CN104829218A - Bimodal active alumina micropowder and preparation method - Google Patents
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Abstract
The invention discloses a preparation method for bimodal active alumina micropowder. The method comprises the following steps: (1) calcining industrial alumina powder at different temperatures so as to obtain calcined alumina powders with a variety of original crystalline sizes; (2) selecting two calcined alumina powders with different original crystalline sizes and carrying out ball milling so as to obtain the bimodal active alumina micropowder, wherein the mass ratio of the two calcined alumina powders with different original crystalline sizes is 0.2-5: 1. The preparation method for the bimodal active alumina micropowder provided by the invention is simple and can obtain bimodal-distribution active alumina micropowder; and the obtained bimodal alumina micropowder can be used for refractory products and can improve performances like construction performance, compactness, slag resistance and mechanical strength of the refractory products.
Description
Technical field
The present invention relates to fire resisting material field, be specifically related to a kind of bimodal activity alumina powder and preparation method thereof.
Background technology
Reactive alumina is a kind of very important refractory raw material, its Al
2o
3content is generally more than 98%.Reactive alumina is raw material mainly with commercial alumina, adopts tunnel furnace (rotary kiln) high-temperature calcination, forms, have that purity is high, α-Al through grinding classification
2o
3the features such as transformation efficiency is high, true specific gravity is large, stable crystal form, narrow particle size distribution and good dispersity, are widely used in pottery, electroceramics, refractory materials, sparking plug, support of the catalyst, glass insulator filler, premium insulation parts, high-purity refractory fibre, poured with epoxy resin stopping composition, grinding, polishing abrasive material etc.
Active Calcined polishing aluminum oxide micro mist, as the important component part of refractory castable mesostroma material, has the irreplaceable effects of other refractory raw materials such as high temperature resistant, acceleration of sintering.What the Calcined polishing aluminum oxide powder size distribution used in the market presented is unimodal distribution, little for the effect changing mould material mobility, in the active Calcined polishing aluminum oxide micro mist of produced in conventional processes in addition, the content of sodium oxide is higher, for producing the disadvantageous effect of high-temperature behavior in mould material.
The bimodal activity alumina powder received much concern in recent years, its granularity presents bimodal distribution, and this bomodal size distribution is more conducive to the mould material mobility improved, and improves the workability of mould material.Meanwhile, the bomodal size distribution of bimodal activity alumina powder can better fill pore, is formed tightly packed in mould material, makes mould material densification more, improves physical strength.Bimodal activity alumina powder can improve the use properties of refractory castable greatly, extends the work-ing life of refractory castable.Therefore develop excellent property and stable bimodal activity alumina powder product, there is great meaning.
Application publication number is the production technique that the patent of invention document of CN103028482A discloses a kind of alumina powder, this patent relates to a kind of sorting process of aluminum oxide powder, settling process and press over system is adopted to extract the aluminum oxide powder of two kinds of granularities, then mixing overflow process is carried out, namely obtain a kind of abrasive material aluminum oxide powder, there is granularity and can design, in process of lapping, obviously reduce the feature scratched.But this method complex process, production efficiency are low, cost is high.
Application publication number is that the patent of invention document of CN104108923A discloses a kind of active Calcined polishing aluminum oxide micro mist and complete processing thereof, with commercial alumina, aluminium hydroxide for major ingredient, grinding aid and composite mineralizer are auxiliary material, after all raw material mixing and ball milling, balling-up, dry, in shaft furnace, low temperature burns slowly, obtains a kind of active Calcined polishing aluminum oxide micro mist.This patent is only analyzed calcining process, but does not control aluminum oxide powder size-grade distribution, and alumina powder prepared by this method farthest can not improve the performance of mould material.
Application publication number is that the patent of invention document of CN103351012A discloses a kind of alumina powder jointed preparation method, its preparation process with Aluminum chloride anhydrous and ammoniacal liquor for raw material, first Aluminum chloride anhydrous is carried out sublimating and condensing purification, then by its wiring solution-forming, under agitation with ammonia neutralization, obtain aluminium hydroxide powder, drying, high-temperature calcination, obtain high purity alumina powder.Although but this type of aluminum oxide powder has high-purity feature, do not carry out adjusting and optimizing to its granularity, be unfavorable for the flowing property of raising mould material, density and physical strength, and production cost is higher.
Application publication number is the preparation method that the patent of invention document of CN102849762A discloses a kind of nano-alumina powder, aluminium powder and solvent n-hexyl alcohol is adopted to react, first obtained alcohol aluminum compound, then through hydrolysis, distillation, separation, sinter process, prepares nano-alumina powder product.This patent produces that product foreign matter content is few, pore volume is large, specific surface is large, pore size distribution is reasonable, is as Industrial Catalysis agent carrier.Application publication number is the preparation method that the patent of invention document of CN1374251 discloses a kind of superpurity nano level alumina powder, react by fine aluminium and low-carbon alcohol and generate aluminium-alcohol salt, raffinal alkoxide is obtained again through decompression complexing rectification and purification, alkoxide is dissolved in high-purity non-polar solvent, aluminium hydroxide is generated with the hydrolysis of ultrapure water steam, again through aging, washing and filtering, final high temperature thermal treatment obtains superpurity nano level alumina powder.That prepares by this inventive method ultrapure nano alumina powder jointedly can be applicable to fluorescent material, support of the catalyst, artificial lens, electronic component, the fields such as abrasive material.But this technical scheme production cost disclosed in two patents is high, and aluminum oxide powder granularity is concentrated, and be used for the high-end ceramic products such as support of the catalyst, the matrix be not suitable for as mould material uses.
Alumina powder of the prior art, mostly is unimodal distribution, and granularity is concentrated, and production cost is higher, is unfavorable for improving mould material performance, for this reason, for the deficiency that traditional activated alumina powder exists, needs to develop bimodal (activity) alumina powder.
Summary of the invention
The invention provides a kind of bimodal activity alumina powder and preparation method thereof, preparation technology is simple, the Reactive alumina of bimodal distribution can be obtained, the bimodal activity alumina powder of gained is used in refractory product, the performances such as the workability of refractory product, compactness, slag resistance and physical strength can be improved.
A preparation method for bimodal activity alumina powder, comprises the following steps:
(1) industrial alumina powder is calcined at different temperature, obtain the calcined oxide aluminium powder with multiple former brilliant size;
(2) choose the calcined oxide aluminium powder that two kinds have different former brilliant sizes, carry out ball milling, obtain described bimodal activity alumina powder.
In described industrial alumina powder, the massfraction of each composition is: Al
2o
3>=99.0%, Fe
2o
3≤ 0.04%, SiO
2≤ 0.04%, R
2o≤0.12%, igloss≤0.80%, moisture≤0.50%.
In described industrial alumina powder, the powder particle size of massfraction more than 95% is-325 orders.Namely described industrial alumina powder can account for more than 95% of industrial alumina powder total mass by the quality of 325 orders (44 μm) screen portion.
Owing to containing γ-Al in commercial alumina
2o
3many with intermediate compound, about have the volumetric shrinkage of 14.5% during sintering, therefore, commercial alumina can not be directly used in making refractory product, and needs to carry out pre-treatment according to the purposes of performance and refractory product, adopts calcining and pulverize in the present invention.
The former brilliant size of calcined oxide aluminium powder will affect the size distribution of bimodal activity alumina powder, has a significant impact the performance of bimodal activity alumina powder, and preferably, the former crystalline substance of described calcined oxide aluminium powder is of a size of 0.1 μm ~ 30 μm.Further preferably, the former crystalline substance of described calcined oxide aluminium powder is of a size of 0.5 μm ~ 20 μm.Preferred again, the former crystalline substance of described calcined oxide aluminium powder is of a size of 0.5 μm ~ 10 μm.Most preferably, the former crystalline substance of described calcined oxide aluminium powder is of a size of 0.5 μm ~ 5 μm.
Industrial alumina powder adopts tunnel furnace of the prior art, rotary kiln or shaft furnace to calcine, in order to obtain the stable calcined oxide aluminium powder of homogeneous grain diameter, need to be optimized the calcining process of commercial alumina, typically, the factor affecting commercial alumina calcining process comprises: temperature rise rate when calcining temperature, calcination time, calcining and rate of temperature fall.
Specifically, temperature during calcining is higher, and soaking time is longer, temperature rise rate and rate of temperature fall slower, then the former brilliant size of the Calcined polishing aluminum oxide obtained is larger.
Preferably, the temperature rise rate in step (1) during calcining is 1 ~ 30 DEG C/min, and calcining temperature is 1100 DEG C ~ 1700 DEG C, and rate of temperature fall is 1 ~ 30 DEG C/min.Soaking time is 1 ~ 24h.With this understanding, the former brilliant size range of the Calcined polishing aluminum oxide of acquisition is 0.1 ~ 30 μm.
Further preferably, the temperature rise rate in step (1) during calcining is 1 ~ 20 DEG C/min, and calcining temperature is 1100 DEG C ~ 1600 DEG C, and rate of temperature fall is 1 ~ 20 DEG C/min.Soaking time is 1 ~ 16h.With this understanding, the former brilliant size range of the Calcined polishing aluminum oxide of acquisition is 0.5 ~ 20 μm.
Preferred again, the temperature rise rate in step (1) during calcining is 1 ~ 15 DEG C/min, and calcining temperature is 1100 DEG C ~ 1600 DEG C, and rate of temperature fall is 1 ~ 15 DEG C/min.Soaking time is 1 ~ 10h.With this understanding, the former brilliant size range of the Calcined polishing aluminum oxide of acquisition is 0.5 ~ 10 μm.
Preferred again, the temperature rise rate in step (1) during calcining is 1 ~ 10 DEG C/min, and calcining temperature is 1100 DEG C ~ 1500 DEG C, and rate of temperature fall is 1 ~ 10 DEG C/min.Soaking time is 1 ~ 8h.With this understanding, the former brilliant size range of the Calcined polishing aluminum oxide of acquisition is 0.5 ~ 5 μm.
The acquisition of the calcined oxide aluminium powder of different former brilliant size, obtain after different calcining temperature places is incubated for some time, such as, 1200 DEG C are warming up to the speed of temperature rise rate 8 DEG C/min, after 1200 DEG C of insulation 5h, be down to room temperature with the speed of rate of temperature fall 8 DEG C/min again, obtain the calcined oxide aluminium powder that former crystalline substance is of a size of 1 ± 0.2 μm.
In order to obtain the calcined oxide aluminium powder of larger former brilliant size or reduce calcining temperature thus reduce energy consumption, add mineralizer in industrial alumina powder after, calcine at different temperature, the mass ratio of described mineralizer and industrial alumina powder is 0.1 ~ 5:100.Described mineralizer is at least one in boric acid, ammonium chloride, Neutral ammonium fluoride, aluminum fluoride.
The kind of mineralizer and the selection of add-on can have influence on size and the pattern of Calcined polishing aluminum oxide crystal, and introducing mineralizer can promote the γ-Al in commercial alumina
2o
3to α-Al
2o
3transform, remove Na
2o, reduces the calcining temperature of calcined oxide aluminium powder or increases the former brilliant size of calcined oxide aluminium powder.
According to needs, two kinds of calcined oxide aluminium powders with different former brilliant size can be chosen arbitrarily and carry out ball milling, obtain bimodal activity alumina powder.If obtain multimodal Reactive alumina, the multiple calcined oxide aluminium powder with different former brilliant size can be chosen arbitrarily as required and carry out ball milling acquisition.
In order to obtain the good bimodal activity alumina powder of use properties, the quality of the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference can not be excessive than difference, and preferably, the mass ratio of the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference is 0.2 ~ 5:1.
Further preferably, the mass ratio of the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference is 0.3 ~ 3:1.Preferred again, the mass ratio of the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference is 0.5 ~ 2:1.
The mass ratio of the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference directly affects the grain size distribution of bimodal activity alumina powder, by selecting suitable mass ratio, the grain size distribution of optimization can be obtained, improve workability and the density of mould material, fill pore, promote the high temperature sintering of mould material.
As preferably, the ratio of grinding media to material of ball milling is 2.5 ~ 5:1.
The ratio of grinding media to material of ball milling and Ball-milling Time can affect the size-grade distribution of bimodal activity aluminum oxide, during ball milling, ensure the Calcined polishing aluminum oxide sphere of powder to be milled to former brilliant size as much as possible, and are fully mixed by the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference.
Present invention also offers a kind of bimodal activity alumina powder, the preparation method of the bimodal activity alumina powder described in employing prepares.
Bimodal activity alumina powder provided by the invention and preparation method thereof, by selecting the Calcined polishing aluminum oxide micro mist with suitable former brilliant size, prepare the bimodal activity alumina powder with desired particle size distribution, the grain size distribution realizing bimodal activity alumina powder is controlled.The bimodal activity alumina powder of preparation is used in refractory castable, the mobility of refractory castable can be improved, improve the index such as density and physical strength, greatly improve the use properties of refractory castable, improve the work-ing life of refractory castable.
Embodiment
Embodiment 1 ~ 8
(1) industrial alumina powder is calcined at different temperature, obtain the calcined oxide aluminium powder with multiple former brilliant size;
(2) choose the calcined oxide aluminium powder that two kinds have different former brilliant sizes, carry out ball milling, obtain bimodal activity alumina powder, the former brilliant size of the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference, mass ratio and ratio of grinding media to material are as shown in table 1.
Table 1
Comparative example 1
The Calcined polishing aluminum oxide of two kinds of former brilliant sizes in embodiment 1 is carried out ball milling respectively, the ratio of grinding media to material of ball milling and Ball-milling Time identical with embodiment 1, obtain each self-corresponding Reactive alumina.
Comparative example 2
The Calcined polishing aluminum oxide of two kinds of former brilliant sizes in embodiment 5 is carried out ball milling respectively, the ratio of grinding media to material of ball milling and Ball-milling Time identical with embodiment 5, obtain each self-corresponding Reactive alumina.
Comparative example 3
The Calcined polishing aluminum oxide former crystalline substance being of a size of 2 μm carries out ball milling, and ratio of grinding media to material and Ball-milling Time, with embodiment 4, obtain Reactive alumina.
Performance characterization
The specific surface area BET of bimodal activity alumina powder and particle diameter D
50and D
90as shown in table 2.
Table 2
| Embodiment sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| BET/m 2·g -1 | 7.5 | 7.3 | 6.2 | 5.7 | 4.8 | 4.1 | 3.5 | 3.3 |
| D 50/μm | 0.5 | 0.7 | 1.0 | 1.2 | 1.5 | 1.7 | 1.9 | 2.0 |
| D 90/μm | 1.9 | 2.0 | 2.8 | 3.1 | 3.6 | 4.5 | 4.6 | 4.9 |
In mould material, add bimodal activity alumina powder that embodiment 1 ~ 8 obtains and the Reactive alumina that comparative example 1 ~ 3 obtains respectively, carry out performance characterization to mould material, result is as shown in table 4.The composition of mould material is as shown in table 3.
Table 3
In table 3, ZX1 is the dispersed aluminum oxide of retardation setting type, and ZD1 is the dispersed aluminum oxide of short solidifying type.
Wherein, in comparative example 1, the additional proportion of two kinds of Reactive aluminas is with the mass ratio of two kinds of Calcined polishing aluminum oxides in embodiment 1, and in comparative example 2, the additional proportion of two kinds of Reactive aluminas is with the mass ratio of two kinds of Calcined polishing aluminum oxides in embodiment 5.
In comparative example 1 ~ 3, total add-on of Reactive alumina is identical with the add-on of bimodal activity alumina powder in table 3.
Table 4
As can be seen from Table 2, the size-grade distribution of bimodal activity alumina powder provided by the invention is adopted to present bimodal, owing to adopting the preparation of low sodium alumina raw material, in the product obtained, Na2O content is extremely low, bimodal size-grade distribution is conducive to the mobility improving refractory castable, as shown in table 4, improve the workability of refractory castable, fill pore better, formed tightly packed in refractory castable, make refractory castable densification more, improve the physical strength (as after demoulding folding strength in table 4 and process, folding strength all has lifting) of refractory castable, improve the use properties of refractory castable, extend the work-ing life of refractory castable.
Claims (8)
1. a preparation method for bimodal activity alumina powder, is characterized in that, comprises the following steps:
(1) industrial alumina powder is calcined at different temperature, obtain the calcined oxide aluminium powder with multiple former brilliant size;
(2) choose the calcined oxide aluminium powder that two kinds have different former brilliant sizes, carry out ball milling, obtain described bimodal activity alumina powder.
2. the preparation method of bimodal activity alumina powder as claimed in claim 1, it is characterized in that, the mass ratio of the calcined oxide aluminium powder of two kinds of former brilliant sizes of difference is 0.2 ~ 5:1.
3. the preparation method of bimodal activity alumina powder as claimed in claim 1, it is characterized in that, the ratio of grinding media to material of ball milling is 2.5 ~ 5:1.
4. the preparation method of bimodal activity alumina powder as claimed in claim 1, it is characterized in that, the former crystalline substance of described calcined oxide aluminium powder is of a size of 0.1 μm ~ 30 μm.
5. the preparation method of bimodal activity alumina powder as claimed in claim 1, is characterized in that, the temperature rise rate in step (1) during calcining is 1 ~ 30 DEG C/min, and calcining temperature is 1100 DEG C ~ 1700 DEG C, and rate of temperature fall is 1 ~ 30 DEG C/min.
6. the preparation method of bimodal activity alumina powder as claimed in claim 1, it is characterized in that, after adding mineralizer, calcine at different temperature in industrial alumina powder, the mass ratio of described mineralizer and industrial alumina powder is 0.1 ~ 5:100.
7. the preparation method of bimodal activity alumina powder as claimed in claim 6, it is characterized in that, described mineralizer is at least one in boric acid, ammonium chloride, Neutral ammonium fluoride, aluminum fluoride.
8. a bimodal activity alumina powder, is characterized in that, adopt as arbitrary in claim 1 ~ 7 as described in preparation method prepare.
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| CN113603465A (en) * | 2021-08-27 | 2021-11-05 | 新化县顺达电子陶瓷有限公司 | Ceramic material for temperature controller and preparation method thereof |
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| CN105294138A (en) * | 2015-12-08 | 2016-02-03 | 武汉科技大学 | Doublet aluminum oxide micropowder and preparation method thereof |
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| CN111498883A (en) * | 2020-03-13 | 2020-08-07 | 苏州盛曼特新材料有限公司 | Preparation method of large-primary-crystal high-purity calcined α -alumina micropowder |
| CN113045298A (en) * | 2021-03-24 | 2021-06-29 | 苏州盛曼特新材料有限公司 | Alumina-based coagulant for refractory castable and preparation method and application thereof |
| CN113045298B (en) * | 2021-03-24 | 2022-12-13 | 苏州盛曼特新材料有限公司 | Alumina-based coagulant for refractory castable and preparation method and application thereof |
| CN113603465A (en) * | 2021-08-27 | 2021-11-05 | 新化县顺达电子陶瓷有限公司 | Ceramic material for temperature controller and preparation method thereof |
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Application publication date: 20150812 Assignee: Shaoxing Hongyi New Material Co.,Ltd. Assignor: ZHEJIANG ZILI ADVANCED MATERIALS Co.,Ltd. Contract record no.: X2021330000208 Denomination of invention: Bimodal activated alumina powder and preparation method thereof Granted publication date: 20170111 License type: Common License Record date: 20210831 Application publication date: 20150812 Assignee: Zhejiang Zili High Temperature Technology Co.,Ltd. Assignor: ZHEJIANG ZILI ADVANCED MATERIALS Co.,Ltd. Contract record no.: X2021330000207 Denomination of invention: Bimodal activated alumina powder and preparation method thereof Granted publication date: 20170111 License type: Common License Record date: 20210831 |