CN107529518B - A kind of preparation method of superfine alumina powder - Google Patents
A kind of preparation method of superfine alumina powder Download PDFInfo
- Publication number
- CN107529518B CN107529518B CN201710951141.5A CN201710951141A CN107529518B CN 107529518 B CN107529518 B CN 107529518B CN 201710951141 A CN201710951141 A CN 201710951141A CN 107529518 B CN107529518 B CN 107529518B
- Authority
- CN
- China
- Prior art keywords
- alumina
- preparation
- dispersing agent
- slurry
- particle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention provides a kind of preparation methods of ultra-fine alumina, comprising the following steps: (1) roughly grinds in the presence of the first dispersing agent to alumina slurry；(2) alumina slurry through roughly grinding is filtered；(3) fine grinding is carried out to filtered alumina slurry in the presence of the second dispersing agent；(4) finely ground alumina slurry is dried and is crushed, first dispersing agent is ammonium polyacrylate, and second dispersing agent is the mixture of polyacrylic acid and ammonium polyacrylate.The present invention also provides the lithium ion battery separator coatings or electrode coating by the preparation-obtained superfine alumina powder of the preparation method, and comprising the Ultrafine High-purity Alumina powder.
Description
Technical field
This invention relates generally to aluminium oxide fields, more particularly to a kind of superfine alumina powder preparation method.It is described
Not only partial size is small for superfine alumina powder, but also particle size dispersion is narrow, easy dispersion, and has high purity.
Background technique
The attention of great attention with the whole world to energy environment protection, electric car and energy storage system by height, and
The superiority of lithium ion battery becomes the first choice of power system of electric automobile.But the use of lithium battery, which still remains many, asks
Topic, most allow people's worry is exactly safety problem.
It, can be by alumina coated on diaphragm coating in order to effectively improve the safety of lithium battery.But the technology pair
Alumina powder itself it is more demanding, for example, having strictly to the partial size of alumina powder, specific surface area, apparent density etc.
Requirement, dispersibility of the alumina powder on diaphragm coating is required especially harsh.
Therefore, in order to obtaining the aluminium oxide granule for being suitable for use in diaphragm coating, particularly lithium ion battery separator coating
Grain, there is an urgent need to a kind of improved alumina powder preparation techniques.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of improved ultra-fine alumina, by the ultra-fine of this method preparation
Aluminium oxide have desired property, especially partial size, particle diameter distribution, dispersibility, in terms of, be especially suitable for
Diaphragm coating in the battery of lithium ion.
In the first aspect of the present invention, the preparation method of ultra-fine alumina is provided, comprising the following steps:
(1) alumina slurry is roughly ground in the presence of the first dispersing agent；
(2) alumina slurry through roughly grinding is filtered；
(3) fine grinding is carried out to filtered alumina slurry in the presence of the second dispersing agent；
(4) finely ground alumina slurry is dried and is crushed,
First dispersing agent is ammonium polyacrylate, and second dispersing agent is the mixing of polyacrylic acid and ammonium polyacrylate
Object.
In preferred preparation method, in the second dispersing agent, the mass ratio of polyacrylic acid and ammonium polyacrylate is 99:1
To 1:99, preferably 2:1-1:2.Polyacrylic acid and polyacrylic acid in particularly advantageous embodiment, in the second dispersing agent
The mass ratio of ammonium is 1:(0.8-1.5), such as 1:1 or 1:1.2.
In a further preferred embodiment, the dosage of first dispersing agent is alumina particle total weight
0.1%-1%.In a further preferred embodiment, the dosage of second dispersing agent is alumina particle total weight
0.1%-1%.
As dispersing agent used in the present invention, the weight average molecular weight that polyacrylic acid preferably has is about 2000-10000,
The weight average molecular weight that ammonium polyacrylate preferably has is about 2000-10000.
Superfine alumina powder preparation method of the invention is generally directed to conventional in the market alumina powder or aluminium oxide
Slurry.Under normal circumstances, the average grain diameter of alumina particle therein is substantially at 10 μm or less.It is understandable to be, it is thinner
Alumina particle is more favorable, such as average grain diameter is at 8 μm or even 5um or less.
In the case where particularly advantageous, in (1) step, with the zirconium oxide bead of diameter 4.0mm -7.0mm to oxidation aluminium paste
Material corase grinding certain time, preferably from about 2-4 hours.In (3) step, with the zirconium oxide bead of diameter 0.8mm-2mm to oxidation aluminium paste
Expect fine grinding for a period of time, preferably from about 1-3 hours.
In the preparation process in accordance with the present invention, the alumina particle in alumina slurry is mainly Alpha-alumina, and purity has
It is greater than the Alpha-alumina of 99.9%, preferably greater than 99.99% sharply.
The present invention also further provides a kind of superfine alumina powder in second aspect, particularly by being sent out according to this
It is obtained prepared by bright preparation method.Particle size range D10 >=0.2 μm of the superfine alumina powder, 0.45 μm≤D50≤1.0 μ
M, D90≤3.0 μm, D99≤6.0 μm, specific surface area 4.0-9.0m2/ g, pH are between 6.5-9.0, tap density 1.0-
1.35g/cm3。
Since superfine alumina powder of the invention has excellent disperse properties, particularly suitable for lithium-ion electric
Pond diaphragm coating or electrode coating.
Detailed description of the invention
Fig. 1 and 2: the stereoscan photograph and grain of the alumina particle as raw material not yet ground according to the method for the present invention
Distribution map (before grinding) is spent, wherein serious reunion has occurred in particle；
Fig. 3 and 4: according to embodiments of the present invention 4 ground after stereoscan photograph and particle size distribution figure.It can send out
Existing, basic disappearance of reuniting, the dispersibility of alumina particle is significantly improved.
Specific embodiment
The present invention will be described with regard to some specific embodiments below.
For the raw material in preparation method of the invention, i.e., initial alumina slurry can be commercially available conventional oxygen
Change aluminium powder body.It is industrial largely to prepare alumina powder usually using method for calcinating.But such alumina powder prepares work
Skill is difficult to prepare the alumina powder haveing excellent performance.The requirement for especially facing increasingly strict battery performance, to aluminium oxide
Particle diameter distribution and dispersibility of powder etc. are proposed increasingly higher demands.And the present invention only by adjusting grinding the step of
And relevant parameter, it will be able to significantly improve the performances such as particle diameter distribution and the dispersibility of alumina powder.Advantageously, as raw material
Alumina powder, there is average grain diameter less than 10 μm.Particle in common alumina powder is usually at normal distribution.Cause
This, the alumina powder that can be used for preparation method of the present invention advantageously has following particle diameter distribution: D10≤0.80μm,D50
≤2.5μm,D90≤5.5μm,D99≤10.0μm.According to the method for the present invention, by grinding (either corase grinding or fine grinding)
Afterwards, particle still retains normal distribution, but distribution curve can be optimized.
The term " alumina slurry " used in this application refers to the suspension of alumina particle in water.
The preparation method of ultra-fine alumina according to the present invention, including two key steps: corase grinding and fine grinding.Can first by
Alumina particle and water are hybridly prepared into alumina slurry, then prepared alumina slurry is added to the kibbling mill of corase grinding
In.It can also directly be separately added into alumina particle and water into kibbling mill, form alumina slurry in kibbling mill.
The purpose of corase grinding mainly breaks up the bulky grain reunited in powder together as far as possible, so as to ensure to demonstrate,prove D99
It is qualified.Zirconium oxide bead (being hereafter also referred to as zirconium pearl) can be used when corase grinding as abrasive media, preferably diameter 4.0mm-
The zirconium pearl of 7.0mm, particularly 5.0mm-5.5mm.
In rough grinding pass, needs into abrasive media, dispersing agent is added into kibbling mill.Point that the corase grinding stage uses
Powder is known as " the first dispersing agent ".Dispersing agent can be the inclined sodium of six phosphoric acid, polyacrylic acid, ammonium polyacrylate or their times
One combination.The additive amount of dispersing agent can be 0.1%-1%, the preferably 0.4-0.7% of alumina particle total weight, particularly preferably
About 0.5%.It can be added at one time, the first dispersing agent can also be added with portioning.
The time roughly ground to alumina slurry is preferably controlled in 2-4 hours.The corase grinding time is too short, then the group of not can guarantee
Poly- particle is broken up, and roughly grinds overlong time, can cause soft-agglomerated while increase energy consumption.
Broken zirconium pearl fragment may be mixed with by roughly grinding in obtained alumina slurry, and therefore, it is necessary to filter out zirconium pearl
After fragment in being transferred to atomizer mill.The strainer with appropriate mesh can be used for example to be filtered.It can also be according to specific item
Part uses other filter types.
Also zirconium pearl can be used in fine grinding as abrasive media.Zirconium bead diameter used in fine grinding is less than used in corase grinding
Zirconium bead diameter.It is preferable to use be diameter be less than 2mm, such as 0.8mm -2mm zirconium pearl.It is particularly preferably used in the fine grinding stage
It is the zirconium pearl of 1 ± 0.2mm of diameter.
During fine grinding, it is also desirable into abrasive media, dispersing agent be added into atomizer mill.The fine grinding stage uses
Dispersing agent is known as " the second dispersing agent ".Dispersing agent can for the inclined sodium of six phosphoric acid, polyacrylic acid, ammonium polyacrylate or they
Any combination.The additive amount of dispersing agent can be the 0.1%-1%, preferably 0.4-0.7% of alumina particle total weight, especially excellent
Choosing about 0.5%.It can be added at one time, the second dispersing agent can also be added with portioning.Preferably portioning gradually adds the second dispersion
Agent.For example, the second dispersing agent can be added with per half an hour, as long as guaranteeing that the total amount of the dispersing agent of addition is alumina particle gross weight
The 0.1%-1% of amount.
The time that alumina slurry carries out fine grinding is needed to control at 1-3 hours, preferably 1.5-2.5 hours, most preferably
It is 2 hours.The time of fine grinding is too short or too long, all not can guarantee alumina particle partial size and meets technical requirement.
According to the present invention, the first dispersing agent in corase grinding may be the same or different with the second dispersing agent in fine grinding.
In preparation method specifically preferred according to the invention, the first dispersing agent is ammonium polyacrylate, and the second dispersing agent is polyacrylic acid and gathers
The mixture of ammonium acrylate.Present inventors have surprisingly found that the first dispersing agent is poly- third in the technique for preparing ultra-fine alumina
When olefin(e) acid ammonium and the second dispersing agent are the mixture of polyacrylic acid and ammonium polyacrylate, it can be prepared in partial size, partial size point
The all satisfactory superfine alumina powder of cloth, dispersibility, specific surface area etc..In a further preferred embodiment,
The mass ratio of polyacrylic acid and ammonium polyacrylate is 99:1 to 1:99, preferably 1:10 to 10:1 in second dispersing agent.For example, second
The mass ratio of polyacrylic acid and ammonium polyacrylate can be 1:5 to 5:1 in dispersing agent.In particularly preferred embodiments,
The mass ratio of polyacrylic acid and ammonium polyacrylate can be 1:2 to 2:1, such as 1:(0.8-1.5 in two dispersing agents), it especially can be with
For 1:1 or 1:1.2.
The polyacrylic acid and ammonium polyacrylate being used in the present invention are generally the conventional polyacrylic acid for being used as dispersing agent
And ammonium polyacrylate.For example, the weight average molecular weight of polyacrylic acid can be about 2000-10000, smaller or larger Weight-average molecular
Amount is also feasible.The weight average molecular weight of preferred polyacrylic acid is about 3000-8000, more preferably no more than about 5000.Poly- third
The weight average molecular weight of olefin(e) acid ammonium can be about 2000-10000, and smaller or larger weight average molecular weight is also feasible.Preferably
The weight average molecular weight of ammonium polyacrylate is about 3000-8000, more preferably no more than about 5000.
It is understood that when the second dispersing agent is the mixture of polyacrylic acid and ammonium polyacrylate, second dispersion
Both substances in agent dividually can also be added individually, only need to guarantee that additive amount meets aforementioned proportion.
The drying of alumina slurry experience, the crushing obtained after fine grinding, results in superfine alumina powder.
It is uniformly dispersed according to the alumina powder that the above method is prepared.Partial size have following distribution, D10 >=0.2 μm,
0.45 μm≤D50≤1.0 μm, D90≤3.0 μm, D99≤6.0 μm.The specific surface area of alumina particle is 4.0-9.0m2/ g, pH
6.5-9.0 tap density 1.0-1.35g/cm3。
Particularly, in the preparation process in accordance with the present invention, it is preferable to use purity is greater than 99.99% alpha aluminium oxide particle conduct
Raw material.The alumina particle that preparation method according to the present invention obtains does not introduce new impurity, so products obtained therefrom is also
Purity is greater than 99.99% alpha aluminium oxide particle, and has above-mentioned excellent performance in terms of particle diameter distribution, dispersibility.
The yield of the preparation method of Ultrafine High-purity Alumina according to the present invention not only final products is high, in the whole process
Substantially it is not lost, and product is entirely qualified, yield rate is even greater than 99%.Also basic no three wastes produces in process of production simultaneously
It is raw.The final particle diameter distribution for obtaining aluminium oxide granule granule product is narrow, and D50 can be between 0.45-1.0 μm.
And aluminium oxide granule granule product according to the present invention is since partial size is thin, particle diameter distribution is narrow, and dispersibility is very good etc., and has
There are suitable specific surface area, pH value, tap density etc., so the electrode or diaphragm of lithium battery can be coated fairly evenly, has
Improve to effect the safety of lithium ion battery.Therefore, alumina particle according to the present invention or prepared according to the methods of the invention
Alumina particle be especially suitable for the diaphragm of lithium ion battery or the coating of electrode.
Embodiment
The present invention will be described further with regard to following embodiment, however, it should be noted that the embodiment is only to illustrate it
With, and it is not necessarily to be construed as limitation of the present invention.The inclined sodium of six phosphoric acid, polyacrylic acid and ammonium polyacrylate used in embodiment
Commercially available acquisition.
In the examples below,
Polyacrylic acid: molecular weight 5000 or so, one Chemical Co., Ltd. of Weifang Shandong, trade mark RY9500, solid content >=
50%；
Ammonium polyacrylate: molecular weight 5000 or so, one Chemical Co., Ltd. of Weifang Shandong, trade mark RY9527, solid content >=
40%.
The scanned photograph of the used pure alpha-aluminum oxide particle (purity 99.99%) as raw material as shown in Figure 1, from
It can be found that serious reunion has occurred in the alumina particle in photo.The partial size of alumina particle is measured, initial grain
Diameter distribution meets following require: D10≤0.80μm,D50≤2.5μm,D90≤5.5μm,D99≤10.0μm.Raw alumina is swept
Retouch electromicroscopic photograph and particle size distribution figure difference referring to Fig. 1 and Fig. 2.
Embodiment 1:
Then 800-1000g deionized water is added in the zirconium pearl that 4kg diameter 5.3mm is added into kibbling mill, then weigh on 1kg
It states the pure alpha-aluminum oxide that purity is 99.99% to be added thereto, opens stirring, be added account for pure alpha-aluminum oxide quality by several times
The inclined sodium of 0.5% [5g] six phosphoric acid carries out surface and is modified, and after 30r/min revolving speed ball milling 3 hours, stops stirring, slurry crosses 100
Mesh filter screen is transferred to atomizer mill, zirconium pearl diameter 1mm in atomizer mill, quality 1kg, continues ball milling with the revolving speed of 2000r/min, per half
It is 0.5%[5g that hour portioning, which is added and accounts for pure alpha-aluminum oxide quality ,] the inclined sodium of six phosphoric acid, ball milling 2h, by the drying of gained slurry,
Crushing obtains alumina powder.
Claim powder obtained by 40g in colorimetric cylinder, 60g deionized water is added, shake up 5min, stands 48h, observation sedimentation feelings
Condition.
Gained powder data: D10 is 0.347 μm, and D50 is 2.016 μm, and D90 is 4.567 μm, and D99 is 8.367 μm, compares table
Area is 9.5m2/ g, pH 10.3, tap density 1.24g/cm3；Powder is sunk to the bottom completely after 48h, poor dispersion.
Embodiment 2:
Then 800-1000g deionized water is added in the zirconium pearl that 4kg diameter 5.3mm is added into kibbling mill, then weigh on 1kg
It states the pure alpha-aluminum oxide that purity is 99.99% to be added thereto, opens stirring, be added account for pure alpha-aluminum oxide quality by several times
0.5%[5g] polyacrylic acid to carry out surface modified, after 30r/min revolving speed ball milling 3 hours, stop stirring, slurry crosses 100 mesh
Strainer is transferred to atomizer mill, zirconium pearl diameter 1mm in atomizer mill, quality 1kg, continues ball milling with the revolving speed of 2000r/min, every half is small
When portioning be added account for pure alpha-aluminum oxide quality be 0.5%[5g] polyacrylic acid, ball milling 2h, by gained slurry drying, crush
Obtain alumina powder.
Claim powder obtained by 40g in colorimetric cylinder, 60g deionized water is added, shake up 5min, stands 48h, observation sedimentation feelings
Condition.
Gained powder data: D10 is 0.324 μm, and D50 is 1.023 μm, and D90 is 2.141 μm, and D99 is 6.03 μm, compares table
Area is 7.4m2/ g, pH 5.43, tap density 0.96g/cm3；Powder is sunk to the bottom substantially after 48h, poor dispersion.
Embodiment 3:
Then 800-1000g deionized water is added in the zirconium pearl that 4kg diameter 5.3mm is added into kibbling mill, then weigh on 1kg
It states the pure alpha-aluminum oxide that purity is 99.99% to be added thereto, opens stirring, be added account for pure alpha-aluminum oxide quality by several times
0.5%[5g] ammonium polyacrylate to carry out surface modified, after 30r/min revolving speed ball milling 3 hours, stop stirring, slurry crosses 100
Mesh filter screen is transferred to atomizer mill, zirconium pearl diameter 1mm in atomizer mill, quality 1kg, continues ball milling with the revolving speed of 2000r/min, per half
Hour portioning is added and accounts for pure alpha-aluminum oxide quality 0.5%[5g] ammonium polyacrylate, ball milling 2h, by the drying of gained slurry, powder
It is broken to obtain alumina powder.
Claim powder obtained by 40g in colorimetric cylinder, 60g deionized water is added, shake up 5min, stands 48h, observation sedimentation feelings
Condition.
Gained powder data: D10 is 0.243 μm, and D50 is 1.036 μm, and D90 is 2.697 μm, and D99 is 5.42 μm, compares table
Area is 7.6m2/ g, pH 8.9, tap density 1.06g/cm3；There is obvious layering in powder after 48h, and dispersibility is general.
Embodiment 4:
Then 800-1000g deionized water is added in the zirconium pearl that 4kg diameter 5.3mm is added into kibbling mill, then weigh on 1kg
It states the pure alpha-aluminum oxide that purity is 99.99% to be added thereto, opens stirring, be added account for pure alpha-aluminum oxide quality by several times
0.5%[5g] ammonium polyacrylate to carry out surface modified, after 30r/min revolving speed ball milling 3 hours, stop stirring, slurry crosses 100
Mesh filter screen is transferred to atomizer mill, zirconium pearl diameter 1mm in atomizer mill, quality 1kg, continues ball milling with the revolving speed of 2000r/min, per half
Hour portioning is added and accounts for pure alpha-aluminum oxide quality 0.5%[5g] polyacrylic acid and ammonium polyacrylate (mass ratio 1:1.2)
The drying of gained slurry, crushing are obtained alumina powder by mixture, ball milling 2h.
Claim powder obtained by 40g in colorimetric cylinder, 60g deionized water is added, shake up 5min, stands 48h, observation sedimentation feelings
Condition.
Gained powder data: D10 is 0.451 μm, and D50 is 0.888 μm, and D90 is 1.586 μm, and D99 is 2.501 μm, compares table
Area is 7.6m2/ g, pH 7.4, tap density 1.15g/cm3；Obviously being layered does not occur in powder after 48h, good dispersion.It should
The stereoscan photograph and particle size distribution figure of powder are respectively referring to Fig. 3 and Fig. 4.
Embodiment 5:
Then 800-1000g deionized water is added in the zirconium pearl that 4kg diameter 5.3mm is added into kibbling mill, then weigh on 1kg
It states the pure alpha-aluminum oxide that purity is 99.99% to be added thereto, opens stirring, be added account for pure alpha-aluminum oxide quality by several times
0.5%[5g] ammonium polyacrylate to carry out surface modified, after 30r/min revolving speed ball milling 3 hours, stop stirring, slurry crosses 100
Mesh filter screen is transferred to atomizer mill, zirconium pearl diameter 1mm in atomizer mill, quality 1kg, continues ball milling with the revolving speed of 2000r/min, per half
Hour portioning is added and accounts for pure alpha-aluminum oxide quality 0.5%[5g] polyacrylic acid and ammonium polyacrylate (mass ratio 1:1.2)
The drying of gained slurry, crushing are obtained alumina powder by mixture, ball milling 1.5h.
Claim powder obtained by 40g in colorimetric cylinder, 60g deionized water is added, shake up 5min, stands 48h, observation sedimentation feelings
Condition.
Gained powder data: D10 is 0.347 μm, and D50 is 0.883 μm, and D90 is 2.951 μm, and D99 is 4.063 μm, compares table
Area is 8.0m2/ g, pH 7.5, tap density 1.08g/cm3；Obviously being layered does not occur in powder after 48h, favorable dispersibility.
Embodiment 6:
Then 800-1000g deionized water is added in the zirconium pearl that 4kg diameter 5.3mm is added into kibbling mill, then weigh on 1kg
It states the pure alpha-aluminum oxide that purity is 99.99% to be added thereto, opens stirring, be added account for pure alpha-aluminum oxide quality by several times
0.5%[5g] ammonium polyacrylate to carry out surface modified, after 30r/min revolving speed ball milling 3 hours, stop stirring, slurry crosses 100
Mesh filter screen is transferred to atomizer mill, zirconium pearl diameter 1mm in atomizer mill, quality 1kg, continues ball milling with the revolving speed of 2000r/min, per half
Hour portioning is added and accounts for pure alpha-aluminum oxide quality 0.5%[5g] polyacrylic acid and ammonium polyacrylate (mass ratio 1:1.2)
The drying of gained slurry, crushing are obtained alumina powder by mixture, ball milling 2.5h.
Claim powder obtained by 40g in colorimetric cylinder, 60g deionized water is added, shake up 5min, stands 48h, observation sedimentation feelings
Condition.
Gained powder data: D10 is 0.351 μm, and D50 is 0.762 μm, and D90 is 1.586 μm, and D99 is 3.656 μm, compares table
Area is 7.8m2/ g, pH 7.6, tap density 1.24g/cm3；Obviously being layered does not occur in powder after 48h, favorable dispersibility.
Content documented by above, only several embodiments to realize the present invention, without this should and cannot be limited with this
The practical range of invention.It is all according to simple equivalence changes made by claims of the present invention and patent specification content with repair
Decorations, still remain within the scope of the patent.
Claims (10)
1. a kind of preparation method of ultra-fine alumina, comprising the following steps:
(1) alumina slurry is roughly ground in the presence of the first dispersing agent；
(2) alumina slurry through roughly grinding is filtered；
(3) fine grinding is carried out to filtered alumina slurry in the presence of the second dispersing agent；
(4) finely ground alumina slurry is dried and is crushed,
Wherein first dispersing agent is ammonium polyacrylate,
Second dispersing agent is the mixture of polyacrylic acid and ammonium polyacrylate, wherein the matter of polyacrylic acid and ammonium polyacrylate
Amount ratio is 2:1-1:2,
Wherein in (1) step, alumina slurry is roughly ground 2-4 hours with the zirconium oxide bead of diameter 4.0mm -7.0mm；
In (3) step, with the zirconium oxide bead of diameter 0.8mm-2mm to alumina slurry fine grinding 1-3 hours.
2. preparation method according to claim 1, wherein in the second dispersing agent, the matter of polyacrylic acid and ammonium polyacrylate
Amount is than being 1:(0.8-1.5).
3. preparation method according to claim 1, wherein the dosage of first dispersing agent is alumina particle total weight
0.1%-1%.
4. preparation method according to claim 1, wherein the dosage of second dispersing agent is alumina particle total weight
0.1%-1%.
5. preparation method according to claim 1, wherein the weight average molecular weight of polyacrylic acid is about 2000-10000, poly- third
The weight average molecular weight of olefin(e) acid ammonium is about 2000-10000.
6. preparation method according to claim 1, wherein in alumina slurry before corase grinding alumina particle average grain
Diameter is at 10 μm or less.
7. preparation method according to claim 1, wherein the alumina particle in alumina slurry is greater than for purity
99.9% Alpha-alumina.
8. preparation method according to claim 1, wherein the alumina particle in alumina slurry is greater than for purity
99.99% Alpha-alumina.
9. by the preparation-obtained superfine alumina powder of the preparation method of any one of claim 1-8, wherein described ultra-fine
Particle size range D10 >=0.2 μm of alumina powder, 0.45 μm≤D50≤1.0 μm, D90≤3.0 μm, table is compared in D99≤6.0 μm
Area is 4.0-9.0m2/ g, pH are between 6.5-9.0, tap density 1.0-1.35g/cm3。
10. lithium ion battery separator coating or electrode coating, it includes the Ultrafine High-purity Alumina powders of claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710951141.5A CN107529518B (en) | 2017-10-13 | 2017-10-13 | A kind of preparation method of superfine alumina powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710951141.5A CN107529518B (en) | 2017-10-13 | 2017-10-13 | A kind of preparation method of superfine alumina powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107529518A CN107529518A (en) | 2018-01-02 |
| CN107529518B true CN107529518B (en) | 2019-05-31 |
Family
ID=60766306
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710951141.5A Active CN107529518B (en) | 2017-10-13 | 2017-10-13 | A kind of preparation method of superfine alumina powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107529518B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516782A (en) * | 2018-10-25 | 2019-03-26 | 建德华明高纳新材料有限公司 | Lithium battery ceramic diaphragm easy dispersed alumina and preparation method thereof |
| CN109336148A (en) * | 2018-11-21 | 2019-02-15 | 方复(上海)新材料科技有限公司 | Lithium battery ceramic diaphragm coating aluminium oxide and preparation method thereof |
| CN111732421A (en) * | 2020-05-25 | 2020-10-02 | 浙江爱科新材料有限公司 | Preparation method of alumina ceramic composite powder |
| CN111995404A (en) * | 2020-08-27 | 2020-11-27 | 建德华明高纳新材料有限公司 | Superfine alumina for lithium battery ceramic diaphragm and preparation method thereof |
| CN112158867A (en) * | 2020-09-07 | 2021-01-01 | 美轲（广州）化学股份有限公司 | Alumina slurry and preparation method and application thereof |
| CN112876263A (en) * | 2021-02-01 | 2021-06-01 | 江苏厚生新能源科技有限公司 | High-specific-surface-area ceramic powder, preparation method thereof and high-liquid-retention-capacity ceramic diaphragm |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092381A (en) * | 1993-03-08 | 1994-09-21 | 圣戈本/诺顿工业塘瓷有限公司 | tabular alumina |
| CN101824279A (en) * | 2010-05-10 | 2010-09-08 | 上海高纳粉体技术有限公司 | High accuracy aluminum oxide polishing powder and production method thereof |
| CN102522557A (en) * | 2011-10-24 | 2012-06-27 | 连云港连连化学有限公司 | Preparation method for high-purity ultrathin easily-dispersible aluminum oxide for lithium ion battery |
| CN102602968A (en) * | 2012-03-30 | 2012-07-25 | 山东晶鑫晶体科技有限公司 | Method for producing alumina powder used for plasma display panel (PDP) fluorescent powder |
| CN103553098A (en) * | 2013-11-10 | 2014-02-05 | 襄阳市金控特种陶瓷科技有限公司 | Preparation method of alpha aluminum oxide micro-fine crystal powder |
| CN104163446A (en) * | 2014-09-05 | 2014-11-26 | 沈阳工业大学 | Preparation method of micron-sized spherical alumina supporter |
| CN104229844A (en) * | 2014-09-12 | 2014-12-24 | 广西平果铝朗琨科技有限公司 | Preparation method of superfine low-sodium alpha-alumina powder with high activity |
| CN104446509A (en) * | 2014-10-23 | 2015-03-25 | 江苏金石研磨有限公司 | Preparation method of submicron aluminum oxide superfine powder by virtue of cascade grinding |
| CN104787787A (en) * | 2015-02-16 | 2015-07-22 | 青海圣诺光电科技有限公司 | Method for preparing ultra-micro alumina powder by using mechanical crushing |
| CN105347778A (en) * | 2015-10-13 | 2016-02-24 | 刘冠华 | Preparation method for high-purity ultrafine alumina used for lithium battery ceramic diaphragm |
| CN105753023A (en) * | 2016-02-29 | 2016-07-13 | 雅安百图高新材料有限公司 | Method for preparing superfine low-sodium alphas-phase aluminum oxide through silica sol coating |
| CN106281221A (en) * | 2016-04-26 | 2017-01-04 | 福吉米株式会社 | Grinding-material, composition for polishing and Ginding process |
| CN106784529A (en) * | 2016-12-27 | 2017-05-31 | 深圳中兴创新材料技术有限公司 | A kind of lithium ion battery separator and preparation method thereof |
| CN106810214A (en) * | 2017-01-05 | 2017-06-09 | 中北大学 | A kind of preparation method of high strength and low cost alumina ceramic substrate used for electronic packaging |
-
2017
- 2017-10-13 CN CN201710951141.5A patent/CN107529518B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092381A (en) * | 1993-03-08 | 1994-09-21 | 圣戈本/诺顿工业塘瓷有限公司 | tabular alumina |
| CN101824279A (en) * | 2010-05-10 | 2010-09-08 | 上海高纳粉体技术有限公司 | High accuracy aluminum oxide polishing powder and production method thereof |
| CN102522557A (en) * | 2011-10-24 | 2012-06-27 | 连云港连连化学有限公司 | Preparation method for high-purity ultrathin easily-dispersible aluminum oxide for lithium ion battery |
| CN102602968A (en) * | 2012-03-30 | 2012-07-25 | 山东晶鑫晶体科技有限公司 | Method for producing alumina powder used for plasma display panel (PDP) fluorescent powder |
| CN103553098A (en) * | 2013-11-10 | 2014-02-05 | 襄阳市金控特种陶瓷科技有限公司 | Preparation method of alpha aluminum oxide micro-fine crystal powder |
| CN104163446A (en) * | 2014-09-05 | 2014-11-26 | 沈阳工业大学 | Preparation method of micron-sized spherical alumina supporter |
| CN104229844A (en) * | 2014-09-12 | 2014-12-24 | 广西平果铝朗琨科技有限公司 | Preparation method of superfine low-sodium alpha-alumina powder with high activity |
| CN104446509A (en) * | 2014-10-23 | 2015-03-25 | 江苏金石研磨有限公司 | Preparation method of submicron aluminum oxide superfine powder by virtue of cascade grinding |
| CN104787787A (en) * | 2015-02-16 | 2015-07-22 | 青海圣诺光电科技有限公司 | Method for preparing ultra-micro alumina powder by using mechanical crushing |
| CN105347778A (en) * | 2015-10-13 | 2016-02-24 | 刘冠华 | Preparation method for high-purity ultrafine alumina used for lithium battery ceramic diaphragm |
| CN105753023A (en) * | 2016-02-29 | 2016-07-13 | 雅安百图高新材料有限公司 | Method for preparing superfine low-sodium alphas-phase aluminum oxide through silica sol coating |
| CN106281221A (en) * | 2016-04-26 | 2017-01-04 | 福吉米株式会社 | Grinding-material, composition for polishing and Ginding process |
| CN106784529A (en) * | 2016-12-27 | 2017-05-31 | 深圳中兴创新材料技术有限公司 | A kind of lithium ion battery separator and preparation method thereof |
| CN106810214A (en) * | 2017-01-05 | 2017-06-09 | 中北大学 | A kind of preparation method of high strength and low cost alumina ceramic substrate used for electronic packaging |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107529518A (en) | 2018-01-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107529518B (en) | A kind of preparation method of superfine alumina powder | |
| CN106082993B (en) | A method of preparing high-performance ITO pelletizing | |
| CN104592789B (en) | A kind of preparation method of flame retardant of magnesium hydroxide | |
| CN101500943B (en) | Zirconium oxide and method for the production thereof | |
| JP5415215B2 (en) | Magnesium oxide powder having excellent dispersibility and method for producing the same | |
| CN101284983B (en) | Superfine and spheroidizing rare-earth polish and preparing process thereof | |
| TWI582055B (en) | Ultra fine milk of lime composition | |
| CN104300119B (en) | A kind of preparation method of lithium iron phosphate positive material | |
| CN110534719B (en) | Preparation method of aluminum-doped magnesium-nickel-manganese spherical cobaltosic oxide | |
| TWI401211B (en) | Indium oxide powder and method for producing same | |
| CN107585768B (en) | Method for preparing superfine tungsten carbide powder by oxidation-reduction method | |
| JPH10182150A (en) | Ito stock powder and sintered compact and their production | |
| CN112408439B (en) | Method for preparing superfine magnesium hydroxide for flame retardant by using magnesium hydroxide coarse powder as raw material | |
| CN107971502A (en) | A kind of preparation method of high dispersiveness spherical silver powder | |
| CN113620328B (en) | Preparation method of nano alumina seed crystal and preparation method of high-purity alumina nanocrystalline | |
| EP3006403A1 (en) | Lithium titanate, production method for same, and electrical storage device employing same | |
| CN108640677A (en) | A kind of nano composite oxides zirconium powder preparation that crystallite dimension is controllable | |
| CN105732010A (en) | High-flexibility 95 ceramic and preparation method thereof | |
| CN107758751B (en) | A kind of preparation method of resistance slurry ruthenic oxide | |
| CN113023789A (en) | Olive-type carbonate ternary precursor with large specific surface area and preparation method thereof | |
| CN111072375A (en) | Preparation method of aluminum oxide grinding balls | |
| CN113060748B (en) | Submicron boehmite and preparation method | |
| CN102079950A (en) | Preparation method of monodisperse rare earth polishing powder | |
| CN106698501B (en) | A kind of preparation method of lithium titanate with spinel structure | |
| JP3324164B2 (en) | Indium oxide powder, method for producing the same, and method for producing ITO sintered body |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20190321 Address after: 315000 No. 7 024 Block 108, Qingyi Road, Ningbo High-tech Zone, Zhejiang Province Applicant after: Zhejiang Aike New Materials Co., Ltd. Address before: 222228 Lingang Industrial Zone, Guanyun County, Lianyungang City, Jiangsu Province Applicant before: Jiangsu chemical Limited by Share Ltd |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A preparation method of ultrafine alumina powder Effective date of registration: 20210602 Granted publication date: 20190531 Pledgee: Ningbo Tongshang Bank Co.,Ltd. Pledgor: Zhejiang Aike New Materials Co.,Ltd. Registration number: Y2021330000501 |