CN114873616B - Low-sodium alumina and preparation method thereof - Google Patents
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- C01F7/00—Compounds of aluminium
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Abstract
The application particularly relates to low-sodium aluminum oxide and a preparation method thereof, which belong to the technical field of aluminum oxide preparation, and the method comprises the following steps: pre-roasting aluminum hydroxide to obtain roasted aluminum oxide; mixing and pulping the calcined alumina and water to obtain slurry; introducing neutral gas into the slurry to perform a neutralization reaction, and then performing liquid-solid separation, washing and drying to obtain low-sodium aluminum oxide; wherein the components of the neutralization gas comprise carbon dioxide, the volume concentration of the carbon dioxide is 35-40%, and the pressure of the neutralization gas is 0MP-0.6MP; CO is introduced under the pressurized condition 2 The gas is used for removing sodium, the sodium oxide content of the product is low, and the washing liquid can be recycled, so that the method is environment-friendly.
Description
Technical Field
The application belongs to the technical field of aluminum oxide preparation, and particularly relates to low-sodium aluminum oxide and a preparation method thereof.
Background
The calcination raw material of the high-temperature alumina is aluminum hydroxide, and because the content of sodium oxide in the industrial common aluminum hydroxide is higher, a certain amount of beta-alumina is generated in the calcination process, so that the conversion speed and conversion rate of alpha-alumina are greatly reduced, meanwhile, the crystal grains of the alumina are coarsened, the crystal form is irregular, and the deformation of a corundum refractory product is caused by the change of the beta-alumina in the conversion process of the beta-alumina to the alpha-alumina at a high temperature. The higher the sodium oxide content, the poorer the high temperature alumina insulation properties and the lower the mechanical strength.
The low-sodium high-temperature alumina has the characteristics of low sodium oxide content, good sintering activity, rapid cooling and rapid heating resistance, difficult deformation, high product yield and the like, is widely applied to industries such as high-temperature porcelain, wear-resistant porcelain, electronic substrates, polished products, high-grade refractory materials and the like, and has very broad application prospect.
The current method for producing low-sodium high-temperature alumina mainly comprises the following steps: 1. after the industrial aluminum hydroxide is light burned, washing with distilled water or dilute hydrochloric acid and the like to remove sodium, and then roasting again, wherein in the method, the distilled water is used in a large amount, and acid radical ions such as chloride ions seriously corrode equipment; 2. hydrogen oxidationAluminium or aluminium oxide addition H 3 BO 3 、AlF 3 Mineralizers such as NH4F and the like are baked to remove alkali, sodium sublimates into kiln ash circulation in the method, the product quality is affected, and meanwhile, the tail gas treatment is difficult; 3. use H for industrial aluminium hydroxide 3 BO 3 Soaking with inorganic acid or salt such as hydrochloric acid and NH4Cl, pressing into blocks, calcining at high temperature, and pulverizing. The method for producing the low-sodium high-temperature alumina not only can increase the production cost of the product, but also can cause pollution to the environment.
Disclosure of Invention
The application aims to provide low-sodium alumina and a preparation method thereof, which solve the problem that the low-sodium alumina produced at present causes environmental pollution.
The embodiment of the application provides a preparation method of low-sodium aluminum oxide, which comprises the following steps:
pre-roasting aluminum hydroxide to obtain roasted aluminum oxide;
mixing and pulping the calcined alumina and water to obtain slurry;
introducing neutral gas into the slurry to perform a neutralization reaction, and then performing liquid-solid separation, washing and drying to obtain low-sodium aluminum oxide;
wherein the components of the neutralization gas comprise carbon dioxide, the volume concentration of the carbon dioxide is 35-40%, and the pressure of the neutralization gas is 0MP-0.6MP.
Optionally, the aeration speed of the neutralization gas is 20m 3 /h-100m 3 /h。
Optionally, the ventilation time of the neutralizing gas is 20min-40min.
Optionally, the roasting temperature of the pre-roasting is 650 ℃ to 900 ℃.
Optionally, the roasting time of the pre-roasting is 20min-60min.
Optionally, the particle size D50 of the calcined alumina is 50 μm to 110 μm, and the weight content of sodium oxide in the calcined alumina is less than 0.3%.
Optionally, the temperature of the slurry is 35 ℃ to 70 ℃.
Optionally, the slurry has a solid mass content of 200g/L to 400g/L.
Based on the same inventive concept, the embodiment of the application also provides low-sodium alumina, which is characterized in that the low-sodium alumina is prepared by adopting the preparation method of the low-sodium alumina.
Optionally, the weight content of sodium oxide in the low-sodium alumina is less than or equal to 0.04%.
One or more technical solutions in the embodiments of the present application at least have the following technical effects or advantages:
the embodiment of the application provides a preparation method of low-sodium aluminum oxide, which comprises the following steps: pre-roasting aluminum hydroxide to obtain roasted aluminum oxide; mixing and pulping the calcined alumina and water to obtain slurry; introducing neutral gas into the slurry to perform a neutralization reaction, and then performing liquid-solid separation, washing and drying to obtain low-sodium aluminum oxide; wherein the components of the neutralization gas comprise carbon dioxide, the volume concentration of the carbon dioxide is 35-40%, and the pressure of the neutralization gas is 0MP-0.6MP; CO is introduced under the pressurized condition 2 The gas is used for removing sodium, the sodium oxide content of the product is low, and the washing liquid can be recycled, so that the method is environment-friendly.
The foregoing description is only an overview of the present application, and is intended to be implemented in accordance with the teachings of the present application in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present application more readily apparent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of a method provided by an embodiment of the present application.
Detailed Description
The advantages and various effects of the present application will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the application, not to limit the application.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present application are commercially available or may be prepared by existing methods.
The technical scheme of the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
according to an exemplary embodiment of the present application, there is provided a method for preparing low sodium alumina, the method comprising:
s1, pre-roasting aluminum hydroxide to obtain roasted aluminum oxide;
s2, mixing and pulping the calcined alumina and water to obtain slurry;
s3, introducing neutral gas into the slurry to perform a neutralization reaction, and then performing liquid-solid separation, washing and drying to obtain low-sodium aluminum oxide; the components of the neutralizing gas comprise carbon dioxide, the volume concentration of the carbon dioxide is 35-40%, and the pressure of the neutralizing gas is 0MP-0.6MP.
The reason for controlling the volume concentration of the carbon dioxide to be 35-40% is based on the comprehensive consideration of the absorption rate and the neutralization reaction efficiency of the carbon dioxide, and the adverse effect of the excessive concentration is that the absorption rate of the carbon dioxide is low, a large amount of unreacted gas escapes, so that the production cost is increased and the choking risk exists; an adverse effect of too small is a decrease in production efficiency.
The reason for controlling the pressure of the neutralization gas to be 0MP-0.6MP is based on the comprehensive consideration of the absorption rate and the neutralization reaction efficiency of the carbon dioxide gas, and the adverse effect of the excessive pressure value is that the flow rate of the carbon dioxide gas is too high, and the contact time with the slurry is too short, so that the absorption rate of the carbon dioxide gas is too low; an excessively small adverse effect is that the contact surface of carbon dioxide gas with slurry is small, the gas stirring action is not obvious, the reaction efficiency is low, and the productivity is lowered.
As an alternative embodiment, the aeration rate of the neutralization gas is 20m 3 /h-100m 3 And/h, the ventilation time of the neutralizing gas is 20-40 min.
Generally, under a condition that the total ventilation amount is constant, the higher the ventilation speed, the shorter the required ventilation time, and the lower the ventilation speed, the longer the required ventilation time. Controlling the aeration rate of the neutralization gas to be 20m 3 /h-100m 3 The reason why the ventilation time is 20-40 min is based on the comprehensive consideration of production cost, production efficiency and sodium reduction effect, and the adverse effect of the excessive value is that a large amount of unreacted carbon dioxide gas escapes, so that the cost is increased; an excessively small adverse effect is low neutralization efficiency, insignificant sodium-lowering effect, resulting in reduced productivity;
as an alternative embodiment, the pre-baking temperature is 650-900 ℃ and the pre-baking time is 20-60 min.
Generally, the higher the firing temperature, the shorter the firing time required, and the lower the firing temperature, the longer the firing time required to achieve a certain firing effect. The reason for controlling the roasting temperature of the pre-roasting at 650-900 ℃ and the roasting time at 20-60 min is based on comprehensive consideration of the influence on the roasting alumina pore channels, and the adverse effect of overlarge value is that the sintering and sealing of partial pore channels of the roasting alumina are caused, so that the sodium reduction effect is influenced; the adverse effect of too small is that partial pore channels of the calcined alumina are not opened, and the sodium reduction effect is affected;
as an alternative embodiment, the calcined alumina has a particle size D50 of 50 μm to 110 μm and the sodium oxide content of the calcined alumina is < 0.3% by weight.
The reason for controlling the particle size D50 of the calcined alumina to be 50-110 mu m is that the calcining equipment has the particle size requirement on the calcined material, and the adverse effect of overlarge value is that insufficient calcining can be caused, and the adverse effect of overlarge value is that dust pollution is easily caused to the environment in the calcining process;
the reason for controlling the weight content of sodium oxide in the roasted aluminum hydroxide to be less than 0.3 percent is based on the comprehensive consideration of the sodium reduction effect and the production cost, the adverse effect of the excessive value is that the sodium reduction effect does not meet the requirement, and the adverse effect of the excessive value is that the raw material production cost is high;
as an alternative embodiment, the temperature of the slurry is between 35 ℃ and 70 ℃.
The reason for controlling the temperature of the slurry to be 35-70 ℃ is based on comprehensive consideration of the sodium reduction effect and the production cost, the adverse effect of the excessive value is that the high temperature can lead to the reduction of the carbon dioxide gas absorption rate, the temperature of the slurry can increase the production cost, the adverse effect of the excessive small value is that the solubility of sodium oxide in alumina is low at low temperature, the neutralization reaction speed is low, and the sodium reduction effect is poor;
as an alternative embodiment, the slurry has a solids mass content of 200g/L to 400g/L.
The reason for controlling the solid mass content of the slurry to be 200g/L-400g/L is based on the comprehensive consideration of production equipment and production efficiency, the adverse effect of the excessive value is that the solid content is too high, the industrialized pipeline transportation is limited, and the adverse effect of the too small value is that the production efficiency is low;
according to another exemplary embodiment of the present application, there is provided a low sodium alumina, characterized in that the low sodium alumina is prepared by the preparation method of the low sodium alumina provided above.
The low sodium alumina of the present application and the method for preparing the same will be described in detail with reference to examples, comparative examples and experimental data.
Example 1
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 700 ℃, the roasting time is 30 minutes, the granularity D50 is 78 mu m, and the sodium oxide content is 0.28 percent.
2) Mixing distilled water at room temperature of 50 ℃ with roasted alumina, pulping, controlling the solid content of slurry at 300g/l, stirring uniformly, introducing carbon dioxide gas with concentration of 35%, introducing gas with gas introducing amount of 1m3 slurry at 90m 3/h, maintaining the gas introducing pressure at 0.1MP for 20min, performing liquid-solid separation, and washing with hot distilled water to obtain low-sodium alumina, wherein Na2O in the low-sodium alumina product is less than 0.04%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Example 2
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 650 ℃, the roasting time is 60 minutes, the granularity D50 is 72 mu m, and the sodium oxide content is 0.25 percent.
2) Mixing distilled water at 60 ℃ and baked alumina, pulping, controlling the solid content of slurry at 350g/l, stirring uniformly, introducing 35% carbon dioxide gas, introducing 1m3 slurry gas with the gas introducing amount of 90m 3/h, introducing the gas with the gas introducing pressure of 0.2MP for 20 minutes, performing liquid-solid separation, washing with hot distilled water, and obtaining the low-sodium alumina, wherein Na2O in the low-sodium alumina product is less than 0.04%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Example 3
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 700 ℃, the roasting time is 0.5 hour, the granularity D50 is 90 mu m, and the sodium oxide content is 0.28 percent.
2) Mixing distilled water at 60 ℃ and baked alumina, pulping, controlling the solid content of slurry at 350g/l, stirring uniformly, introducing 35% carbon dioxide gas, introducing 1m3 slurry gas with the gas introducing amount of 60m 3/h, introducing the gas with the gas introducing pressure of 0.3MP, introducing the gas for 30 minutes, performing liquid-solid separation, and washing with hot distilled water to obtain the low-sodium alumina, wherein Na2O in the low-sodium alumina product is less than 0.04%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Example 4
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 850 ℃, the roasting time is 20 minutes, the granularity D50 is 74 mu m, and the sodium oxide content is 0.28 percent.
2) Mixing distilled water at 60 ℃ and baked alumina, pulping, controlling the solid content of slurry at 350g/l, stirring uniformly, introducing 35% carbon dioxide gas, introducing 1m3 slurry gas with the gas introducing amount of 60m 3/h, introducing the gas with the gas introducing pressure of 0.6MP, introducing the gas for 20 minutes, performing liquid-solid separation, and washing with hot distilled water to obtain the low-sodium alumina, wherein Na2O in the low-sodium alumina product is less than 0.04%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Comparative example 1
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 550 ℃, the roasting time is 60 minutes, the granularity D50 is 101 mu m, and the sodium oxide content is 0.28 percent.
2) Mixing distilled water at 16 ℃ and baked alumina, pulping, controlling the solid content of slurry at 350g/l, stirring uniformly, introducing 35% carbon dioxide gas, keeping the gas introducing amount of 1m3 slurry at 90m 3/h, keeping the gas introducing pressure at 0.1MP for 20 minutes, performing liquid-solid separation, washing with hot distilled water, and obtaining the low-sodium alumina, wherein Na2O in the low-sodium alumina product is 0.078%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Comparative example 2
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 650 ℃, the roasting time is 10 minutes, the granularity D50 is 68 mu m, and the sodium oxide content is 0.25 percent.
2) Mixing distilled water at 60 ℃ and baked alumina, pulping, controlling the solid content of slurry at 300g/l, stirring uniformly, introducing 35% carbon dioxide gas, introducing 1m3 slurry gas with the gas introducing amount of 90m 3/h, introducing the gas with the gas introducing pressure of 0.2MP for 30 minutes, performing liquid-solid separation, washing with hot distilled water, and obtaining the low-sodium alumina, wherein Na2O in the low-sodium alumina product is 0.085%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Comparative example 3
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 700 ℃, the roasting time is 90 minutes, the granularity D50 is 117 mu m, and the sodium oxide content is 0.3 percent.
2) Mixing distilled water at 60 ℃ and baked alumina, pulping, controlling the solid content of slurry at 350g/l, stirring uniformly, introducing 35% carbon dioxide gas, introducing 1m3 slurry gas with the gas introducing amount of 60m 3/h, introducing air under normal pressure for 20 minutes, performing liquid-solid separation, and washing with hot distilled water to obtain the low-sodium alumina, wherein Na2O in the low-sodium alumina product is 0.091%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Comparative example 4
A method for preparing low sodium alumina, comprising the steps of:
1) The preparation method of the low-sodium aluminum oxide takes common industrial aluminum hydroxide as a raw material, the roasting temperature is 850 ℃, the roasting time is 20 minutes, the granularity D50 is 52 mu m, and the sodium oxide content is 0.447 percent.
2) Mixing distilled water at 60 ℃ and baked alumina, pulping, controlling the solid content of slurry at 350g/l, stirring uniformly, introducing 35% carbon dioxide gas, introducing 1m3 slurry gas with the gas introducing amount of 90m 3/h, introducing the gas with the gas introducing pressure of 0.2MP for 20 minutes, performing liquid-solid separation, washing with hot distilled water, and obtaining the low-sodium alumina, wherein Na2O in the low-sodium alumina product is 0.067%.
3) Calcining at 1350 ℃ for 3 hours to obtain the low-sodium high-temperature alumina.
Na of Low sodium high temperature alumina prepared in examples 1 to 4 and comparative examples 1 to 4 2 The weight content of O is shown in the following table:
| Na 2 o weight content | |
| Example 1 | ≤0.04％ |
| Example 2 | ≤0.04％ |
| Example 3 | ≤0.04％ |
| Example 4 | ≤0.04％ |
| Comparative example 1 | 0.078％ |
| Comparative example 2 | 0.085％ |
| Comparative example 3 | 0.092％ |
| Comparative example 4 | 0.067％ |
From the above table, na in the low-sodium alumina prepared by the method provided by the embodiment of the application 2 The weight content of O is controlled to be less than or equal to 0.04%, and when a certain parameter is not in the embodiment of the application, na in the obtained low-sodium alumina can appear 2 And the weight content of O is higher.
One or more technical solutions in the embodiments of the present application at least have the following technical effects or advantages:
(1) The method provided by the embodiment of the application is simple and feasible, is easy to implement, reduces the sodium oxide content of the alumina from 0.28% to below 0.04%, has less washing water consumption, can be recycled, can reduce the cost, and is beneficial to industrialized popularization and application;
(2) The method provided by the embodiment of the application uses the low-sodium alumina as the raw material to obtain the low-sodium high-temperature alumina after calcination, and mineralizer is not used in the high-temperature calcination process, so that secondary pollution to the product is avoided, the method is environment-friendly, and the product has uniform crystal grains, is easy to sinter and is easy to crush. The preparation method of the low-sodium aluminum oxide has the advantages of low washing water consumption, simple production process and easy implementation;
(3) The method provided by the embodiment of the application introduces CO under the pressurizing condition 2 The gas is used for removing sodium, the sodium oxide content of the product is low, and the washing liquid can be recycled, so that the method is environment-friendly.
Finally, it is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (2)
1. A method for preparing low sodium alumina, the method comprising:
pre-roasting aluminum hydroxide to obtain roasted aluminum oxide;
mixing and pulping the calcined alumina and water to obtain slurry;
introducing neutral gas into the slurry to perform a neutralization reaction, and then performing liquid-solid separation, washing and drying to obtain low-sodium alumina, wherein the weight content of sodium oxide in the low-sodium alumina is less than or equal to 0.04%;
wherein the components of the neutralization gas comprise carbon dioxide, the volume concentration of the carbon dioxide is 35-40%, and the pressure of the neutralization gas is 0MP-0.6MP;
the aeration rate of the neutralization gas is 20m 3 /h-100m 3 /h；
The ventilation time of the neutralizing gas is 20min-40min;
the roasting temperature of the pre-roasting is 650-900 ℃;
the roasting time of the pre-roasting is 20min-60min;
the granularity D50 of the calcined alumina is 50-110 mu m, and the weight content of sodium oxide in the calcined alumina is less than 0.3%;
the temperature of the slurry is 35-70 ℃.
2. The method for producing low-sodium alumina according to claim 1, wherein the slurry has a solid mass content of 200g/L to 400g/L.
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| CN102070168A (en) * | 2010-12-08 | 2011-05-25 | 中国铝业股份有限公司 | Method for reducing sodium oxide in aluminum oxide by using carbon dioxide |
| CN109761254A (en) * | 2019-02-02 | 2019-05-17 | 中国铝业股份有限公司 | A method of reducing aluminium hydroxide or sodium oxide in aluminum oxide impurity content |
| CN113233877A (en) * | 2021-05-12 | 2021-08-10 | 中铝山东有限公司 | Sodium removal method for calcining alpha alumina |
| CN113716590A (en) * | 2021-10-25 | 2021-11-30 | 中铝山东工程技术有限公司 | Process for removing sodium oxide impurities in aluminum oxide |
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