CN107572568A - A kind of preparation method of micron-size spherical alumina powder - Google Patents
A kind of preparation method of micron-size spherical alumina powder Download PDFInfo
- Publication number
- CN107572568A CN107572568A CN201710987998.2A CN201710987998A CN107572568A CN 107572568 A CN107572568 A CN 107572568A CN 201710987998 A CN201710987998 A CN 201710987998A CN 107572568 A CN107572568 A CN 107572568A
- Authority
- CN
- China
- Prior art keywords
- micron
- preparation
- alumina powder
- spherical alumina
- size spherical
- 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.)
- Granted
Links
Abstract
The invention discloses a kind of preparation method of micron-size spherical alumina powder, comprise the following steps that：Certain density aluminum nitrate aqueous solution is prepared, adds ethanol, glycerine and oleic acid, it is still aging at a certain temperature after being uniformly mixed；Atomization process is carried out by ultrasonic atomizer；Atomization vapour is brought into high temperature process furnances with compressed gas carries out heat resolve；Then the sample after pyrolysis is absorbed with deionized water, is finally centrifuged sample, washed, drying, that is, obtain described ball-aluminium oxide.For the aluminum oxide of this method synthesis for a few micrometers grades of perfections are spherical, uniform particle sizes, simple production process is economic and environment-friendly, is adapted to the application in catalytic field and isolation technics etc..
Description
Technical field
The present invention relates to a kind of preparation method of aluminum oxide, and in particular to a kind of preparation of micron-size spherical alumina powder
Method.
Background technology
It is all that the application of inorganic functional material aluminum oxide is related to ceramics, electronics, adsorbing separation, environmental protection and catalytic reaction etc.
More important field.The physical parameters such as crystal phase structure, crystallite dimension and the pattern of aluminum oxide be applied to performance have it is most important
Influence.Therefore, the growth of crystal phase structure is controlled, obtains the aluminum oxide of specific morphology（Such as sheet, bar-shaped, fibrous and ball
Shape etc.）Cause the interest of numerous researchers, the particularly aluminum oxide with spherical structure, because it has high mechanical strength, biography
The characteristics such as matter is good, is evenly distributed and gain great popularity.It can be obtained from nanometer to millimetre-sized various chis using different preparation methods
Very little ball-aluminium oxide.Water column, oil column or the oil ammonia column method of forming can prepare 1~3 millimeter of alumina balls（Chinese patent CN
106745125A, CN 101549287A, CN 1068975A）；It is spray-dried by predecessor of Alumina gel, then passes through high temperature
Roasting, 10~200 microns of alumina balls can be obtained（Chinese patent CN 1631787A）.Chinese patent CN 106865587A will
Inorganic aluminate, surfactant and precipitating reagent, which are dissolved in solvent, forms solution, passes through in water heating kettle at 120~200 DEG C of heat
Reason, the aluminum oxide micro-sphere of 1~10 micron of diameter can be obtained.Chinese patent CN 101214984A, CN 1169720A and text
Offer（Yang, W. et al., J. Am. Ceram. Soc. 2008, 91, 2732.）Using organic silicon source in incendiary agent
Effect is lower to carry out the alumina balls that high temperature pyrolysis prepares a diameter of 0.05~0.5 microns.
Aluminum oxide with a few micrometers of sizes has ten in the catalytic field and separation technology field of fluidized-bed reactor
Divide significant application value.However, in the method for above-mentioned synthesizing micron-grade ball-aluminium oxide, some needs use the organo-aluminium of costliness
Reagent is as raw material so that production cost is too high；Some need to prepare the Alumina gel with specific composition as silicon source so that raw
Production process is excessively cumbersome；Some synthesis need to carry out in high-pressure bottle, substantially increase the safe class of production；Some synthesis
Need to add substantial amounts of incendiary agent, and at extreme temperatures（Such as：More than more than 1000 DEG C）Reacted so that in generating process
Produce a large amount of ammonia nitrogens and other waste gas.
The content of the invention
It is an object of the invention to for above-mentioned the deficiencies in the prior art, there is provided one kind prepares a few micrometers of sizes, perfect ball
The preparation method of the alumina powder of shape structure and uniform particle sizes.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of micron-size spherical alumina powder, comprises the following steps：
（1）Aluminum nitrate is dissolved in the deionized water that its weight multiple is 2~10 times, then adds ethanol, glycerine and oleic acid, stirring
Solution after well mixed stands 2~12 hours at 30~50 DEG C；
（2）By step（1）Obtained mixed liquor pours into and atomization process is carried out in ultrasonic atomizer, and atomization rates are 10~20mL/
H, form atomization vapour；
（3）Air is passed through step with air compressor（2）In described ultrasonic atomizer, the atomization vapour taken out of is directly entered height
Warm tube furnace carries out heat resolve；
（4）The sample after pyrolysis is absorbed with deionized water；
（5）The sample that collection obtains is centrifuged, washed, drying, obtains described ball-aluminium oxide.
Step（1）Described aluminum nitrate is ANN aluminium nitrate nonahydrate.
Step（1）In, the aluminum nitrate, ethanol, the mass ratio of glycerine and oleic acid are 1:0.001~0.1:0.001~0.05:
0.001~0.05。
Step（2）The droplet size that the ultrasonic atomizer is atomized the atomization vapour to be formed is 0.5~40 micron.
Step（3）Described air inlet pressure is 0.05~0.5MPa, and air mass flow is 0.4 ~ 0.5m3/h。
Step（3）The temperature of the heat resolve is 900 ~ 950 DEG C, and the heat resolve time is 1 ~ 10s.
The present invention compared with prior art, has advantages below and beneficial effect：
Raw material sources of the present invention are easy, cheap；Simple production process；It is economic and environment-friendly.The oxygen of this method synthesis
Change the perfect spherical, uniform particle sizes that aluminium is a few micrometers grades.
Brief description of the drawings
Fig. 1 is the SEM photograph for the ball-aluminium oxide powder that the embodiment of the present invention 1 synthesizes；
Fig. 2 be the embodiment of the present invention it is 2-in-1 into ball-aluminium oxide powder SEM photograph.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
8 grams of ANN aluminium nitrate nonahydrates are dissolved in 18 grams of deionized waters, then add 0.6 gram of ethanol, 0.4 gram of glycerine and 0.1 gram of oil
Acid, the solution after being uniformly mixed stand 4 hours at 40 DEG C.Above-mentioned mixed liquor is poured into ultrasonic atomizer and carried out at atomization
Reason, atomization rates 15mL/h, form atomization vapour.0.1MPa air is passed through atomizer, air mass flow with air compressor
For 0.4m3/ h, the atomization vapour taken out of are directly entered the quartz glass tube that internal diameter is 100mm, carry out heat resolve, quartz glass tube
It is placed in 950 DEG C of high temperature process furnances, the heat resolve time is 4s, and the isothermal region of high temperature process furnances is more than 10cm.Use deionization
Water absorbs the sample after pyrolysis.The sample being collected into finally is subjected to centrifuge washing 2 times with deionized water, obtained solid exists
120 DEG C dry 12 hours, that is, obtain ball-aluminium oxide.
Embodiment 2
75 grams of ANN aluminium nitrate nonahydrates are dissolved in 200 grams of deionized waters, 5 grams of ethanol, 3 grams of glycerine and 2 grams of oleic acid is then added, stirs
Mix the solution after being well mixed and stand 2 hours at 50 DEG C.Above-mentioned mixed liquor is poured into atomization process, mist are carried out in ultrasonic atomizer
Change speed is 20mL/h, forms atomization vapour.0.1MPa air is passed through atomizer with air compressor, air mass flow is
0.5m3/ h, the atomization vapour taken out of are directly entered the quartz glass tube that internal diameter is 100mm, carry out heat resolve, and quartz glass tube is put
In in 900 DEG C of high temperature process furnances, the heat resolve time is 3s, and the isothermal region of high temperature process furnances is more than 10cm.Use deionized water
Absorb the sample after pyrolysis.The sample being collected into finally is subjected to centrifuge washing 2 times with deionized water, obtained solid is 120
DEG C drying 12 hours, that is, obtain ball-aluminium oxide.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (6)
- A kind of 1. preparation method of micron-size spherical alumina powder, it is characterised in that：Comprise the following steps：（1）Aluminum nitrate is dissolved in the deionized water that its weight multiple is 2~10 times, then adds ethanol, glycerine and oleic acid, stirring Solution after well mixed stands 2~12 hours at 30~50 DEG C；（2）By step（1）Obtained mixed liquor pours into and atomization process is carried out in ultrasonic atomizer, and atomization rates are 10~20mL/ H, form atomization vapour；（3）Air is passed through step with air compressor（2）In described ultrasonic atomizer, the atomization vapour taken out of is directly entered height Warm tube furnace carries out heat resolve；（4）The sample after pyrolysis is absorbed with deionized water；（5）The sample that collection obtains is centrifuged, washed, drying, obtains described ball-aluminium oxide.
- 2. the preparation method of micron-size spherical alumina powder according to claim 1, it is characterised in that：Step（1）Institute The aluminum nitrate stated is ANN aluminium nitrate nonahydrate.
- 3. the preparation method of micron-size spherical alumina powder according to claim 1, it is characterised in that：Step（1）In, The aluminum nitrate, ethanol, the mass ratio of glycerine and oleic acid are 1:0.001~0.1:0.001~0.05:0.001~0.05.
- 4. the preparation method of micron-size spherical alumina powder according to claim 1, it is characterised in that：Step（2）Institute State ultrasonic atomizer be atomized the atomization vapour to be formed droplet size be 0.5~40 micron.
- 5. the preparation method of micron-size spherical alumina powder according to claim 1, it is characterised in that：Step（3）Institute The air inlet pressure stated is 0.05~0.5MPa, and air mass flow is 0.4 ~ 0.5m3/h。
- 6. the preparation method of micron-size spherical alumina powder according to claim 1, it is characterised in that：Step（3）Institute The temperature for stating heat resolve is 900 ~ 950 DEG C, and the heat resolve time is 1 ~ 10s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710987998.2A CN107572568B (en) | 2017-10-21 | 2017-10-21 | A kind of preparation method of micron-size spherical alumina powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710987998.2A CN107572568B (en) | 2017-10-21 | 2017-10-21 | A kind of preparation method of micron-size spherical alumina powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107572568A true CN107572568A (en) | 2018-01-12 |
| CN107572568B CN107572568B (en) | 2019-09-13 |
Family
ID=61037976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710987998.2A Active CN107572568B (en) | 2017-10-21 | 2017-10-21 | A kind of preparation method of micron-size spherical alumina powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107572568B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110314001A (en) * | 2018-03-30 | 2019-10-11 | 株式会社松风 | Zirconium oxide assigns liquid with opacity |
| EP3575277A1 (en) * | 2018-03-30 | 2019-12-04 | Shofu Inc. | Opaque imparting liquid for zirconia |
| CN110745851A (en) * | 2019-09-20 | 2020-02-04 | 天津理工大学 | Spherical alpha-alumina fire retardant and preparation method thereof |
| CN112499602A (en) * | 2020-12-02 | 2021-03-16 | 天津泽希新材料有限公司 | Preparation method of spherical micron-sized aluminum nitride powder |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040932A (en) * | 1988-09-08 | 1990-04-04 | 清华大学 | Ultrasonic atomizing preparation of superfine powder |
| JP2003089519A (en) * | 2001-09-13 | 2003-03-28 | Yazaki Corp | Apparatus for producing alumina hollow particle |
| US20040265221A1 (en) * | 2003-04-17 | 2004-12-30 | Yazaki Corporation | Method of producing hollow alumina particle |
| JP2009023888A (en) * | 2007-07-23 | 2009-02-05 | Kansai Electric Power Co Inc:The | Method for producing spherical alumina particle |
| CN104591240A (en) * | 2015-01-09 | 2015-05-06 | 辽阳领跃科技有限公司 | Preparation technology of spherical alumina powder |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
-
2017
- 2017-10-21 CN CN201710987998.2A patent/CN107572568B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040932A (en) * | 1988-09-08 | 1990-04-04 | 清华大学 | Ultrasonic atomizing preparation of superfine powder |
| JP2003089519A (en) * | 2001-09-13 | 2003-03-28 | Yazaki Corp | Apparatus for producing alumina hollow particle |
| US20040265221A1 (en) * | 2003-04-17 | 2004-12-30 | Yazaki Corporation | Method of producing hollow alumina particle |
| JP2009023888A (en) * | 2007-07-23 | 2009-02-05 | Kansai Electric Power Co Inc:The | Method for producing spherical alumina particle |
| CN104591240A (en) * | 2015-01-09 | 2015-05-06 | 辽阳领跃科技有限公司 | Preparation technology of spherical alumina powder |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
Non-Patent Citations (3)
| Title |
|---|
| V.JOKANOVIC等: "Synthesis and Formation Mechanism of Ultrafine Spherical Al2O3 Powders by Ultrasonic Spay Pyrolysis", 《MATERIALS TRANSACTIONS》 * |
| 戴遐明: "喷雾热解-一种重要的微粉制备工艺", 《粉体技术》 * |
| 王龙: "氯化铝溶液直接喷雾热解制取氧化铝及物性表征", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110314001A (en) * | 2018-03-30 | 2019-10-11 | 株式会社松风 | Zirconium oxide assigns liquid with opacity |
| EP3575277A1 (en) * | 2018-03-30 | 2019-12-04 | Shofu Inc. | Opaque imparting liquid for zirconia |
| CN110314001B (en) * | 2018-03-30 | 2022-05-10 | 株式会社松风 | Opacity imparting liquid for zirconium oxide |
| US11622840B2 (en) | 2018-03-30 | 2023-04-11 | Shofu Inc. | Opaque imparting liquid for zirconia |
| CN110745851A (en) * | 2019-09-20 | 2020-02-04 | 天津理工大学 | Spherical alpha-alumina fire retardant and preparation method thereof |
| CN112499602A (en) * | 2020-12-02 | 2021-03-16 | 天津泽希新材料有限公司 | Preparation method of spherical micron-sized aluminum nitride powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107572568B (en) | 2019-09-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107572568B (en) | A kind of preparation method of micron-size spherical alumina powder | |
| CN101618869B (en) | Method for preparing small-size meso-porous hollow carbon sphere | |
| CN103738969B (en) | Mesoporous silica and preparation method thereof | |
| Luo et al. | Rapid synthesis and characterization of ambient pressure dried monolithic silica aerogels in ethanol/water co-solvent system | |
| CN106082317B (en) | A kind of preparation method of hollow hemisphere titanium dioxide | |
| CN104003409B (en) | A kind of preparation method of controlled monodisperse spherical Large stone nano silicon | |
| CN107098353B (en) | flower-shaped silicon dioxide balls and preparation method thereof | |
| CN105502342A (en) | Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source | |
| CN106732722A (en) | A kind of preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure | |
| CN105175781B (en) | The silicon dioxide modified carbon nanotube rod-like nano composite material of organic spherical shape and preparation method | |
| CN107617437A (en) | A kind of ruthenium carried titanium dioxide hollow ball embeds Nano particles of silicon dioxide catalyst and its preparation method and application | |
| CN101475179B (en) | Preparation of organic-inorganic hybridization silicon oxide nanosphere | |
| CN102674379B (en) | Hollow mesoporous silicon dioxide nano particles and method for preparing same | |
| CN103433032A (en) | WO3@mSiO2 microballoon sphere with nuclear shell hollow structure as well as preparation method and application thereof | |
| CN104147986A (en) | Long-chain-thioether-bond-containing mesoporous organic-inorganic hybrid ball of core-hollow-shell structure and preparation method thereof | |
| CN102020283A (en) | Preparation method of silicon dioxide nano hollow sphere with adjustable inner diameter | |
| CN109734102A (en) | The preparation method and its preparation facilities of silica micron ball | |
| CN111252772A (en) | Method for adjusting aperture of silicon dioxide | |
| CN106009346A (en) | Preparation method of monodisperse silica microspheres | |
| CN113651336A (en) | Silica microspheres and preparation method thereof | |
| US9296935B2 (en) | Micro particle for thermal control material and device and method of producing the same using ultrasonic high-temperature vibration scheme | |
| CN103288093B (en) | Method for preparing hollow silicon oxide microspheres by spray drying | |
| CN102755880B (en) | Method for preparing high-purity silica packing through sol-gel process | |
| CN107892289A (en) | A kind of method for preparing monodisperse mesoporous carbosphere | |
| CN108822302B (en) | Janus nano-particle and preparation method and application thereof |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |