CN112374514B - Method for rapidly preparing bayer stone microspheres with uniform particle size by double hydrolysis at room temperature - Google Patents
Method for rapidly preparing bayer stone microspheres with uniform particle size by double hydrolysis at room temperature Download PDFInfo
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- CN112374514B CN112374514B CN202011250721.XA CN202011250721A CN112374514B CN 112374514 B CN112374514 B CN 112374514B CN 202011250721 A CN202011250721 A CN 202011250721A CN 112374514 B CN112374514 B CN 112374514B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2006/12—Surface area
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention discloses a method for rapidly preparing a bayer stone microsphere with uniform particle size by double hydrolysis at room temperature. The method comprises the following steps: firstly, preparing a sodium aluminate solution, then adding absolute ethyl alcohol, and uniformly stirring to obtain a sodium aluminate ethanol aqueous solution system; adding an ammonium acid solution, uniformly stirring, standing, aging and carrying out liquid-phase precipitation reaction for 5-180 min; and filtering the precipitated product after the reaction is finished, washing a filter cake, and drying to obtain a white powdery solid, namely the bayer stone microspheres. The invention utilizes a weak acid salt and sodium aluminate solution to carry out rapid double hydrolysis reaction at room temperature and normal pressure, can obviously shorten the induction time of the crystallization process of the sodium aluminate, and controls the size of the grain diameter by adjusting the concentration of ammonium acid, thereby obtaining the uniform and controllable Bayer stone microspheres with the grain diameter in a certain range.
Description
Technical Field
The invention belongs to the technical field of alumina preparation, and particularly relates to a method for rapidly preparing a bayer stone microsphere with uniform particle size by double hydrolysis at room temperature.
Background
The alumina powder has excellent performances of high melting point, high resistance, high corrosion resistance and the like, and has wide application in the fields of electronics and optical ceramics. The properties of alumina mainly depend on its crystal phase, pore structure and morphology, and especially the morphology and pore structure of the material have important influence on performance, so that the morphology is controlled by the attention of researchers in recent years. Wherein, the narrow particle size distribution and the spherical shape are indispensable factors for obtaining good alumina powder, and the spherical alumina with an equiaxial structure shows unique excellence in the physical and mechanical properties of ceramics. The preparation of spherical alumina is the precursor of alumina, wherein gibbsite and bayer stone are important precursors, and the methods for preparing the two precursors are mainly water/solvothermal method, sol-gel method, hydrolysis method and the like. The traditional hydrothermal method can obtain alumina hydrate microspheres with smooth surfaces and uniform sizes, but the industrialization possibility is lower due to the requirements on energy consumption, waste liquid treatment and other influence factors, and the problems of high cost and great environmental pollution exist. The alumina microspheres obtained by the sol-gel method have good performance, and the experimental process is generally complicated; alumina hydrate microspheres prepared by a simple hydrolysis method generally have a low sphericity and are non-uniform in size.
Shuai et Al (Shuai Wei, Le Zhang, Yue Ben. high dispersion of α -Al2O3powders from co-precipitation method by step-by-step horizontal ball-milling [ J ]. Journal of Materials Science,2017,28(21):254-261.) by ball-milling the coprecipitated alumina precursors, spherical alumina powders with fine particle size of about 1-2 μm are obtained, but the degree of sphericity is poor. Although the method is simple, the obtained alumina microspheres have general properties and low sphericity and uniformity. Hairu et Al (Hairu Xiaoan Wang, Qiao Yin. Effect of Process Factors on Properties of High Dispersion Spherical alpha-Al 2O3 Particles Prepared by Hydrothermal Method [ J ]. Ceramics International,2019,45(17):007-014.) synthesized Spherical alumina using aluminum sulfate and aluminum nitrate as aluminum sources and urea as precipitant. It was found that sulfate ions play a key role in balling, and nitrate ions influence the particle size. Although the hydrothermal method can better control the appearance and the particle size of the alumina, the hydrothermal method has higher requirements on a hydrothermal kettle because the reaction is carried out at a higher temperature under pressure; the hydrothermal balling time is generally longer, and is often more than 6 h. Hui et al (Hui Yang, Yuan Xie, Guiong Hao.preparation of porous alumina microspheres via an oil-in-water emulsion method by a sol-gel process [ J ]. New Journal of Chemistry,2019,40:589-595.) prepared porous alumina microspheres with good morphology by a sol-gel method, and formed gel beads in oil water by using polyvinylpyrrolidone as a stabilizer to obtain microspheres with smooth surfaces. However, the particle size of the microspheres prepared by the method is large and the distribution is not uniform. Ying et al (Ying Zhang, Shili Zheng, Hao du. improved precipitation from sodium aluminate solution by adding methanol [ J ]. Hydrometallurgy,2009,98(1):38-44.) found that alcohol solvent can significantly increase the precipitation rate of the precipitate, the method goes through an induction period of 5h and then enters the crystal growth process, and the formation time of the microspheres is about 10 h. The prepared spherical particles are bigger and are gibbsite with the particle size of about 90 mu m. Similarly, Shaowei You et al (Shaowei You, Yan Li, Yifei Zhang. Synthesis of inorganic particulate base from a sodium aluminate solution reacted with a sodium bicarbonate [ J ]. Industral & Engineering Chemistry Research,2013,52(36): 12710-. On the basis of the above, it is desirable to rapidly prepare small and uniform hydrated alumina microspheres at room temperature.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention mainly aims to provide a method for rapidly preparing a spherical alumina precursor with uniform particle size and controllable size at room temperature by a double hydrolysis method.
According to the previous research technology, the method utilizes a weak acid salt and a sodium aluminate solution to carry out rapid double hydrolysis reaction at room temperature and normal pressure, can obviously shorten the induction time of the crystallization process of the sodium aluminate, and controls the size of the particle size by adjusting the concentration of ammonium, thereby obtaining the uniform and controllable Bayer stone microspheres with the particle size in a certain range.
The purpose of the invention is realized by the following technical scheme:
a method for rapidly preparing Bayer stone microspheres with uniform particle sizes by double hydrolysis at room temperature comprises the following steps:
firstly, preparing a sodium aluminate solution, then adding absolute ethyl alcohol, and uniformly stirring to obtain a sodium aluminate ethanol aqueous solution system; adding an ammonium salt solution, uniformly stirring, standing, aging and carrying out liquid-phase precipitation reaction, wherein the reaction time is 5-180 min; and filtering the precipitated product after the reaction is finished, washing a filter cake, and drying to obtain a white powdery solid, namely the bayer stone microspheres.
Preferably, the liquid phase precipitation reaction is carried out at room temperature and normal pressure.
Preferably, the liquid-phase precipitation reaction time is 5-180 min, and the bayer stone microspheres can be obtained within 5min at the fastest reaction speed.
Further preferably, the time of the liquid phase precipitation reaction is 5-60 min.
Preferably, the ammonium salt is at least one of ammonium oxalate, ammonium acetate or ammonium carbonate.
Preferably, the volume ratio of the absolute ethyl alcohol to the sodium aluminate solution is 1: 1 adding absolute ethyl alcohol.
Preferably, each 40mL of sodium aluminate ethanol aqueous solution system contains 1.20-2.40 g of sodium aluminate.
Preferably, the molar concentration of the ammonium salt solution added during the liquid-phase precipitation reaction is 0.05-0.15 mol/L.
Preferably, the ratio of the volume of the ammonium salt solution to the volume of the sodium aluminate ethanol aqueous solution system is 1: 4.
preferably, in the method, the time for stirring for two times is 1 min; the washing refers to washing by deionized water and absolute ethyl alcohol; the drying is carried out at 60 ℃ for 12 h.
The Bayer stone microspheres obtained by the method are all assembled by nano sheets, the average grain diameter of the microspheres is 1.08-4.59 mu m, and the specific surface area is 3.34-8.09m 2 Per g, pore volume of 0.010-0.023cm 3 (ii) a specific molar mass per gram of the silica, and an average pore diameter of 2.18 to 3.27 nm.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) by adding ammonium sulfate precipitant, the induction time for microsphere formation is greatly shortened. When the molar concentration of the added ammonium salt solution is 0.1M, the spheroidal particles can be obtained within 5min, and the complete microspheres can be obtained within 30 min. The process has the remarkable characteristics of rapidness, mildness, adjustable hydrolysis rate, adjustable microsphere morphology and the like.
(2) By adding ammonium precipitants such as ammonium oxalate, ammonium acetate or ammonium carbonate, the particle size of the obtained product is more uniform and controllable within a certain range. The method comprises the following steps of (1) obtaining the bayer stone microspheres with the average particle size of 1.08-4.6 mu m by changing the concentration of ammonium sulfate; and when the concentration of ammonium is gradually increased, the particle size of the microsphere is reduced. When the molar concentration of the added ammonium salt solution is 0.05M, the Bayer stone microspheres with the average particle size of 3.53-4.59 mu M can be obtained; when the molar concentration of the added ammonium solution is 0.1-0.15M, the Bayer stone microspheres with the average particle size of 1.08-2.07 mu M can be obtained.
Drawings
FIG. 1 is an SEM picture of the Bayer stone microspheres prepared in example 1.
Fig. 2 is an SEM picture of the bayer stone microspheres prepared in example 2.
Fig. 3 is an SEM picture of the bayer stone microspheres prepared in example 3.
Fig. 4 is an SEM picture of the bayer stone microspheres prepared in example 4.
Fig. 5 is an SEM picture of the bayer stone microspheres prepared in example 5.
Fig. 6 is an XRD pattern of the bayer stone microspheres prepared in each example.
FIG. 7 is a nitrogen adsorption-desorption isotherm curve and pore size distribution curve of the Bayer stone microspheres prepared in examples 1-3.
FIG. 8 is a nitrogen adsorption-desorption isotherm curve and pore size distribution curve of the Bayer stone microspheres prepared in examples 4-5.
FIGS. 9-13 are particle size distribution plots for the Bayer stone microspheres prepared in examples 1-5, respectively.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques. In particular, all the precipitation reactions mentioned in the examples were carried out at room temperature (25 ℃) and atmospheric pressure (1 atm).
Example 1
Preparation of bayer stone microspheres: dissolving 1.20g of sodium aluminate in 20mL of deionized water at room temperature, magnetically stirring for 15min to obtain a uniform sodium aluminate solution, adding 20mL of absolute ethyl alcohol, continuously magnetically stirring for 1min, quickly pouring 10mL of 0.1M ammonium oxalate solution, continuously magnetically stirring for 1min, stopping stirring, standing for reaction for 5min, filtering a white turbid solution obtained by the reaction, washing a filter cake with the deionized water for three times, then washing with the absolute ethyl alcohol once, and drying in a forced air drying oven at 60 ℃ for 12h to obtain the beierlite microspheres.
As shown in table 1 and fig. 1, the bayer stone microspheres obtained in example 1 were assembled from nanosheets, and the microspheres had an average particle diameter of 1.08 μm; the specific surface area is 4.64m 2 Perg, pore volume of 0.019cm 3 G, average pore diameter of 3.27 nm.
Example 2
Preparation of bayer stone microspheres: dissolving 1.20g of sodium aluminate in 20mL of deionized water at room temperature, magnetically stirring for 15min to obtain a uniform sodium aluminate solution, adding 20mL of absolute ethyl alcohol, continuously magnetically stirring for 1min, quickly pouring 10mL of 0.1M ammonium acetate solution, continuously magnetically stirring for 1min, stopping stirring, standing for reaction for 30min, filtering a white turbid solution obtained by the reaction, washing a filter cake with the deionized water for three times, then washing with the absolute ethyl alcohol once, and drying in a forced air drying oven at 60 ℃ for 12h to obtain the bayer stone microspheres.
As shown in table 1 and fig. 2, the bayer stone microspheres obtained in example 2 were assembled from nanosheets, and the microspheres had an average particle size of 2.07 μm; the specific surface area is 3.34m 2 Per g, pore volume of 0.010cm 3 (ii)/g, average pore diameter was 3.02 nm.
Example 3
Preparation of bayer stone microspheres: dissolving 1.80g of sodium aluminate in 20mL of deionized water at room temperature, carrying out magnetic stirring for 15min to obtain a uniform sodium aluminate solution, adding 20mL of absolute ethyl alcohol, continuing to carry out magnetic stirring for 1min, then quickly pouring 10mL of 0.10M ammonium carbonate solution, continuing to carry out magnetic stirring for 1min, stopping stirring, standing for reaction for 1h, filtering a white turbid solution obtained by the reaction, washing a filter cake for three times by using the deionized water, then washing the filter cake by using the absolute ethyl alcohol once, and drying the filter cake for 12h at the temperature of 60 ℃ in a forced air drying oven to obtain the bayer stone microspheres.
As shown in table 1 and fig. 3, the bayer stone microspheres obtained in example 3 were assembled from nanosheets, and the microspheres had an average particle diameter of 2.03 μm; the specific surface area is 7.72m 2 Per g, pore volume of 0.012cm 3 (ii)/g, average pore diameter 2.47 nm.
Example 4
Preparation of bayer stone microspheres: dissolving 2.40g of sodium aluminate in 20mL of deionized water at room temperature, magnetically stirring for 15min to obtain a uniform sodium aluminate solution, adding 20mL of absolute ethyl alcohol, continuously magnetically stirring for 1min, quickly pouring 10mL of ammonium oxalate solution with the concentration of 0.05M, continuously magnetically stirring for 1min, stopping stirring, standing for reaction for 1h, filtering a white turbid solution obtained by the reaction, washing a filter cake with the deionized water for three times, then washing with the absolute ethyl alcohol for one time, and drying in a forced air drying oven at the temperature of 60 ℃ for 12h to obtain the bayer stone microspheres.
As shown in table 1 and fig. 4, the bayer stone microspheres obtained in example 4 were assembled from nanosheets, and the microspheres had an average particle size of 3.59 μm; the specific surface area is 4.55m 2 Per g, pore volume of 0.014cm 3 (ii)/g, average pore diameter 2.18 nm.
Example 5
Preparation of bayer stone microspheres: dissolving 2.40g of sodium aluminate in 20mL of deionized water at room temperature, magnetically stirring for 15min to obtain a uniform sodium aluminate solution, adding 20mL of absolute ethyl alcohol, continuously magnetically stirring for 1min, quickly pouring 10mL of 0.15M ammonium oxalate solution, continuously magnetically stirring for 1min, stopping stirring, standing for reaction for 3h, filtering a white turbid solution obtained by the reaction, washing a filter cake with the deionized water for three times, then washing with the absolute ethyl alcohol for one time, and drying in a forced air drying oven at 60 ℃ for 12h to obtain the bayer stone microspheres.
As shown in table 1 and fig. 5, the bayer stone microspheres obtained in example 5 were assembled from nanosheets, and the microspheres had an average particle size of 2.53 μm; the specific surface area is 8.09m 2 Per g, pore volume of 0.023cm 3 (ii)/g, average pore diameter 2.20 nm.
As shown in fig. 1 and 5, the bayer stone in fig. 1 is assembled from fine nano-sheets. At this time, since the formation time of the microspheres is extremely short, the process of crystal growth has not been completed. Fig. 2 shows that the surface of the microspheres becomes smooth from rough with increasing time, the sphericity is gradually complete, and the average particle size of the microspheres increases by about 1 μm, which indicates that the average particle size of the microspheres is influenced by time. From example 3, it can be seen that the particle size of the microspheres did not vary much by changing the concentration of sodium aluminate and the kind of ammonium. However, as can be seen from the analysis of examples 4 and 5, the average particle size of the microspheres obtained was significantly larger, reaching 3.59 μm, when the concentration of ammonium was lower; at higher ammonium concentrations, however, the formation of microspheres takes less time due to the increased rate of hydrolysis, which in turn leads to a decrease in the average particle size.
TABLE 1 pore structure parameters, mean particle size and phase information for samples prepared in each example
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A method for rapidly preparing Bayer stone microspheres with uniform particle sizes by double hydrolysis at room temperature is characterized by comprising the following steps:
firstly, preparing a sodium aluminate solution, then adding absolute ethyl alcohol, and uniformly stirring to obtain a sodium aluminate ethanol aqueous solution system; adding an ammonium acid solution, uniformly stirring, standing, aging and carrying out liquid-phase precipitation reaction for 5-180 min; filtering the precipitated product after the reaction is finished, washing and drying a filter cake to obtain a white powdery solid, namely the bayer stone microspheres;
the ammonium is at least one of ammonium oxalate, ammonium acetate or ammonium carbonate;
according to the volume ratio of the absolute ethyl alcohol to the sodium aluminate solution of 1: 1, adding absolute ethyl alcohol;
1.20-2.40 g of sodium aluminate is contained in each 40mL of sodium aluminate ethanol aqueous solution system;
the molar concentration of the ammonium salt solution added during the liquid-phase precipitation reaction is 0.05-0.15 mol/L.
2. The method for rapidly preparing the bayer stone microspheres with uniform particle sizes through double hydrolysis at room temperature according to claim 1, wherein the liquid phase precipitation reaction is performed at room temperature and normal pressure.
3. The method for rapidly preparing the bayer stone microspheres with uniform particle size through double hydrolysis at room temperature according to claim 1, wherein the time of the liquid phase precipitation reaction is 5-60 min.
4. The method for rapidly preparing the bayer stone microspheres with uniform particle size through double hydrolysis at room temperature according to claim 1, wherein the volume ratio of the ammonium salt solution to the sodium aluminate ethanol aqueous solution system is 1: 4.
5. the method for rapidly preparing the bayer stone microspheres with uniform particle size through double hydrolysis at room temperature according to claim 1, wherein the time for stirring twice is 1 min; the washing refers to washing with deionized water and absolute ethyl alcohol; the drying is carried out at 60 ℃ for 12 h.
6. Bayer stone microspheres obtainable by a process according to any one of claims 1 to 5The method is characterized in that the Bayer stone microspheres are assembled by nano sheets, the average particle size of the microspheres is 1.08-4.59 mu m, and the specific surface area is 3.34-8.09m 2 The pore volume is 0.010-0.023 cm 3 (ii) a specific molar mass per gram of the silica, and an average pore diameter of 2.18 to 3.27 nm.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0340917A (en) * | 1989-07-07 | 1991-02-21 | Mitsubishi Materials Corp | Production of porous spherical alumina grain |
| JPH07133109A (en) * | 1993-11-08 | 1995-05-23 | Mizusawa Ind Chem Ltd | Production of granular alumina and spherical alumina particle |
| CN102432051A (en) * | 2010-09-29 | 2012-05-02 | 中国科学院过程工程研究所 | Method for preparing spherical Bayer stones |
| CN105836761A (en) * | 2016-03-28 | 2016-08-10 | 沈阳工业大学 | Preparation method of spherical bayerite powder with by-production of ammonium nitrate |
| RU2612288C1 (en) * | 2015-12-09 | 2017-03-06 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Method of decomposing aluminate solutions |
| CN106629797A (en) * | 2016-10-25 | 2017-05-10 | 武汉理工大学 | A double-hydrolysis reaction preparing method for texture-property-controllable gamma-aluminum oxide |
| CN108147456A (en) * | 2016-12-02 | 2018-06-12 | 中国科学院大连化学物理研究所 | A kind of preparation method of monodisperse zirconium dioxide microballoon |
| CN108483474A (en) * | 2018-04-10 | 2018-09-04 | 河南科技大学 | A kind of preparation method of nano-level sphere aluminium oxide |
| CN109516482A (en) * | 2019-01-16 | 2019-03-26 | 江苏师范大学 | A kind of preparation method of different-shape boehmite powder |
| CN110386613A (en) * | 2019-08-23 | 2019-10-29 | 广州大学 | A kind of preparation method for the mesoporous alumina hydrate microspherical of graduation that crystal form is controllable |
| CN111498880A (en) * | 2020-04-08 | 2020-08-07 | 广州大学 | Method for mildly preparing bayer stone microspheres by using aqueous two-phase system |
-
2020
- 2020-11-11 CN CN202011250721.XA patent/CN112374514B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0340917A (en) * | 1989-07-07 | 1991-02-21 | Mitsubishi Materials Corp | Production of porous spherical alumina grain |
| JPH07133109A (en) * | 1993-11-08 | 1995-05-23 | Mizusawa Ind Chem Ltd | Production of granular alumina and spherical alumina particle |
| CN102432051A (en) * | 2010-09-29 | 2012-05-02 | 中国科学院过程工程研究所 | Method for preparing spherical Bayer stones |
| RU2612288C1 (en) * | 2015-12-09 | 2017-03-06 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Method of decomposing aluminate solutions |
| CN105836761A (en) * | 2016-03-28 | 2016-08-10 | 沈阳工业大学 | Preparation method of spherical bayerite powder with by-production of ammonium nitrate |
| CN106629797A (en) * | 2016-10-25 | 2017-05-10 | 武汉理工大学 | A double-hydrolysis reaction preparing method for texture-property-controllable gamma-aluminum oxide |
| CN108147456A (en) * | 2016-12-02 | 2018-06-12 | 中国科学院大连化学物理研究所 | A kind of preparation method of monodisperse zirconium dioxide microballoon |
| CN108483474A (en) * | 2018-04-10 | 2018-09-04 | 河南科技大学 | A kind of preparation method of nano-level sphere aluminium oxide |
| CN109516482A (en) * | 2019-01-16 | 2019-03-26 | 江苏师范大学 | A kind of preparation method of different-shape boehmite powder |
| CN110386613A (en) * | 2019-08-23 | 2019-10-29 | 广州大学 | A kind of preparation method for the mesoporous alumina hydrate microspherical of graduation that crystal form is controllable |
| CN111498880A (en) * | 2020-04-08 | 2020-08-07 | 广州大学 | Method for mildly preparing bayer stone microspheres by using aqueous two-phase system |
Non-Patent Citations (3)
| Title |
|---|
| Aluminum Hydroxide Crystallization from Aluminate Solution Using Carbon Dioxide Gas: Effect of Temperature and Time;Somayeh Shayanfar et al.;《Journal of Crystal Growth》;20181231;第1-15页 * |
| Synthesis of morphology-controlled mesoporous transition aluminas derived from the decomposition of alumina hydrates;Wen Qian Jiao et al.;《Microporous and Mesoporous Materials》;20110615;第147卷;第1-10页 * |
| Synthesis of Uniformly Spherical Bayerite from a Sodium Aluminate Solution Reacted with Sodium Bicarbonate;Shaowei You et al.;《Industrial & Engineering Chemistry Research》;20130812;第52卷;第12710-12716页 * |
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