CN113233877A - Sodium removal method for calcining alpha alumina - Google Patents
Sodium removal method for calcining alpha alumina Download PDFInfo
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- CN113233877A CN113233877A CN202110515799.8A CN202110515799A CN113233877A CN 113233877 A CN113233877 A CN 113233877A CN 202110515799 A CN202110515799 A CN 202110515799A CN 113233877 A CN113233877 A CN 113233877A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
Abstract
The invention particularly relates to a sodium removal method for calcining alpha alumina, belonging to the technical field of inorganic non-metallic material synthesis, and the method comprises the following steps: subjecting industrial alumina to CO2Washing and pretreating to obtain a pretreated raw material; mixing the pretreated raw material with a sodium removal agent and a mineralizer to obtain a calcined mixture; calcining the calcined mixture to obtain sodium-removed alpha alumina; provides a two-stage deep sodium removal process for calcining alpha alumina, and the product Na2O can reach up to 0.04%, alpha-Al2O3The content can reach 95-98%, which not only improves the product quality and reduces the usage amount of the mineralizer, but also reduces the adverse effect of the mineralizer on the environment and the product.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metallic material synthesis, and particularly relates to a sodium removal method for calcining alpha alumina.
Background
The advanced ceramic has the advantages of high strength, corrosion resistance, high temperature resistance, insulation, superconductivity, biocompatibility and the like due to the specific fine structure, is widely applied to the fields of national defense, chemical engineering, electronics, machinery, aerospace, biomedicine and the like, and is an industry which is mainly supported and developed in China in recent years. Calcined alpha alumina powder is an irreplaceable key base material for advanced ceramics.
Na2The O content is an important technical index for calcining alpha alumina products, Na2The content of 0 directly influences the application performance of the alumina ceramics and the refractory products. Na (Na)2O can form sodium aluminate in the calcining process, the alpha conversion rate of the alumina powder is reduced, the activity of the powder is reduced, the physicochemical properties of the product are further influenced, and the alumina product is easy to deform and crack in downstream application, and in contrast, Na2The lower the O content, the lower the temperature in the ceramic sintering, the easy sintering shrinkage becomes dense ceramic body, can be widely used in advanced ceramic field.
At present, sodium removal is generally carried out by a single means in domestic and foreign industrial production, for example, the sodium removal is carried out by adding hydrochloric acid and dust collecting materials through open-circuit washing or adding mineralizer, but the effect is limited, and Na exists in the product2High content of O, alpha-Al2O3Low content, wide distribution of original grain size, high re-sintering shrinkage and the like, and is difficult to reach Na20<0.04％，α-Al2O3The content is generally 80-90%, and the product can only be applied to the middle and low-end fields of grinding media, refractory materials and the like. And the use of large amount of mineralizer causes great side effect to the calcining equipment and the production and application of alumina ceramic products. The sodium removal under the vacuum condition has rigorous equipment requirements and higher cost, and is difficult to realize large-scale industrial production.
Disclosure of Invention
In view of the above problems, the present invention has been made to provide a method for sodium removal of calcined alpha alumina that overcomes or at least partially solves the above problems.
The embodiment of the invention provides a sodium removal method for calcining alpha alumina, which comprises the following steps:
subjecting industrial alumina to CO2Washing and pretreating to obtain a pretreated raw material;
mixing the pretreated raw material with a sodium removal agent and a mineralizer to obtain a calcined mixture;
and calcining the calcined mixture to obtain the sodium-removed alpha alumina.
Optionally, the content of sodium oxide in the pretreated raw material is controlled to be 0.1-0.14% by weight fraction.
Optionally, the sodium removing agent is a quartz deep sodium removing agent, the adding amount of the quartz deep sodium removing agent is 0.1% -10% of the adding amount of the industrial alumina, and the particle size of the quartz deep sodium removing agent is 20-30 meshes.
Optionally, the SiO in the quartz deep sodium removal agent is calculated by weight fraction2Accounting for more than 50 percent.
Optionally, the mineralizer is a halogen compound; the addition amount of the halogen compound is 0.01-5% of the addition amount of the industrial alumina in terms of weight fraction.
Optionally, the halogen compound is a fluorine compound and/or a chlorine compound.
Optionally, the fluorine compound comprises at least one of aluminum fluoride, ammonium fluoride and calcium fluoride; the chlorine compound includes at least one of ammonium chloride and magnesium chloride.
Optionally, the calcined mixture is calcined to obtain the sodium-removed alpha alumina, the calcining temperature is controlled to be 1300-1500 ℃, and the calcining time is controlled to be 20-60 min.
Optionally, the content of sodium oxide in the industrial alumina is 0.35-0.50% by weight.
Optionally, mixing the solid form of the sodium removal agent with the pretreated feedstock; the mineralizer is mixed with the pretreated feedstock in solid or liquid form.
One or more technical schemes in the invention at least have the following technical effects or advantages:
the invention provides a sodium removal method for calcining alpha alumina, which comprises the following steps: subjecting industrial alumina to CO2Washing and pretreating to obtain a pretreated raw material; mixing the pretreated raw material with a sodium removal agent and a mineralizer to obtain a calcined mixture; calcining the calcined mixture to obtain sodium-removed alpha alumina; provides a two-stage deep sodium removal process for calcining alpha alumina, and the product Na2O can reach up to 0.04%, alpha-Al2O3The content can reach 95-98%, which not only improves the product quality and reduces the usage amount of the mineralizer, but also reduces the adverse effect of the mineralizer on the environment and the product.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a flow chart of a method provided by an embodiment of the present invention;
fig. 2 is a block diagram of a method provided by an embodiment of the invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings 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 invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In order to solve the technical problems, the general idea is as follows:
in order to improve the chemical purity of the calcined alpha alumina powder, the applicant studied Na2O in gamma-Al2O3The occurrence state in the process and the sodium removal reaction mechanism under different conditions, provides a high-efficiency, low-cost and environment-friendly two-stage deep sodium removal technology, and can remove Na2O is reduced to less than 0.04 percent, alpha-Al2O3The content can reach 95-98%.
According to an exemplary embodiment of the present invention, there is provided a sodium removal method for calcining alpha alumina, the method including:
s1, carrying out CO treatment on industrial alumina2Washing and pretreating to obtain a pretreated raw material; it is to be noted that CO2The specific operation of the washing pretreatment is as follows: the alumina enters a pulping groove for pulping, and pulping liquid is sent into a Venturi reactor through a pump to be mixed with CO2The gases are mixed thoroughly and sodium is removed in a pipeline.
As an alternative embodiment, the content of sodium oxide in the pretreated raw material is controlled to be 0.1-0.14% by weight fraction.
The reason for controlling the sodium oxide content in the pretreated raw material to be 0.1-0.14% is that the lower the sodium oxide content in the pretreated raw material is, the more beneficial the subsequent calcination sodium removal is, the better the subsequent sodium removal effect is, the higher the quality stability is, the better the economy is, the adverse effect of the overlarge content value is that the higher the sodium oxide content in the pretreated raw material is, the more adverse the subsequent quartz sodium removal is, and the worse the sodium removal effect is.
S2, mixing the pretreated raw material with a sodium removal agent and a mineralizer to obtain a calcined mixture;
as an optional embodiment, the sodium removing agent is a quartz deep sodium removing agent, in this application, the quartz deep sodium removing agent may specifically be silica-containing substances such as quartz sand, flint clay, mullite, and the like, and the above list of the quartz deep sodium removing agent is only used to illustrate that the present invention can be implemented, and is not limited to the present invention2Above 870 ℃ the stable phase quartz is converted into high-activity quartz, SiO2The phase change of the crystal particles causes the surface area of the crystal particles to be abnormally increased and the activity to be rapidly increased, and the crystal particles can efficiently adsorb gaseous sodium ions and react with the gaseous sodium ions to generate sodium silicate or sodium aluminosilicate, so that the sodium ions and alumina are removed and separated, and finally the deep purification is realized, wherein the adding amount of the quartz deep sodium remover is 0.1-10% of the adding amount of the industrial alumina (calculated by weight percentage), and the granularity of the quartz deep sodium remover is 20-30 meshes.
The reason for controlling the adding amount of the quartz deep sodium removing agent to be 0.1-10% of the adding amount of the industrial alumina is that the quartz sodium removing agent in the range is adopted, the sodium removing effect and the economy are optimal, the adverse effect of overlarge content value is that the cost is increased, the economy is influenced, the subsequent screening operation is inconvenient, the sodium removing effect is poor, and the sodium content cannot reach the required index.
The particle size of the quartz deep sodium removal agent is controlled to be 20-30 meshes, the adverse effect of overlarge particle size is that the adsorption of sodium oxide in the calcining process is not facilitated, the reaction of the sodium removal agent and the sodium oxide is influenced, the sodium removal effect is poor, the adverse effect of undersize is that the quartz deep sodium removal agent is easy to crush in the calcining process, and is not easy to separate from a product in the later period, so that silicon pollution is easily caused, and the product quality is influenced.
As an alternative embodiment, the quartz is deeply sodium depleted in parts by weightSiO in agent2Accounting for more than 50 percent.
SiO in sodium removal agent for controlling depth of quartz2The reason why the silicon dioxide accounts for more than 50 percent is that the silicon dioxide is an effective component for sodium removal, the content cannot be too low, and the adverse effect of the excessively small proportion is that the smaller the proportion is, the smaller the surface area of exposed silicon-containing particles is, the lower the sodium-alkali removal rate is, and the poor sodium removal effect of the alpha-alumina is caused.
In an alternative embodiment, the mineralizer is a halogen compound, and the mineralizer is added in an amount of 0.01-5% of the raw material by weight fraction. The halogen compound is a fluorine compound and/or a chlorine compound; the fluorine compound includes at least one of aluminum fluoride, ammonium fluoride, and calcium fluoride; the chlorine compound includes at least one of ammonium chloride and magnesium chloride, and specifically, may be selected from one or more of aluminum fluoride and ammonium fluoride, calcium fluoride, ammonium chloride, and magnesium chloride.
The reason for controlling the addition of the halogen compound to be 0.01-5% of the addition of the industrial alumina is to facilitate sodium oxide removal, reduce the phase inversion temperature of alpha alumina and control the primary grain size of the alpha alumina, and the adverse effect of overlarge addition value is that the excessive calcination auxiliary agent causes abnormal growth of the primary grain size and is corrosive to equipment, and the adverse effect of undersize is that the sodium removal effect is not obvious and the mineralization calcination effect cannot be achieved.
And S3, calcining the calcined mixture, naturally cooling after the calcination is finished, and sieving and separating the product and the reacted quartz deep sodium removal agent by using a 40-mesh sieve to obtain the sodium-removed alpha-alumina.
As an optional embodiment, the calcined mixture is calcined to obtain the sodium-removed alpha alumina, the calcining temperature is controlled to be 1300-1500 ℃, and the calcining time is controlled to be 20-60 min.
The calcination temperature is controlled to be 1300-1500 ℃, and the calcination time is controlled to be 20-60min because the crystal grain growth of the alpha alumina is fast at high temperature, under the condition of ensuring complete crystal phase conversion, the retention time of the material in a sintering zone is shortened as much as possible, the adverse effect of excessively taking the crystal phase is to increase the energy consumption to cause the cost rise, and the adverse effect of excessively taking the crystal phase is to cause insufficient crystal phase conversion and incomplete crystal grain development.
The quartz deep sodium removal agent is added in a solid form, is present in a solid form before and during calcination, and the mineralizer can be added in a solid or liquid form, and both need to be uniformly mixed with the raw materials before calcination, and the Na of the alpha alumina can be added by controlling the adding amount of the quartz deep sodium removal agent and the mineralizer2O content and alpha-Al2O3The content is controlled, generally Na2The content of O is stabilized below 0.04 percent, and alpha-Al2O3The content can reach 95-98%.
The method for removing sodium from calcined alpha alumina according to the present application will be described in detail below with reference to examples, comparative examples and experimental data, and it should be noted that the following example may not only represent one experiment but may represent a group of experiments.
Example 1
A method of sodium removal for calcining alpha alumina, the method comprising:
s1, using industrial alumina A (Na)2O content of 0.35-0.5%) as raw material, and performing CO treatment2Washing to remove sodium (Na)2O content reduced to 0.15%);
s2, adding 0.05-1% of aluminum fluoride (the addition amount accounts for the weight percent of the aluminum oxide), wherein the aluminum fluoride is added in a solid form;
s3, uniformly mixing aluminum fluoride and the acid-washed alumina raw material to obtain a calcined mixture, and calcining the calcined mixture in a rotary kiln at the temperature of 1300 ℃ and 1500 ℃ for 20-60 min;
s4, after calcination, naturally cooling, and sieving and separating the product and the reacted quartz deep sodium removal agent by a 40-mesh sieve.
Example 2
A method of sodium removal for calcining alpha alumina, the method comprising:
s1, using industrial alumina A (Na)2O content of 0.35-0.5%) as raw material, and performing CO treatment2Washing to remove sodium (Na)2O content reduced to 0.15%);
s2, adding 0.1-2% of quartz deep sodium removal agent and 0.05-1% of aluminum fluoride (the addition amount accounts for the weight percent of aluminum oxide), wherein the quartz deep sodium removal agent is added in a solid particle form, and the aluminum fluoride is added in a solid form;
s3, uniformly mixing the quartz deep sodium removal agent, the mineralizer and the acid-washed alumina raw material to obtain a calcined mixture, and calcining the calcined mixture in a rotary kiln at the temperature of 1300 ℃ and 1500 ℃ for 20-60 min;
s4, after calcination, naturally cooling, and sieving and separating the product and the reacted quartz deep sodium removal agent by a 40-mesh sieve.
Comparative example 1
A method of sodium removal for calcining alpha alumina, the method comprising:
s1, using industrial alumina A (Na)2O content of 0.35-0.5%) as raw material;
s2, adding 0.05-1% of aluminum fluoride (the addition amount accounts for the weight percent of the aluminum oxide), wherein the aluminum fluoride is added in a solid form;
s3, uniformly mixing a mineralizer with the raw materials to obtain a calcined mixture; calcining in a rotary kiln at the temperature of 1300-1500 ℃ for 20-60 min;
s4, after calcination, naturally cooling, and sieving and separating the product and the reacted quartz deep sodium removal agent by a 40-mesh sieve.
Comparative example 2
A method of sodium removal for calcining alpha alumina, the method comprising:
s1, using industrial alumina A (Na)2O content of 0.35-0.5%) as raw material;
s2, adding 0.1-2% of quartz deep sodium removal agent and 0.05-1% of aluminum fluoride (the addition amount accounts for the weight percent of aluminum oxide), wherein the quartz deep sodium removal agent is added in a solid particle form, and the aluminum fluoride is added in a solid form;
s3, uniformly mixing a mineralizer, a quartz deep sodium removal agent and an industrial alumina raw material to obtain a calcined mixture, and calcining the calcined mixture in a rotary kiln at the temperature of 1300 ℃ and 1500 ℃ for 20-60 min;
s4, after calcination, naturally cooling, and sieving and separating the product and the reacted quartz deep sodium removal agent by a 40-mesh sieve.
Experimental example:
the alpha alumina prepared in examples 1-2 and comparative examples 1-2 was examined and the results are shown in the following table.
| Na2Content of O | α-Al2O3Content (wt.) | Primary grain size | |
| Example 1 | About 0.1 percent | 92％ | About 2.4 mu m |
| Example 2 | ＜0.04％ | 95％-98％ | About 2.1 μm |
| Comparative example 1 | About 0.35 percent | 90％ | About 2.8 mu m |
| Comparative example 2 | About 0.25 percent | 92％ | About 2.4 mu m |
From the above table, it can be seen that Na in the alpha alumina prepared by the method of the present invention2The content of O is easily realized to be less than 0.04 percent, and the content of alpha-Al is easily realized2O3The content can reach 95-98%, which can be obtained by comparing the data of comparative examples 1 and 2 with the data of the examples, when CO is not carried out2In the washing pretreatment, Na2High content of O and alpha-Al2O3The content is low.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) the method provided by the invention carries out CO treatment on common industrial alumina raw materials2Washing pretreatment and quartz deep sodium removal are carried out to obtain Na in alpha alumina2The content of O is easily realized to be less than 0.04 percent, and the content of alpha-Al is easily realized2O3The content can reach 95-98%;
(2) the method provided by the invention reduces the usage amount of the mineralizer, further reduces the adverse effects of the mineralizer on the environment and products, and simultaneously, the quartz deep sodium removal agent can be recycled, thereby reducing the production cost;
(3) the alpha alumina product prepared by the method has high chemical purity (Na)2O can reach within 0.04 percent), alpha-Al2O3High content (up to 95-98%), good fluidity, controllable primary grain size and other excellent physical and chemical properties, lower temperature in ceramic sintering, easy sintering and shrinkage into a compact ceramic body, and can be applied in advanced ceramic middle and high-end fields.
Finally, it should also be 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 invention 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. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A method of sodium removal for calcining alpha alumina, the method comprising:
subjecting industrial alumina to CO2Washing and pretreating to obtain a pretreated raw material;
mixing the pretreated raw material with a sodium removal agent and a mineralizer to obtain a calcined mixture;
and calcining the calcined mixture to obtain the sodium-removed alpha alumina.
2. The method for sodium removal from calcined alpha alumina as claimed in claim 1, wherein the sodium oxide content in the pretreated feedstock is controlled to be 0.1% to 0.14% by weight fraction.
3. The method for sodium removal from calcined alpha alumina as claimed in claim 1, wherein the sodium removal agent is a quartz deep sodium removal agent, the addition amount of the quartz deep sodium removal agent is 0.1% -10% of the addition amount of the industrial alumina by weight fraction, and the particle size of the quartz deep sodium removal agent is 20-30 meshes.
4. The method of claim 1, wherein the silica deep delicacy agent comprises SiO in weight fraction2Accounting for more than 50 percent.
5. The process for the sodium removal of calcined alpha alumina as claimed in claim 1, wherein the mineralizer is a halogen compound; the addition amount of the halogen compound is 0.01-5% of the addition amount of the industrial alumina in terms of weight fraction.
6. The method for sodium removal from calcined alpha alumina of claim 5 wherein the halogen compound is a fluorine compound and/or a chlorine compound.
7. The method of claim 6, wherein the fluorine compound comprises at least one of aluminum fluoride, ammonium fluoride, and calcium fluoride; the chlorine compound includes at least one of ammonium chloride and magnesium chloride.
8. The method for sodium removal by calcination of alpha alumina according to claim 1, wherein the calcination mixture is calcined to obtain sodium-removed alpha alumina, the calcination temperature is controlled to be 1300-1500 ℃, and the calcination time is controlled to be 20-60 min.
9. The process for the sodium removal of calcined alpha alumina as claimed in claim 1, wherein the commercial alumina has a sodium oxide content of 0.35% to 0.50% by weight fraction.
10. The sodium removal process for calcining alpha alumina as claimed in claim 1, wherein the solid form of the sodium removal agent is mixed with the pretreated feedstock; the mineralizer is mixed with the pretreated feedstock in solid or liquid form.
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| CN114455619A (en) * | 2022-01-12 | 2022-05-10 | 中铝山东新材料有限公司 | Low-sodium small primary crystal alpha alumina and preparation method thereof |
| CN114873616A (en) * | 2022-06-13 | 2022-08-09 | 中国铝业股份有限公司 | Low-sodium alumina and preparation method thereof |
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| CN114873616B (en) * | 2022-06-13 | 2023-10-03 | 中国铝业股份有限公司 | Low-sodium alumina and preparation method thereof |
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