxypropylene block copolymer (molecular weight is added
3000-10000) 0.25g is mixed；
(4) it continues up to state in aluminum salt solution obtained and appropriate aluminium hydroxide is added to adjust solution ph as 10, and
In adition process, heating is opened, controls 80 DEG C of solution temperature, speed of agitator 120r/min, 20min is stirred, obtains presoma material
Liquid；
(5) gained presoma feed liquid is transferred in autoclave, control compactedness is 60%, reaction kettle heating rate
For 2 DEG C/min, until reaching holding temperature for 220 DEG C of progress hydrothermal synthesis reactions, soaking time 20h, water-heat process unlatching is stirred
It mixes, mixing speed 120r/min；
(6) after the completion of hydrothermal synthesis reaction, supernatant is discharged after gained slurry is settled 2h, and water is added to be washed,
10 times that amount of water is example weight are controlled, after continuously washing 3 times, material spray drying treatment will be settled, can obtain being used for lithium
Battery diaphragm is coated with flake porous boehmite powder.Experimental example
The flake porous boehmite powder sample for taking above-described embodiment 1-4 to be prepared into respectively is detected, measurement
Its specific surface and size distribution comparative situation, and result is recorded in the following table 1.
1 embodiment of the present invention of table, 1,2,3,4 sample specific surface and size distribution comparison.
By upper table data it is found that the boehmite of the method for the present invention preparation is laminated structure, there is even particle size distribution and ratio
The big advantage in surface, the preparation suitable for cell coating diaphragm.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of preparation method of porous flake boehmite, which comprises the steps of:
(1) aluminium salt material is taken to prepare to obtain aluminum salt solution, it is spare；
(2) Adjunct humectants are added in Xiang Suoshu aluminum salt solution, mix；
(3) continue that pore creating material is added into the aluminum salt solution, mix；
(4) continue to be added auxiliary agent into the aluminum salt solution to adjust material liquid pH to alkalinity, obtain presoma feed liquid；
(5) by gained presoma feed liquid in 150-250 DEG C of progress hydrothermal synthesis reaction；
(6) after the completion of hydro-thermal reaction, gained slurry is settled and is discharged supernatant, after settled slurry is washed through spray drying at
Reason is to get required porous flake boehmite powder.
2. the preparation method of porous flake boehmite according to claim 1, which is characterized in that in the step (1):
The aluminium salt material includes at least one of aluminium chloride, aluminum nitrate, aluminum sulfate；
In the aluminum salt solution, Al is controlled3+Concentration is 0.2-0.6mol/L.
3. the preparation method of porous flake boehmite according to claim 1 or 2, which is characterized in that the step (2)
In:
The Adjunct humectants include polyvinylpyrrolidone, N- ethyl pyrrolidone, n-vinyl pyrrolidone or N- octyl
At least one of pyrrolidones；
In the aluminum salt solution, the addition concentration for controlling the Adjunct humectants is 0.2-0.5g/L.
4. the preparation method of porous flake boehmite according to claim 1-3, which is characterized in that the step
(3) in:
The pore creating material includes polyoxyethylene/polyoxypropylene/polyoxyethylene (PEO-PPO-PEO) triblock copolymer and/or gathers
Ethylene oxide polyoxypropylene block copolymers；
In the aluminum salt solution, the pore creating material and the Al are controlled3+Molar concentration rate be 0.01-0.05:100.
5. the preparation method of porous flake boehmite according to claim 1-4, which is characterized in that the step
(4) in, the auxiliary agent includes at least one of urea, ammonium hydroxide or aluminium hydroxide.
6. the preparation method of porous flake boehmite according to claim 1-5, which is characterized in that the step
(4) in, the pH value for adjusting the presoma feed liquid is 7-11.
7. the preparation method of porous flake boehmite according to claim 1-6, which is characterized in that the step
(4) in, further include the steps that the presoma feed liquid, which is heated to 60-80 DEG C, to be mixed.
8. the preparation method of porous flake boehmite according to claim 1-7, which is characterized in that the step
(5) in, the heating rate for controlling the hydrothermal synthesis step is 1-5 DEG C/min.
9. the preparation method of porous flake boehmite according to claim 1-8, which is characterized in that the step
(6) in, the washing step is to add water washing.
10. the porous flake boehmite being prepared by any one of claim 1-9 the method.
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| CN113371747A (en) * | 2021-06-11 | 2021-09-10 | 中铝郑州有色金属研究院有限公司 | Preparation method of boehmite with sheet structure and application of boehmite |
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| CN104192880A (en) * | 2014-07-18 | 2014-12-10 | 大连理工大学 | Method for preparing high-purity pseudo-boehmite |
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| CN113371747A (en) * | 2021-06-11 | 2021-09-10 | 中铝郑州有色金属研究院有限公司 | Preparation method of boehmite with sheet structure and application of boehmite |
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