CN114804168A - Preparation method of high-purity aluminum-rich magnesium spinel - Google Patents
Preparation method of high-purity aluminum-rich magnesium spinel Download PDFInfo
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- CN114804168A CN114804168A CN202210492554.2A CN202210492554A CN114804168A CN 114804168 A CN114804168 A CN 114804168A CN 202210492554 A CN202210492554 A CN 202210492554A CN 114804168 A CN114804168 A CN 114804168A
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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
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/162—Magnesium aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention provides a preparation method of high-purity aluminum-rich magnesium spinel, which comprises the following steps: preheating gamma-phase alumina fine powder and crystalline magnesium chloride fine powder through a mesh belt kiln; spraying the preheated fine powder to slurry through a water curtain rich in carbon dioxide, then flowing into a stirring barrel, and uniformly stirring to obtain slurry; then sending the slurry into a filter press, and carrying out filter pressing to obtain a filter cake; and finally, sending the filter cake to a high-temperature kiln for pretreatment, calcining to 1200-1400 ℃, preserving the heat for a certain time at the temperature, and naturally cooling to obtain the high-purity aluminum-rich magnesium spinel. The preparation method of the invention has the advantages of stable impurity removal without leaving, and can reduce the sodium oxide component to below 0.1 wt%, the alumina content in the obtained aluminum-rich magnesium aluminate spinel can reach above 95 wt%, the grain diameter can be adjusted within the range of 0.5-1 micron, and the preparation method has the characteristics of a gradient functional material; the preparation method has the advantages of high process stability, convenient production operation and low manufacturing cost.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and relates to a preparation method of aluminum-rich aluminum-magnesium spinel.
Background
The aluminum-magnesium spinel is a main raw material of a high-performance refractory material and a spinel-based special ceramic material, and has extremely high temperature resistance, wear resistance and insulating property. The aluminum-magnesium spinel forms ceramic bonding with other raw materials in the refractory material under the high-temperature condition, and the mechanical property, the erosion resistance and the thermal shock resistance of the refractory material are enhanced. The higher the alumina dissolved in the magnesium aluminate spinel, the sintering performance can be greatly activated due to the melting-out of the alumina under the high-temperature application condition, and the performance improvement of the high-temperature material is promoted. In the production of spinel-based special ceramic products, the aluminum-magnesium spinel can form a spinel-alumina gradient composite structure along with the melting and removal of alumina in the sintering process, so that the crystal boundary is optimized, and the ceramic performance is improved.
In the actual production of the aluminum-magnesium spinel, the aluminum oxide and the magnesium oxide are generally used as raw materials, and mineralizer is added to prepare the aluminum-magnesium spinel through a solid-phase reaction mode of high-temperature calcination. There are several significant limitations to this process route: firstly, during solid phase reaction, impurities in raw materials are difficult to remove, the purity of the aluminum-magnesium spinel is reduced, particularly, sodium oxide impurity components exist, and the aluminum-magnesium spinel can react with other raw materials in a refractory material to generate a low-melting-point phase when being used at high temperature, so that the high-temperature service performance of the refractory material is reduced, and the electrical property of ceramic can be obviously reduced and the quality of a product is reduced in the process of firing special ceramic; secondly, the solid phase reaction temperature is up to more than 1500 ℃, the full reaction can be carried out, the free magnesium oxide is eliminated, the energy consumption is high, and the manufacturing cost is high; the chemical content of alumina in the magnesium aluminate spinel prepared by the solid-phase reaction is generally not more than 95 percent, which limits the preparation of high-performance refractory materials and spinel-based special ceramic materials.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a preparation method of high-purity aluminum-rich magnesium spinel.
The method comprises the following steps:
firstly, flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 4-7:1 on a conveyor belt, wherein the thickness of the gamma-phase alumina fine powder and the crystalline magnesium chloride fine powder is 3-10 mm, and preheating the gamma-phase alumina fine powder and the crystalline magnesium chloride fine powder to 60-80 ℃ through a mesh belt kiln;
spraying the preheated fine powder to slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, and uniformly stirring to obtain slurry;
step three, feeding the slurry into a filter press, and performing filter pressing to obtain a filter cake with the water content of 20-40 wt%;
step four, sending the filter cake to a high-temperature kiln for pretreatment, then calcining to 1200-1400 ℃, carrying out heat preservation reaction at the temperature, and naturally cooling to obtain the aluminum-rich magnesium spinel;
wherein the impurity sodium oxide content of the gamma-phase alumina fine powder is less than or equal to 0.50 wt%, and the magnesium chloride content of the crystalline magnesium chloride fine powder is more than or equal to 46 wt%.
Further, in the second step, carbon dioxide gas is introduced into water and sprayed on the surface of the preheated fine powder to prepare slurry with the temperature of 30-50 ℃ and the solid content of 20-40 wt%.
Furthermore, the carbon dioxide gas is obtained by liquid carbon dioxide or dry ice, and the content of the carbon dioxide in the liquid carbon dioxide or the dry ice is more than or equal to 99.99 wt%.
Furthermore, in the second step, the stirring time is 15-30 minutes.
Furthermore, in the fourth step, the heat preservation time is 1-10 hours.
In addition, in the third step, the used filter pressing equipment is a centrifugal filter press or a plate blank filter press, and in the fourth step, the used high-temperature kiln is a tunnel kiln or a rotary kiln.
Compared with the prior art, the invention adopts the principles of wet chemical reaction and solid-phase kinetic reaction, soluble impurities such as sodium oxide, lithium oxide, potassium oxide and the like are subjected to dissolution reaction in aqueous slurry to produce water-soluble carbonate with carbon dioxide, magnesium ions in the solution are combined with the carbonate to generate magnesium carbonate which is uniformly attached to the surface of alumina, the soluble impurities such as sodium ions, lithium ions, potassium ions, chloride ions and the like obtained after the reaction can be removed through a filter pressing process, and the filtrate produced in the filter pressing process is pollution-free and can be recycled; in the pretreatment stage of the high-temperature kiln, magnesium carbonate is decomposed to obtain super-active magnesium oxide, and the obtained mixture of the active magnesium oxide and the aluminum oxide can complete spinel reaction at the lower temperature of 1200-1400 ℃, so that the energy consumption required by the reaction can be obviously reduced; the waste heat discharged after the high-temperature kiln is calcined can be used for assisting the preheating of the mesh belt kiln and the pretreatment of filter cakes after filter pressing, so that the heat can be recycled, and the energy consumption and the cost are further reduced.
The reaction equation involved in the invention is as follows:
2CO 2 +R 2 O+MgCl 2 +H 2 O＝MgCO 3 ↓+RCl+H 2 O，
Al 2 O 3 +MgCO 3 ＝MgO·Al 2 O 3 +CO 2 ↑，
wherein R is Na, Li, K, etc.
The preparation method of the invention has the advantages of stable impurity removal without leaving, and capability of obviously removing soluble impurities in the raw materials, particularly reducing the content of sodium oxide components to be below 0.1 wt%; the alumina content of the prepared aluminum-rich magnesium spinel can reach more than 95 wt%, the grain diameter of the aluminum-rich magnesium spinel can be adjusted within the range of 0.5-1 micron, aluminum-rich magnesium spinels with different grain diameters can be obtained according to the combination of different calcination temperatures and different heat preservation times, and the aluminum-rich magnesium spinel has the characteristic of a gradient functional material; the preparation method has the advantages of high process stability, convenient production operation and low manufacturing cost.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to these examples, and the advantages of the present invention will be clearly understood by the following descriptions. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention. Other parts of the embodiments which are not described in detail are all the prior art.
In the following examples, the fine γ -phase alumina powder used had a content of sodium oxide as an impurity of 0.45 wt% as measured, the fine crystalline magnesium chloride powder used had a content of magnesium chloride of 46.3 wt% as measured, and the carbon dioxide gas used was obtained by passing liquid carbon dioxide having a carbon dioxide content of not less than 99.99 wt%.
In addition, in the preparation process of the microcrystalline alpha-phase alumina, the used filter pressing equipment is a centrifugal filter press or a plate blank filter press, and the used high-temperature kiln is a tunnel kiln or a rotary kiln. In the following examples, the press filter equipment used was a slab press filter, and the high temperature kiln used was a tunnel kiln.
Example 1
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with a mass ratio of 4:1 on a conveying belt, wherein the thickness of the fine powder is 5 mm, and preheating the fine powder to 75 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 25 minutes to obtain uniform slurry, wherein the solid content of the slurry is 25 wt%, and the temperature of the slurry is 35 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 25 wt%; and (3) sending the filter cake to a high-temperature kiln for pretreatment, then calcining to 1250 ℃, preserving heat for 6 hours at the temperature, and naturally cooling to obtain the aluminum-rich magnesium spinel.
Example 2
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 5:1 on a conveyor belt, wherein the thickness of the fine powder is 4 mm, and preheating the fine powder to 65 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 20 minutes to obtain uniform slurry, wherein the solid content of the slurry is 35 wt%, and the temperature of the slurry is 45 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 22 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1350 ℃, preserving the heat for 8 hours at the temperature, and naturally cooling to obtain the aluminum-rich magnesium aluminate spinel.
Example 3
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 6:1 on a conveyor belt, wherein the thickness of the fine powder is 6 millimeters, and preheating the fine powder to 80 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 20 minutes to obtain uniform slurry, wherein the solid content of the slurry is 30 wt%, and the temperature of the slurry is 50 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 30 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1350 ℃, preserving the heat for 10 hours at the temperature, and naturally cooling to obtain the aluminum-rich aluminum-magnesium spinel.
Example 4
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 7:1 on a conveying belt, wherein the thickness is 5 mm, and preheating to 65 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 15 minutes to obtain uniform slurry, wherein the solid content of the slurry is 25 wt%, and the temperature of the slurry is 45 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 28 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1350 ℃, preserving the heat for 8 hours at the temperature, and naturally cooling to obtain the aluminum-rich magnesium aluminate spinel.
Example 5
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with a mass ratio of 4:1 on a conveyor belt, wherein the thickness of the fine powder is 8 mm, and preheating the fine powder to 75 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 25 minutes to obtain uniform slurry, wherein the solid content of the slurry is 25 wt%, and the temperature of the slurry is 35 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 25 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1300 ℃, preserving heat for 1.5 hours at the temperature, and naturally cooling to obtain the aluminum-rich aluminum magnesium spinel.
Example 6
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 5:1 on a conveyor belt, wherein the thickness of the fine powder is 4 mm, and preheating the fine powder to 65 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then allowing the slurry to flow into a stirring barrel, and stirring for 30 minutes to obtain uniform slurry, wherein the solid content of the slurry is 35 wt%, and the temperature of the slurry is 45 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 22 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1350 ℃, preserving the heat for 1.5 hours at the temperature, and naturally cooling to obtain the aluminum-rich aluminum-magnesium spinel.
Example 7
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 6:1 on a conveying belt, wherein the thickness of the fine powder is 10 mm, and preheating the fine powder to 80 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then allowing the slurry to flow into a stirring barrel, and stirring for 25 minutes to obtain uniform slurry, wherein the solid content of the slurry is 30 wt%, and the temperature of the slurry is 50 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 30 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1350 ℃, preserving the heat for 1.5 hours at the temperature, and naturally cooling to obtain the aluminum-rich aluminum-magnesium spinel.
Example 8
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 7:1 on a conveyor belt, wherein the thickness of the fine powder is 4 mm, and preheating the fine powder to 65 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 25 minutes to obtain uniform slurry, wherein the solid content of the slurry is 35 wt%, and the temperature of the slurry is 45 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 28 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1350 ℃, preserving the heat for 1.5 hours at the temperature, and naturally cooling to obtain the aluminum-rich aluminum-magnesium spinel.
Example 9
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 7:1 on a conveyor belt, wherein the thickness of the fine powder is 4 mm, and preheating the fine powder to 65 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 25 minutes to obtain uniform slurry, wherein the solid content of the slurry is 35 wt%, and the temperature of the slurry is 45 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 28 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1350 ℃, preserving the heat for 2.5 hours at the temperature, and naturally cooling to obtain the aluminum-rich aluminum-magnesium spinel.
Example 10
Flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with a mass ratio of 4:1 on a conveying belt, wherein the thickness of the fine powder is 5 mm, and preheating the fine powder to 75 ℃ through a mesh belt kiln; spraying the preheated fine powder into slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, stirring for 25 minutes to obtain uniform slurry, wherein the solid content of the slurry is 25 wt%, and the temperature of the slurry is 35 ℃; sending the slurry into a plate blank filter press for filter pressing, wherein the water content of a filter cake obtained after filter pressing is 25 wt%; and (3) sending the filter cake to a tunnel kiln for pretreatment, then calcining to 1300 ℃, preserving the heat for 2.5 hours at the temperature, and naturally cooling to obtain the aluminum-rich aluminum-magnesium spinel.
Comparative example
The fine gamma-phase alumina powder and the fine crystalline magnesium chloride powder which are the same as those in the examples 1 to 10 are used as raw materials, aluminum chloride is used as an additive, the fine gamma-phase alumina powder, the crystalline magnesium chloride and the aluminum chloride are uniformly mixed according to the mass ratio of 100:10:1.5, then the mixture is put into a sagger, the mixture is heated to 1520 ℃ in a tunnel kiln which is the same as those in the examples 1 to 10 for calcination, the temperature is kept for 8 hours, and then the mixture is naturally cooled to prepare the aluminum-rich magnesium spinel of the comparative example.
The alumina chemical content, the sodium oxide content and the grain diameter of the aluminum-rich magnesium spinel obtained in examples 1 to 10 and the comparative example were measured, and the results are shown in the following table.
TABLE 1 examination of Aluminumrich magnesium spinel
As can be seen from Table 1, the alumina chemical content of the alumina-rich magnesia spinel prepared by the method can reach more than 95 percent, which is slightly higher than that of the alumina of the comparative example; the impurity sodium oxide content of the aluminum-rich magnesium spinel prepared by the method can be reduced to be below 0.1 wt%, which is far lower than that of the impurity sodium oxide component of a comparative example; the grain diameter of the aluminum-rich magnesium aluminate spinel prepared by the invention is adjustable within the range of 0.5-1 micron, and the aluminum-rich magnesium aluminate spinel with different grain diameters can be obtained according to the combination of different calcination temperatures and different heat preservation times.
The preferred embodiments of the present invention have been described in detail with reference to the specific examples, however, the present invention is not limited to the details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications all fall within the scope of protection of the present invention.
Claims (5)
1. A preparation method of high-purity aluminum-rich magnesium spinel is characterized by comprising the following steps:
firstly, flatly paving gamma-phase alumina fine powder and crystalline magnesium chloride fine powder with the mass ratio of 4-7:1 on a conveyor belt, wherein the thickness of the gamma-phase alumina fine powder and the crystalline magnesium chloride fine powder is 3-10 mm, and preheating the gamma-phase alumina fine powder and the crystalline magnesium chloride fine powder to 60-80 ℃ through a mesh belt kiln;
spraying the preheated fine powder to slurry through a water curtain rich in carbon dioxide, then enabling the slurry to flow into a stirring barrel, and uniformly stirring to obtain slurry;
step three, feeding the slurry into a filter press, and performing filter pressing to obtain a filter cake with the water content of 20-40 wt%;
step four, sending the filter cake to a high-temperature kiln for pretreatment, then calcining to 1200-1400 ℃, carrying out heat preservation reaction at the temperature, and naturally cooling to obtain the aluminum-rich magnesium spinel;
wherein the impurity sodium oxide content of the gamma-phase alumina fine powder is less than or equal to 0.50 wt%, and the magnesium chloride content of the crystalline magnesium chloride fine powder is more than or equal to 46 wt%.
2. The process of claim 1 for preparing a high purity aluminum-rich magnesium spinel, wherein: in the second step, carbon dioxide gas is introduced into water and sprayed on the surface of the preheated fine powder to prepare slurry with the temperature of 30-50 ℃ and the solid content of 20-40 wt%.
3. The method for preparing high-purity aluminum-rich magnesium spinel according to claim 2, wherein the method comprises the following steps: the carbon dioxide gas is obtained by liquid carbon dioxide or dry ice, and the content of the carbon dioxide in the liquid carbon dioxide or the dry ice is more than or equal to 99.99 wt%.
4. A process for preparing a high purity aluminum enriched magnesium spinel according to any of claims 1-3, wherein: in the second step, the stirring time is 15-30 minutes.
5. The process of claim 4, wherein the aluminum-rich magnesium spinel has a high purity, and the process comprises the steps of: in the fourth step, the heat preservation time is 1-10 hours.
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