CN115108571A - Modified alpha-phase alumina and preparation method thereof - Google Patents
Modified alpha-phase alumina and preparation method thereof Download PDFInfo
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- CN115108571A CN115108571A CN202210891792.0A CN202210891792A CN115108571A CN 115108571 A CN115108571 A CN 115108571A CN 202210891792 A CN202210891792 A CN 202210891792A CN 115108571 A CN115108571 A CN 115108571A
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- C—CHEMISTRY; METALLURGY
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- 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
- C01F7/021—After-treatment of oxides or hydroxides
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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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
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Abstract
The invention relates to a modified alpha-phase alumina and a preparation method thereof, wherein the preparation method comprises the following steps: preparing alpha-phase alumina; crushing the alpha-phase alumina to obtain an alpha-phase alumina powder material with the particle size of 1-2 mu m; mixing the alpha-phase alumina powder material with an acid additive and a binder, and dispersing and stirring to obtain mixed slurry; spray drying the mixed slurry to obtain dried powder; and carrying out secondary drying treatment on the dried powder to obtain the modified alpha-phase alumina.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to modified alpha-phase alumina and a preparation method thereof.
Background
Alumina ceramics is one of special ceramics, and has excellent performances of high mechanical strength, good electrical insulation performance, high temperature resistance and the like; is widely applied to the fields of spaceflight, electronic devices, precise instruments, medicine and the like.
The most common aluminum oxide has three crystal forms of alpha, beta and gamma; wherein, alpha-Al 2 O 3 Commonly known as corundum, and belongs to the trigonal crystal system. alpha-Al is expressed in nature 2 O 3 The crystal form has the advantages of most compact crystal structure, highest stability, low chemical activity and best electrochemical property, and other isomeric crystal forms can be converted into alpha-Al through high-temperature calcination 2 O 3 。
At present, the preparation methods of alumina are roughly classified into three types, i.e., gas phase method, liquid phase method and solid phase method. The solid phase method is a preferred process for mass production because it is simple and does not generate waste water or exhaust gas. For example, the publication "research on the process for preparing flaky alpha-alumina powder by high-temperature solid phase method". However, the flaky alpha alumina powder prepared by the high-temperature solid phase method has poor fluidity and low apparent density, and the application and the expansion of the solid-phase sintered alpha alumina powder are greatly limited.
The flowability and apparent density of the product are directly affected by the shape of the alumina granulated powder. Therefore, how to ensure that the granulated powder has a good particle shape, thereby improving the fluidity and the apparent density of the solid-phase sintered alumina, is a problem that needs to be solved by the production process.
Disclosure of Invention
The embodiment of the invention provides modified alpha-phase alumina and a preparation method thereof.
In a first aspect, an embodiment of the present invention provides a method for preparing modified α -phase alumina, including:
preparing alpha-phase alumina;
crushing the alpha-phase alumina to obtain an alpha-phase alumina powder material with the particle size of 1-2 mu m;
mixing the alpha-phase alumina powder material with an acidic auxiliary agent and a binder, and dispersing and stirring to obtain a mixed slurry;
spray drying the mixed slurry to obtain dried powder;
and carrying out secondary drying treatment on the dried powder to obtain the modified alpha-phase alumina.
Preferably, the preparation of alpha-phase alumina comprises:
industrial aluminum hydroxide is used as a raw material, and alpha-phase aluminum oxide is prepared by calcining at 900-1200 ℃ in an inert atmosphere;
the alpha-phase alumina is in a sheet adhesion structure, the pH value is 10-11, the powder fluidity is less than or equal to 1g/s, and the powder apparent density is less than or equal to 0.3g/cm 3 。
Preferably, the acidic auxiliary agent is a solid acidic agent, and comprises one or more of oxalic acid, citric acid, boric acid and succinic acid; the acid auxiliary agent accounts for 0.05-0.2% of the mass of the alpha-phase alumina powder material;
the binder is specifically a resin binder or carboxymethyl cellulose CMC; the binder accounts for 0.03-0.1% of the mass of the alpha-phase alumina powder material.
Further preferably, the acidic adjuvant is citric acid.
Preferably, the spray drying is spray drying by using an air pressure type spray dryer;
the air pressure of the air pressure type spray dryer is 0.35MPa-0.4 MPa; the inlet temperature is 290-300 ℃, and the outlet temperature is not lower than 120 ℃.
Preferably, the secondary drying treatment is drying treatment in a drying oven under an inert environment, wherein the drying temperature is 150-200 ℃, and the drying time is 8-12 hours.
In a second aspect, the embodiment of the present invention provides a modified α -phase alumina prepared by the method for preparing a modified α -phase alumina according to the first aspect.
Preferably, the modified alpha-phase alumina is granular, the pH value is 7-9, the powder fluidity is more than or equal to 1.5g/s, and the powder apparent density is more than or equal to 0.55g/cm 3 。
According to the preparation method of the modified alpha-phase alumina provided by the embodiment of the invention, the alpha-phase alumina is modified through the synergistic effect of the acid auxiliary agent and the binder, so that on one hand, the pH value of the alpha-phase alumina is reduced through the acid auxiliary agent to increase the flowability of the powder, and on the other hand, the size of powder particles is increased through the addition of the binder to increase the apparent density of the powder. By the preparation method, the alpha-phase alumina with the flaky surface appearance is converted into the granular alpha-phase alumina with smooth surface and uniform shape, and the function of increasing the flowability of the powder is also realized.
The preparation method provided by the invention has low preparation temperature and does not generate waste gas and waste liquid; the method has the advantages of simple process, contribution to industrial production, low price and great reduction of production cost, and the used raw material is industrial aluminum hydroxide.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
FIG. 1 is a flow chart of a method for preparing modified alpha-phase alumina according to an embodiment of the present invention;
FIG. 2 is an X-ray diffraction (XRD) pattern of an alpha phase oxide produced during the production process of example 1 of the present invention;
FIG. 3 is one of Scanning Electron Microscope (SEM) images of an alpha phase alumina powder bulk material prepared during the preparation method of example 1 of the present invention;
FIG. 4 is a second SEM image of an alpha-phase alumina powder material prepared by the preparation method of example 1 of the present invention;
FIG. 5 is one of SEM images of modified alpha-phase alumina prepared in example 1 of the present invention;
FIG. 6 is a second SEM image of a modified alpha-phase alumina prepared according to example 1 of the present invention;
fig. 7 is an XRD pattern of the modified alpha-phase alumina prepared in example 1 of the present invention.
Detailed Description
The invention is further illustrated by the following figures and specific examples, but it should be understood that these examples are for the purpose of illustration only and are not to be construed as in any way limiting the present invention, i.e., as in no way limiting its scope.
The embodiment of the invention provides a preparation method of modified alpha-phase alumina, which mainly comprises the following preparation steps as shown in figure 1:
industrial aluminum hydroxide is used as a raw material, and is calcined for 8 to 12 hours at 900 to 1200 ℃ under inert atmosphere to prepare alpha-phase aluminum oxide; the alpha-phase alumina is in a sheet adhesion structure, the pH value is 10-11, the powder fluidity is less than or equal to 1g/s, and the powder apparent density is less than or equal to 0.3g/cm 3 。
Because different aluminum-containing raw materials determine different preparation methods of the alpha-phase aluminum oxide and finally determine the production cost, the embodiment selects the industrial aluminum hydroxide as the aluminum raw material, and has lower price compared with the aluminum oxide and the aluminum hydroxide, so that the production cost can be effectively reduced.
the pulverization treatment may specifically be a multistage pulverization method.
For example, the alpha-phase alumina powder material with the particle size of 1-2 μm is obtained by first performing primary crushing by a jaw crusher, performing secondary crushing by a roller mill and finally crushing the powder by an air flow mill.
The micro appearance of the alpha-phase alumina powder material obtained by crushing integrally presents an adhered and agglomerated worm-like appearance, the powder has poor fluidity and low apparent density.
in the mixing, dispersing and stirring process in the step, the obtained alpha-phase alumina powder material can be added with deionized water to prepare slurry, then the acid auxiliary agent and the binder are added into the prepared slurry according to a proportion, and a high-speed dispersion machine is used for stirring and dispersing to prepare mixed slurry.
The acidic auxiliary agent is solid acidic agent, including one or more of oxalic acid, citric acid, boric acid, and succinic acid; the acid auxiliary agent accounts for 0.05-0.2% of the mass of the alpha-phase alumina powder material; the binder is specifically resin binder or carboxymethyl cellulose (CMC); the adhesive accounts for 0.03-0.1% of the mass of the alpha-phase alumina powder material.
In the specific implementation of the invention, citric acid is preferably selected as the acidic auxiliary agent, and the chemical formula is C 6 H 8 O 7 The modified alpha-phase alumina only contains C, H, O elements, and can be volatilized and discharged in the form of carbon dioxide and water in a sintering step involved in the subsequent industrial application process of the modified alpha-phase alumina, and no other impurities are generated. Carboxymethyl cellulose (CMC) is preferably used as the binder.
the spray drying is carried out by adopting a spray dryer, preferably a pneumatic spray dryer;
the air pressure of the air pressure type spray dryer is 0.35MPa-0.4 MPa; the inlet temperature is 290-300 ℃, and the outlet temperature is not lower than 120 ℃.
The fluidity and the apparent density of the powder subjected to spray drying are both increased, and the pH value of the powder is obviously reduced due to the action of the acidic auxiliary agent.
And 150, carrying out secondary drying treatment on the dried powder to obtain the modified alpha-phase alumina.
The secondary drying treatment is specifically drying treatment in a drying oven under an inert environment, wherein the drying temperature is 150-200 ℃, and the drying time is 8-12 hours.
After step 140, the powder flowability and bulk density are improved, but not significantly. In addition, the pH of the powder obtained in step 140 is low, so that a small amount of the acidic substance may be volatilized by the secondary drying treatment to increase the pH of the material.
The drying temperature is not suitable to be too high, and the drying at the too high temperature can cause excessive loss of acidic substances and cannot play a role of adding acid, so the drying temperature is selected to be 150-200 ℃.
The modified alpha-phase alumina prepared by the preparation method is granular, the pH value is 7-9, the powder fluidity is more than or equal to 1.5g/s, and the powder apparent density is more than or equal to 0.55g/cm 3 。
According to the preparation method of the modified alpha-phase alumina provided by the embodiment of the invention, the alpha-phase alumina is modified through the synergistic effect of the acid auxiliary agent and the binder, so that on one hand, the pH value of the alpha-phase alumina is reduced through the acid auxiliary agent to increase the flowability of the powder, and on the other hand, the size of powder particles is increased through the addition of the binder to increase the apparent density of the powder. By the preparation method, the alpha-phase alumina with the flaky surface appearance is converted into the granular alpha-phase alumina with smooth surface and uniform shape, and the function of increasing the flowability of the powder is also realized.
In order to better understand the technical scheme provided by the invention, the following specific examples respectively illustrate the specific processes and characteristics of preparing the modified alpha-phase alumina by using the methods provided by the above embodiments of the invention.
Example 1
The embodiment 1 of the invention provides a preparation method of modified alpha-phase alumina. The method comprises the following specific steps:
step 1, preparing alpha-phase alumina:
the industrial aluminum hydroxide was used as a raw material, and the particle size (hereinafter, the median diameter Dv50) was 50 μm.
The industrial aluminum hydroxide is calcined for 8 hours at 1200 ℃ to obtain alpha-phase alumina. Fig. 2 is an XRD pattern of the alpha phase alumina prepared in this step.
And 2, crushing the alpha-phase alumina:
firstly, primarily crushing the alpha-phase alumina calcined in the step 1 by using a jaw crusher to obtain alpha-phase alumina powder with the particle size of about 20 microns; then carrying out secondary crushing on the mixture by a roller to obtain alumina powder with the grain size of about 15 mu m; finally, the powder is smashed through an air flow mill, and the alpha-phase alumina powder with the grain size of 1-2 mu m is obtained.
The micro morphology of the powder is shown in fig. 3 and 4, and the whole powder presents an adhered and agglomerated worm-like morphology, which may cause poor powder flowability and low apparent density. The alpha-phase alumina powder has the flowability of 0.5g/s and the apparent density of 0.28g/cm 3 The pH was 10.42.
Step 3, mixing, dispersing and stirring the alpha-phase alumina powder material with an acid auxiliary agent and a binder:
and (3) adding deionized water into the alpha-phase alumina powder material obtained in the step (2) to prepare slurry with the solid content of 30%, stirring and dispersing the slurry for about 30min at 1000rpm by using a high-speed dispersion machine, adding an acid auxiliary agent citric acid accounting for 0.1% of the mass of the alpha-phase alumina powder material and a binder carboxymethyl cellulose (CMC) accounting for 0.05% of the mass of the alpha-phase alumina powder material, and continuously stirring and dispersing for 1 hour to prepare mixed slurry.
And 4, carrying out spray drying on the mixed slurry:
adopting a pneumatic spray dryer with the air pressure of 0.4kg/cm 3 (ii) a The inlet temperature was 300 ℃ and the outlet temperature was 120 ℃. The fluidity of the powder subjected to spray drying treatment is increased, and the measured fluidity is 0.85 g/s; loose density 0.32g/cm 3 . Due to acid-base neutralization, the pH value of the powder is obviously reduced, and the pH value is 4.35 and is acidic.
And 5, carrying out secondary drying treatment on the dried powder.
And drying the powder obtained by spray drying at the drying temperature of 200 ℃ for 10 hours to obtain the modified alpha-phase alumina.
The modified alpha-phase alumina is tested, and the pH value is 8.7, the fluidity is 1.82g/s, and the loose packed density is 0.65g/cm 3 . The fluidity and the apparent density of the powder are respectively improved by 264 percent and 132 percent compared with the alpha-phase alumina in the step 2, and the fluidity of the powder is greatly improved.
The surface morphology of the modified alpha-phase alumina powder body of the embodiment measured by a scanning electron microscope is shown in fig. 5 and 6. As can be seen from fig. 5 and 6, the powder has a smooth surface and no adhesion between particles. The smooth surface topography is also responsible for its strong flow properties. Fig. 7 is an XRD pattern of the modified α -phase alumina powder of this example, and it can be seen that all diffraction peaks correspond to the α -phase alumina crystal structure in fig. 3, no impurity peak is generated, and the modified α -phase alumina powder is still pure α -phase alumina. The results show that the amount of the acidic auxiliary and the binder added in the present example is small, and the crystal structure of the alumina is not affected.
Example 2
The embodiment 2 of the invention provides a preparation method of modified alpha-phase alumina. The method comprises the following specific steps:
step 1, preparing alpha-phase alumina:
the industrial aluminum hydroxide was used as a raw material, and the particle size (hereinafter, the median diameter Dv50) was 48 μm.
Industrial aluminum hydroxide was calcined at 1000 ℃ for 8 hours to obtain alpha-phase alumina.
Step 2, crushing alpha-phase alumina:
firstly, primarily crushing the alpha-phase alumina calcined in the step 1 by using a jaw crusher to obtain alpha-phase alumina powder with the particle size of about 20 microns; then carrying out secondary crushing on the mixture by a roller to obtain alumina powder with the grain size of about 14 mu m; finally, the powder is smashed by air flow milling to obtain the alpha-phase alumina powder with the grain size of 1-2 mu m.
The alpha-phase alumina powder has the flowability of 0.49g/s and the apparent density of 0.27g/cm 3 The pH was 10.4.
Step 3, mixing, dispersing and stirring the alpha-phase alumina powder material with an acid auxiliary agent and a binder:
and (3) adding deionized water into the alpha-phase alumina powder material obtained in the step (2) to prepare slurry with the solid content of 30%, stirring and dispersing the slurry for about 30min at 1000rpm by using a high-speed dispersion machine, adding an acidic auxiliary agent oxalic acid accounting for 0.1% of the mass of the alpha-phase alumina powder material and a binder phenolic resin accounting for 0.03% of the mass of the alpha-phase alumina powder material, and continuously stirring and dispersing for 1 hour to prepare mixed slurry.
And 4, carrying out spray drying on the mixed slurry:
adopting a pneumatic spray dryer with the air pressure of 0.35kg/cm 3 (ii) a The inlet temperature was 290 ℃ and the outlet temperature was 130 ℃.
And 5, carrying out secondary drying treatment on the dried powder.
And drying the powder obtained by spray drying at 150 ℃ for 12 hours to obtain the modified alpha-phase alumina.
The modified alpha-phase alumina was tested to determine a pH of 8.6, a flowability of 1.76g/s, and a bulk density of 0.63g/cm 3 . The fluidity and the apparent density of the powder are respectively improved by 259% and 133% relative to the alpha-phase alumina in the step 2, and the fluidity of the powder is greatly improved.
Example 3
The embodiment 3 of the invention provides a preparation method of modified alpha-phase alumina. The method comprises the following specific steps:
step 1, preparing alpha-phase alumina:
the industrial aluminum hydroxide was used as a raw material, and the particle size (hereinafter, the median diameter Dv50) was 51 μm.
Industrial aluminum hydroxide was calcined at 900 ℃ for 10 hours to obtain alpha-phase alumina.
And 2, crushing the alpha-phase alumina:
firstly, primarily crushing the alpha-phase alumina calcined in the step 1 by using a jaw crusher to obtain alpha-phase alumina powder with the particle size of about 22 microns; then carrying out secondary crushing by a roller to obtain alumina powder with the grain size of about 17 mu m; finally, the powder is smashed through an air flow mill, and the alpha-phase alumina powder with the grain size of 1-2 mu m is obtained.
The alpha-phase alumina powder is tested to obtain the fluidity of 0.51g/s and the apparent density of 0.29g/cm 3 The pH was 10.61.
Step 3, mixing, dispersing and stirring the alpha-phase alumina powder material with an acid auxiliary agent and a binder:
and (3) adding deionized water into the alpha-phase alumina powder material obtained in the step (2) to prepare slurry with the solid content of 30%, stirring and dispersing the slurry for about 30min at 1000rpm by using a high-speed dispersion machine, adding an acid auxiliary agent boric acid accounting for 0.2% of the mass of the alpha-phase alumina powder material and a binder carboxymethyl cellulose accounting for 0.05% of the mass of the alpha-phase alumina powder material, and continuously stirring and dispersing for 1 hour to prepare mixed slurry.
And 4, carrying out spray drying on the mixed slurry:
adopting a pneumatic spray dryer with the air pressure of 0.4kg/cm 3 (ii) a The inlet temperature was 295 ℃ and the outlet temperature was 125 ℃.
And 5, carrying out secondary drying treatment on the dried powder.
And drying the powder obtained by spray drying at 180 ℃ for 10 hours to obtain the modified alpha-phase alumina.
The modified alpha-phase alumina was tested to determine a pH of 8.2, a flowability of 1.79g/s, and a bulk density of 0.67g/cm 3 . The flowability and the apparent density of the powder are respectively improved by 251% and 131% relative to the alpha-phase alumina in the step 2, and the flowability of the powder is greatly improved.
The preparation method provided by the invention has low preparation temperature and does not generate waste gas and waste liquid; the method has the advantages of simple process, contribution to industrial production, low price and great reduction of production cost, and the used raw material is industrial aluminum hydroxide.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A preparation method of modified alpha-phase alumina is characterized by comprising the following steps:
preparing alpha-phase alumina;
crushing the alpha-phase alumina to obtain an alpha-phase alumina powder material with the particle size of 1-2 mu m;
mixing the alpha-phase alumina powder material with an acid additive and a binder, and dispersing and stirring to obtain mixed slurry;
spray drying the mixed slurry to obtain dried powder;
and carrying out secondary drying treatment on the dried powder to obtain the modified alpha-phase alumina.
2. The method of preparing modified alpha-phase alumina according to claim 1, wherein the preparing alpha-phase alumina comprises:
industrial aluminum hydroxide is used as a raw material, and alpha-phase aluminum oxide is prepared by calcining at 900-1200 ℃ in an inert atmosphere;
the alpha-phase alumina is in a sheet adhesion structure, the pH value is 10-11, the powder fluidity is less than or equal to 1g/s, and the powder apparent density is less than or equal to 0.3g/cm 3 。
3. The method for producing a modified alpha-phase alumina according to claim 1,
the acid additive is specifically a solid acid agent and comprises one or more of oxalic acid, citric acid, boric acid and succinic acid; the acid auxiliary agent accounts for 0.05-0.2% of the mass of the alpha-phase alumina powder material;
the binder is specifically a resin binder or carboxymethyl cellulose CMC; the binder accounts for 0.03-0.1% of the mass of the alpha-phase alumina powder material.
4. The method of claim 3, wherein the acidic adjuvant is citric acid.
5. The method for preparing modified alpha-phase alumina according to claim 1, wherein the spray drying is spray drying with an air pressure type spray dryer;
the air pressure of the air pressure type spray dryer is 0.35MPa-0.4 MPa; the inlet temperature is 290-300 ℃, and the outlet temperature is not lower than 120 ℃.
6. The method for preparing modified alpha-phase alumina according to claim 1, wherein the secondary drying treatment is drying treatment in a drying oven under inert environment, wherein the drying temperature is 150-200 ℃, and the drying time is 8-12 hours.
7. A modified alpha-phase alumina prepared by the method of any one of claims 1 to 6.
8. The modified alpha-phase alumina of claim 7, wherein the modified alpha-phase alumina is in the form of particles, the pH value is 7-9, the powder fluidity is not less than 1.5g/s, and the powder bulk density is not less than 0.55g/cm 3 。
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