CN100469699C - Method for the treatment of aluminum oxide powder - Google Patents
Method for the treatment of aluminum oxide powder Download PDFInfo
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- CN100469699C CN100469699C CNB2005101120228A CN200510112022A CN100469699C CN 100469699 C CN100469699 C CN 100469699C CN B2005101120228 A CNB2005101120228 A CN B2005101120228A CN 200510112022 A CN200510112022 A CN 200510112022A CN 100469699 C CN100469699 C CN 100469699C
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Abstract
The invention relates to a method for treating alumina oxide powder. It comprises following steps: preparing powder pretreating liquid, adding alumina oxide powder, stirring mechanically to mix slurry, distributing with supersonic wave at the same time, the pretreating time is more than 30 minutes, drying slurry after the powder is thoroughly treated and getting dried powder. The invention is characterized in that it adds alumina oxide into acid treating liquid and achieves higher activity for raw material powder.
Description
Technical field
The invention belongs to the preparation and the process field of powder body material, be specifically related to a kind ofly to alumina powder jointed treatment process, the activity by this kind method material powder can increase substantially; Simultaneously, the treatment process of this powder is also applicable to other micro nano powders.
Background technology
The aluminum oxide output of China occupies the first in the world, but also has very big gap in preparation alumina powder jointed field of high quality high-performance and international most advanced level.This gap mainly shows the powder handling process aspect.The level of hardware of China's powder preparing industry can with abroad compare, but caused alumina powder jointed performance quality of China and external gap in the gap of concrete powder handling process aspect.
In addition, because powder raw material is the basis of preparation high-performance block materials, the performance of powder raw material has often determined the development and the use of block materials.If the powder of high-temperature point has had higher activity energy, just can be at lower temperature spot sintering, thereby widened the sintering range of this kind powder body material, this has very big meaning for some matrix material, for the research and development of advanced composite material preparation provides more optional space.Simultaneously, powder body material has higher activity energy, can reduce sintering temperature and reduce sintering time, thereby help saving the energy and production cost.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art existence and a kind of method that makes the more highly active treatment of aluminum oxide powder of material powder acquisition is provided.
Purpose of the present invention can be achieved through the following technical solutions: a kind of method of treatment of aluminum oxide powder, it is characterized in that, this method may further comprise the steps: allotment powder pretreatment fluid, sneak into the alumina raw material powder, mechanical stirring mixes slurry, simultaneously can be equipped with ultrasonic dispersing, pretreatment time is greater than 30 minutes, treats that powder fully handles the after drying slurry and obtain dry powder.
Described powder pretreatment fluid concocting method is as follows: remove ionized water, add acid, mix.
The deionized water quality of described use is less than the quality of pretreating raw material powder.
Described acid comprises and is selected from one or more mixtures in mineral acid, high price small molecular weight organic acid, the polyelectrolyte organic acid.
Described mineral acid comprises nitric acid, phosphoric acid, carbonic acid, hydrochloric acid, and described high price small molecular weight organic acid comprises citric acid, 2-phosphonic acids butane-1,2, the 4-tricarboxylic acid, and described polyelectrolyte organic acid comprises polyacrylic acid, polymethyl acrylic acid.
The usage quantity of described mineral acid is advisable less than 3 with the pretreatment fluid pH value, and described high price small molecular weight organic acid usage quantity and polyelectrolyte organic acid usage quantity are that the benchmark conversion is greater than 100ppm with pretreated raw material powder quality.
The ultrasonic frequency that described ultrasonic dispersing is used is 500～2000KHz.
The method that the dispersed alumina powder granule of reunion is separated in the acquisition of described acid solution washing aluminum oxide powder also can replace water or organic solvent washing nano alumina powder in the preparation process of nano alumina powder, obtain to separate the nano alumina powder preferably of reuniting.
Compared with prior art, the present invention proposes to utilize acid to alumina powder jointed particulate effect, alumina raw material powder is sneaked in the ready pickling agent, thereby make material powder obtain higher activity.Wherein, high price small molecular weight organic acid action effect is the most remarkable, and active raising has the greatest impact for powder sintering.Wherein active raising is improvement to the powder granule pattern to mineral acid for powder sintering.Wherein active raising is to the improvement of powder granule pattern with to the depolymerization of material powder cluster of grains aggressiveness high price small molecular weight organic acid for powder sintering for the active raising of powder sintering and polyelectrolyte organic acid, and it is separated collecting process and comprises the soft-agglomerated depolymerization of material powder particle and the depolymerization of part hard aggregation.Wherein said raw material powder purity, granularity are not limit, but raw material powder purity is high more, granularity is more little, and the effect of powder pretreatment process is good more, and the powder active after the processing is high more.Wherein said alumina powder jointed treatment process and in the preparation process of nano alumina powder role, also be applicable to the processing and the preparation of other nano-powders.
Embodiment
Below in conjunction with concrete treatment process and embodiment, the invention will be further described.
A kind of alumina powder jointed treatment process of the present invention, concrete processing step is as follows:
(1) allotment powder pretreatment fluid:
Remove ionized water, the water yield is relevant with the purity and the granularity of pre-treatment powder, and the deionized water quality of described use is advisable less than the quality of pretreating raw material powder; Add acid of the present invention, acid and deionized water are mixed, the usage quantity of wherein said mineral acid is advisable less than 3 with the pretreatment fluid pH value, and high price small molecular weight organic acid usage quantity and polyelectrolyte organic acid usage quantity are that the benchmark conversion is advisable greater than 100ppm with pretreated raw material powder quality.
(2) add alumina raw material powder:
The raw material powder add-on, with respect to the mixed slurry of water and powder, the volume percent of powder is to be advisable less than 55vol%; After sneaking into alumina raw material powder, the mixed slurry of water and powder can leave standstill processing, and the treatment time was greater than 6 hours; Suitable mechanical stirring can make slurry mix, and churning time is to be advisable less than time of repose, and the treatment time was greater than 3 hours; If be equipped with ultrasonic dispersing simultaneously, ultrasonic wave should intermittently be used, and avoids the slurry heating to be advisable, and the ultrasonic frequency that ultrasonic dispersing is used is 500-2000KHz, and the treatment time is greater than 30min.
(3) treat that powder fully handles the after drying slurry, mechanical mill can obtain exsiccant high reactivity powder.
Process for making for nano alumina powder, alumina powder jointed treatment process of the present invention, can replace water or organic solvent washing nano alumina powder in manufacturing process, obtain to separate the nano alumina powder preferably of reuniting, its step can suitably be simplified to adapt to concrete production technique.
For the processing and the preparation of other nano-powders, powder handling method of the present invention also can be used, but in the concrete steps usage quantity of acid and treatment time according to different material powder and different.
Embodiment 1
Raw materials used as follows:
High purity aluminium oxide powder (Al
2O
3Purity 〉=99.99wt%), trade mark LM2-N214, Dalian Luming Nanometer Material Co., Ltd. provides;
Citric acid (chemical pure), Shanghai chemical reagents corporation provides;
Magnesium nitrate (analytical pure), Shanghai chemical reagents corporation provides;
Deionized water, water factory of Fudan University.
Raw materials used proportioning is as follows:
Deionized water and aluminum oxide powder add by weight 1:1, and citric acid adding amount is basic 0.5wt% with aluminum oxide powder.Raw material powder treatment process: remove ionized water, add citric acid, stir, add pretreated aluminum oxide powder and adopt the manual machinery stirring that mixed slurry is mixed, leave standstill 6 hours treatment times with glass stick.
Performance comparison experimental program before and after raw material powder is handled: compare experiment with pure zirconia aluminium powder and the powder mix that adds the 0.1wt%MgO sintering aid respectively with two kinds of powders before and after handling.The sample forming method adopts the 200MPaCIP moulding, synthermal sintering in vacuum oven, the volume density of survey sintered specimen.
The contrast test result is as follows:
By data in the last table as can be seen, the powder sintering activity of handling has significantly raising, under identical sintered density, and low about 100 ℃ of more former sintering temperature.
Embodiment 2
Raw materials used as follows:
High purity aluminium oxide powder (Al
2O
3Purity 〉=99.99wt%), trade mark LM2-N214, Dalian Luming Nanometer Material Co., Ltd. provides;
Nitric acid (analytical pure), Shanghai chemical reagents corporation provides;
Deionized water, water factory of Fudan University.
Raw materials used proportioning is as follows:
Deionized water and aluminum oxide powder add by weight 1:1, and the nitric acid add-on is exceeded with pretreatment fluid PH=2.
Raw material powder treatment process: remove ionized water, add nitric acid, stir, add pretreated aluminum oxide powder and adopt the manual machinery stirring that mixed slurry is mixed, leave standstill 9 hours treatment times with glass stick.
Performance comparison experimental program before and after raw material powder is handled: compare experiment with the pure zirconia aluminium powder respectively with two kinds of powders before and after handling.The sample forming method adopts the 200MPaCIP moulding, synthermal sintering in vacuum oven, the volume density of survey sintered specimen.
By data in the last table as can be seen, the powder sintering activity of handling is improved to some extent, and still with respect to the powder of citric acid treatment, its sintering activity increase rate is less.
Embodiment 3
Raw materials used as follows:
High purity aluminium oxide powder (Al
2O
3Purity 〉=99.99wt%), trade mark LM2-N214 Dalian Luming Nanometer Material Co., Ltd. provides;
The polyacrylic acid aqueous solution, water treatment plant, Wujin, Jiangsu provides;
Deionized water, water factory of Fudan University.
Raw materials used proportioning is as follows:
Deionized water and aluminum oxide powder add by weight 1:1, and the polyacrylic acid add-on is basic 1wt% with aluminum oxide powder.
Raw material powder treatment process: remove ionized water, add polyacrylic acid, stir, add pretreated aluminum oxide powder and adopt the manual machinery stirring that mixed slurry is mixed, leave standstill 6 hours treatment times with glass stick.
Performance comparison experimental program before and after raw material powder is handled: compare experiment with pure zirconia aluminium powder and the powder mix that adds the 0.1wt%MgO sintering aid respectively with two kinds of powders before and after handling.The sample forming method adopts the 200MPaCIP moulding, synthermal sintering in vacuum oven, the volume density of survey sintered specimen.
The contrast test result is as follows:
By data in the last table as can be seen, the powder sintering activity of handling is improved to some extent, and its sintering activity is between citric acid treatment powder and nitric acid treatment powder, and visible polyacrylic acid treatment effect is than the citric acid difference but be better than nitric acid.
Embodiment 4
Raw materials used as follows:
High purity aluminium oxide powder (Al
2O
3Purity 〉=99.99wt%), trade mark LM2-N214, Dalian Luming Nanometer Material Co., Ltd. provides;
The PBTCA aqueous solution, water treatment plant, Wujin, Jiangsu provides;
Deionized water, water factory of Fudan University.
Raw materials used proportioning is as follows:
Deionized water and aluminum oxide powder add by weight 1:1, and the PBTCA add-on is basic 1wt% with aluminum oxide powder.
Raw material powder treatment process and embodiment 1 are same, and performance comparison experimental program and embodiment 2 were together before and after raw material powder was handled.Data are close among contrast test result and the embodiment 1.
Embodiment 5
Raw materials used as follows:
High purity aluminium oxide powder (Al
2O
3Purity 〉=99.99wt%), trade mark LM2-N214, Dalian Luming Nanometer Material Co., Ltd. provides;
Phosphoric acid (analytical pure), Shanghai chemical reagents corporation provides;
Deionized water, water factory of Fudan University.
Raw materials used proportioning is as follows:
Deionized water and aluminum oxide powder add by weight 1:1, and the phosphoric acid add-on is exceeded with pretreatment fluid PH=3.
Raw material powder treatment process and embodiment 2 are same, and performance comparison experimental program and embodiment 2 were together before and after raw material powder was handled.Data are close among contrast test result and the embodiment 2.
In the foregoing description, the parameter of each component raw material and consumption and preparation process, only be the representative of choosing in order to describe the present invention, in fact a large amount of experiments show, all can obtain in summary of the invention part institute restricted portion and above-mentioned similar than the more high performance aluminum oxide powder of raw material powder.
Claims (2)
1. the method for a treatment of aluminum oxide powder, it is characterized in that, this method may further comprise the steps: allotment powder pretreatment fluid, sneak into the alumina raw material powder, mechanical stirring mixes slurry, be equipped with ultrasonic dispersing simultaneously, pretreatment time treats that greater than 30 minutes the abundant pre-treatment after drying of powder slurry obtains dry powder; Described powder pretreatment fluid concocting method is as follows: remove ionized water, add acid, mix, the deionized water quality of described use is less than the quality of pretreating raw material powder, described acid comprises and is selected from mineral acid, high price small molecular weight organic acid, one or more mixtures in the polyelectrolyte organic acid, described mineral acid comprises nitric acid, phosphoric acid, carbonic acid, hydrochloric acid, described high price small molecular weight organic acid comprises citric acid, 2-phosphonic acids butane-1,2, the 4-tricarboxylic acid, described polyelectrolyte organic acid comprises polyacrylic acid, polymethyl acrylic acid, the usage quantity of described mineral acid is to make the pH value of pretreatment fluid less than 3, and described high price small molecular weight organic acid usage quantity and polyelectrolyte organic acid usage quantity are for being that benchmark conversion is greater than 100ppm with pretreated raw material powder quality; The raw material powder add-on, with respect to the mixed slurry of water and powder, the volume percent of powder is less than 55vol%.
2. the method for a kind of treatment of aluminum oxide powder according to claim 1 is characterized in that, the ultrasonic frequency that described ultrasonic dispersing is used is 500～2000KHz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101120228A CN100469699C (en) | 2005-12-27 | 2005-12-27 | Method for the treatment of aluminum oxide powder |
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| CNB2005101120228A CN100469699C (en) | 2005-12-27 | 2005-12-27 | Method for the treatment of aluminum oxide powder |
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| CN100469699C true CN100469699C (en) | 2009-03-18 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441408B (en) * | 2010-10-13 | 2014-05-21 | 中国石油化工股份有限公司 | Preparation method for hydrogenation catalyst |
| CN104559796B (en) * | 2013-10-14 | 2018-01-26 | 天津西美半导体材料有限公司 | Preparation method applied to the modified aluminum oxide polishing fluid of superhard surfaces |
| CN106276993B (en) * | 2015-05-27 | 2017-08-11 | 裕祥化工（大连）有限公司 | A kind of nano aluminium oxide thickened pulp and preparation method thereof |
| RU2746675C2 (en) * | 2016-08-29 | 2021-04-19 | СЭСОЛ (ЮЭсЭй) КОРПОРЕЙШН | METHOD FOR PRODUCING ALUMINUM OXIDE DISPERSED AT pH GREATER THAN 8 |
| CN107352563A (en) * | 2017-07-21 | 2017-11-17 | 江苏万路达环保科技有限公司 | A kind of pretreatment technology of aluminum oxide for catalyst powder body material |
| CN111348668B (en) * | 2020-03-16 | 2022-03-15 | 中国铝业股份有限公司 | Preparation method of aluminum oxide for heat-conducting filler |
| CN118045614B (en) * | 2024-04-16 | 2024-06-11 | 烟台百川汇通科技有限公司 | Oil column forming method of alumina microspheres for propylene preparation process by propane dehydrogenation |
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Granted publication date: 20090318 Termination date: 20181227 |