CN116081663A - Preparation method of low-sodium microcrystalline alpha-alumina - Google Patents
Preparation method of low-sodium microcrystalline alpha-alumina Download PDFInfo
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- CN116081663A CN116081663A CN202310046438.2A CN202310046438A CN116081663A CN 116081663 A CN116081663 A CN 116081663A CN 202310046438 A CN202310046438 A CN 202310046438A CN 116081663 A CN116081663 A CN 116081663A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000011734 sodium Substances 0.000 title claims abstract description 44
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 74
- 238000005406 washing Methods 0.000 claims abstract description 35
- 239000012065 filter cake Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000002253 acid Substances 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 20
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001948 sodium oxide Inorganic materials 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 description 24
- 238000004537 pulping Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- -1 aluminum alkoxide Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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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
- C01F7/021—After-treatment of oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The application relates to a preparation method of low-sodium microcrystalline alpha-alumina, which comprises the following steps: providing an alumina raw material, and mixing the alumina raw material with hydrated pulp to obtain first pulp; adding a first acid agent for dissolving sodium oxide into the first slurry to obtain a second slurry; filtering and washing the second slurry to obtain a first filter cake; calcining the first filter cake at a preset temperature, and cooling to obtain an alumina intermediate; mixing the alumina intermediate with hydrated slurry to obtain second slurry; stirring, filtering and washing the second slurry to obtain a second filter cake; drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina. The method not only obtains the microcrystalline alpha-alumina with sodium oxide less than 0.02 percent and grain size less than 1 mu m, but also is equivalent to only adding the steps of reslurrying, washing and drying compared with the traditional acid washing and calcining method, and has lower production cost and simpler process.
Description
Technical Field
The present application relates to the field of aluminum industry, and in particular to microcrystalline alpha-alumina.
Background
Microcrystalline alpha-alumina is an important base material and is widely applied to the fields of functional ceramics, refractory materials, special glass, polishing and the like due to the excellent chemical stability, hardness and electrical insulation property. With the gradual increase of the requirements of the fields on the product performance, the requirements on raw materials are also higher and higher, wherein the requirements on the sodium oxide content and the primary grain size are gradually refined.
The traditional pickling and calcining method for preparing the microcrystalline alpha-alumina cannot simultaneously ensure that sodium oxide is less than or equal to 0.02 percent and the primary grain size is less than or equal to 1 mu m, and has higher alpha phase content. In order to control the content of sodium oxide and control the primary crystal, a plurality of methods including a sol-gel method, a hydrothermal synthesis method, an aluminum alkoxide hydrolysis method and the like are proposed, but the methods have high production cost and complex process, and are difficult to realize large-scale and low-cost production.
Disclosure of Invention
The embodiment of the application provides a preparation method of low-sodium microcrystalline alpha-alumina, which aims to solve the technical problems of high production cost and complex process of the existing microcrystalline alpha-alumina.
The embodiment of the application provides a preparation method of low-sodium microcrystalline alpha-alumina, which comprises the following steps:
providing an alumina raw material, and mixing the alumina raw material with hydrated pulp to obtain first pulp;
adding a first acid agent for dissolving sodium oxide into the first slurry to obtain a second slurry;
filtering and washing the second slurry to obtain a first filter cake;
calcining the first filter cake at a preset temperature, and cooling to obtain an alumina intermediate;
mixing the alumina intermediate with hydrated slurry to obtain second slurry;
stirring, filtering and washing the second slurry to obtain a second filter cake;
drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina.
In some embodiments of the present application, the mixing the alumina feedstock with a hydrated slurry, wherein the mass of water used for slurrying is 2-5 times that of the alumina feedstock.
In some embodiments of the present application, the first acid agent is at least one of acetic acid, oxalic acid, and hydrochloric acid.
In some embodiments of the present application, the second slurry is filtered, washed, wherein the mass of wash water does not exceed 3 times the solids in the second slurry.
In some embodiments of the present application, the predetermined temperature is 1200-1600 ℃.
In some embodiments of the present application, the alumina intermediate is combined with the hydrated slurry while a second acid agent is also added.
In some embodiments of the present application, the second acid agent is carbon dioxide.
In some embodiments of the present application, the combining the alumina intermediate with a hydrated slurry, the slurrying water is 2-5 times the mass of the alumina intermediate.
In some embodiments of the present application, the agitation time is 0.2-2 hours.
In some embodiments of the present application, the second slurry is stirred, filtered, washed, wherein the mass of wash water does not exceed 3 times the solids content of the second slurry.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the preparation method of the low-sodium microcrystalline alpha-alumina, firstly, sodium oxide in an alumina raw material is dissolved through a first acid agent, so that sodium content in the alumina is reduced; then forming an alumina intermediate rich in alpha-alumina by calcination, and pulping the alumina intermediate again to reduce the granularity of the alpha-alumina; and then the sodium content is further reduced by means of stirring and washing after filtering, and finally the obtained second filter cake is dried to obtain the low-sodium microcrystalline alpha-alumina. The method not only obtains the microcrystalline alpha-alumina with sodium oxide less than 0.02 percent and grain size less than 1 mu m, but also is equivalent to only adding the steps of reslurrying, washing and drying compared with the traditional acid washing and calcining method, and has lower production cost and simpler process.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic flow chart of a preparation method of low-sodium microcrystalline α -alumina according to an embodiment of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
Unless specifically stated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Thus, 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 specifically indicated otherwise, the various raw materials, reagents, instruments, equipment, and the like used in this application are commercially available or may be prepared by existing methods.
The existing microcrystalline alpha-alumina has the technical problems of high production cost and complex process.
The technical scheme provided by the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
an embodiment of the present application provides a method for preparing low-sodium microcrystalline α -alumina, referring to fig. 1, the method for preparing low-sodium microcrystalline α -alumina includes the following steps:
s1: providing an alumina raw material, and mixing the alumina raw material with hydrated pulp to obtain first pulp;
s2: adding a first acid agent for dissolving sodium oxide into the first slurry to obtain a second slurry;
s3: filtering and washing the second slurry to obtain a first filter cake;
s4: calcining the first filter cake at a preset temperature, and cooling to obtain an alumina intermediate;
s5: mixing the alumina intermediate with hydrated slurry to obtain second slurry;
s6: stirring, filtering and washing the second slurry to obtain a second filter cake;
s7: drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina.
The first acid agent can be any acid substance which is favorable for dissolving sodium oxide, such as acid, salt and oxide, wherein the acid can be hydrochloric acid, nitric acid and sulfuric acid, the salt can be ammonium chloride and ammonium bisulfate, and the oxide can be SO 2 、SO 3 。
As will be understood by those skilled in the art, slurrying refers to slurrying an alumina feedstock with water. The concrete method of slurrying can be, for example, ball milling with water, stirring and the like.
As will be appreciated by those skilled in the art, the first acid agent serves to dissolve sodium oxide impurities incorporated in the alumina feedstock into the solution, reducing the sodium content in the alumina.
The content of alpha-alumina in the alumina intermediate obtained after calcination in step S4 generally reaches 90-97%.
Firstly, dissolving sodium oxide in an alumina raw material through a first acid agent to reduce sodium content in the alumina; then forming an alumina intermediate rich in alpha-alumina by calcination, and pulping the alumina intermediate again to reduce the granularity of the alpha-alumina; and then the sodium content is further reduced by means of stirring and washing after filtering, and finally the obtained second filter cake is dried to obtain the low-sodium microcrystalline alpha-alumina. The method not only obtains the microcrystalline alpha-alumina with sodium oxide less than 0.02 percent and grain size less than 1 mu m, but also is equivalent to only adding the steps of reslurrying, washing and drying compared with the traditional acid washing and calcining method, and has lower production cost and simpler process.
In some embodiments of the present application, the mixing the alumina feedstock with a hydrated slurry, wherein the mass of water used for slurrying is 2-5 times that of the alumina feedstock.
The mass of the water for the slurry is 2-5 times of that of the alumina raw material, so that sufficient water can be provided to ensure the dispersion effect of the alumina, and the subsequent filtering difficulty caused by too much water can be avoided.
In some embodiments of the present application, the first acid agent is at least one of acetic acid, oxalic acid, and hydrochloric acid.
In some embodiments of the present application, the second slurry is filtered, washed, wherein the mass of wash water does not exceed 3 times the solids in the second slurry.
The mass of wash water is 3 times the mass of solids in the second slurry sufficient for adequate washing. Excessive washing water causes alumina loss, and excessive water consumption causes cost increase.
In some embodiments of the present application, the predetermined temperature is 1200-1600 ℃.
It will be appreciated by those skilled in the art that the above calcination temperatures are advantageous for the formation of alpha-alumina.
In some embodiments of the present application, the alumina intermediate is combined with the hydrated slurry while a second acid agent is also added.
In some embodiments of the present application, the second acid agent is carbon dioxide.
The sodium oxide in the alumina can be further removed by introducing carbon dioxide; carbon dioxide is weak in acidity, volatile, pollution-free, and can be removed even if the carbon dioxide remains after being dried in the step S7.
In some embodiments of the present application, the combining the alumina intermediate with a hydrated slurry, the slurrying water is 2-5 times the mass of the alumina intermediate.
The mass of the water for the slurry is 2-5 times of that of the alumina intermediate, so that sufficient water can be provided to ensure the dispersion effect of the alumina, and the subsequent filtering difficulty caused by too much water can be avoided.
In some embodiments of the present application, the agitation time is 0.2-2 hours.
Too short a stirring time is detrimental to the adequate dispersion and cleaning of the alumina. The production efficiency is affected if the stirring and washing time is too long.
In some embodiments of the present application, the second slurry is stirred, filtered, washed, wherein the mass of wash water does not exceed 3 times the solids content of the second slurry.
The mass of wash water is 3 times the solids content of the second slurry sufficient for adequate washing. Excessive washing water causes alumina loss, and excessive water consumption causes cost increase.
The present application is further illustrated below in conjunction with specific embodiments. It should be understood that these examples are illustrative only of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
The embodiment provides a method for preparing low-sodium microcrystalline α -alumina, please refer to fig. 1, wherein the method for preparing XX low-sodium microcrystalline α -alumina comprises the following steps:
sa: providing an alumina feedstock, contacting the alumina feedstock with water at a ratio of 1:3, pulping according to the mass ratio to obtain first slurry;
sb: adding acetic acid for dissolving sodium oxide into the first slurry to obtain second slurry;
sc: filtering and washing the second slurry to obtain a first filter cake;
sd: calcining the first filter cake at 1200 ℃, and cooling to obtain an alumina intermediate;
se: mixing the alumina intermediate with water at a ratio of 1:3, pulping according to the mass ratio to obtain second slurry;
sf: stirring and washing the second slurry for 1h, filtering to obtain filter residues, and washing the filter residues to obtain a second filter cake;
sg: and drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina.
Example 2
Sa: providing an alumina feedstock, contacting the alumina feedstock with water at a ratio of 1:3, pulping according to the mass ratio to obtain first slurry;
sb: adding oxalic acid for dissolving sodium oxide into the first slurry to obtain second slurry;
sc: filtering and washing the second slurry to obtain a first filter cake;
sd: calcining the first filter cake at 1300 ℃, and cooling to obtain an alumina intermediate;
se: mixing the alumina intermediate with water at a ratio of 1:3, pulping according to the mass ratio to obtain second slurry;
sf: stirring and washing the second slurry for 1h, filtering to obtain filter residues, and washing the filter residues to obtain a second filter cake;
sg: and drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina.
Example 3
Sa: providing an alumina feedstock, contacting the alumina feedstock with water at a ratio of 1:3, pulping according to the mass ratio to obtain first slurry;
sb: adding hydrochloric acid for dissolving sodium oxide into the first slurry to obtain second slurry;
sc: filtering and washing the second slurry to obtain a first filter cake;
sd: calcining the first filter cake at 1400 ℃, and cooling to obtain an alumina intermediate;
se: mixing the alumina intermediate with water at a ratio of 1:3, pulping according to the mass ratio to obtain second slurry;
sf: stirring and washing the second slurry for 1h, filtering to obtain filter residues, and washing the filter residues to obtain a second filter cake;
sg: and drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina.
Example 4
Sa: providing an alumina feedstock, contacting the alumina feedstock with water at a ratio of 1:3, pulping according to the mass ratio to obtain first slurry;
sb: adding sulfuric acid for dissolving sodium oxide into the first slurry to obtain second slurry;
sc: filtering and washing the second slurry to obtain a first filter cake;
sd: calcining the first filter cake at 1600 ℃, and cooling to obtain an alumina intermediate;
se: mixing the alumina intermediate with water at a ratio of 1:3, pulping according to the mass ratio to obtain second slurry;
sf: stirring and washing the second slurry for 1h, filtering to obtain filter residues, and washing the filter residues to obtain a second filter cake;
sg: and drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina.
Related experiment and effect data:
repeating the process of example 1 four times, taking the obtained low-sodium microcrystalline alpha-alumina as a sample 11, a sample 12, a sample 13 and a sample 14, and taking the obtained alumina intermediate as a sample 15, a sample 16, a sample 17 and a sample 18;
repeating the process of example 2 four times, taking the obtained low-sodium microcrystalline alpha-alumina as a sample 21, a sample 22, a sample 23 and a sample 24, and taking the obtained alumina intermediate as a sample 25, a sample 26, a sample 27 and a sample 28;
repeating the process of example 3 four times, and taking the obtained low-sodium microcrystalline alpha-alumina as a sample 31, a sample 32, a sample 33 and a sample 44;
example 4 was repeated four times to obtain low-sodium microcrystalline α -alumina as samples 41, 42, 33, and 44.
Samples 15-18 were subjected to chemical composition detection, grain size detection, effective density detection, and burning-off detection, and the results are shown in Table 1.
All of the above tests were carried out according to GB/T6609.2-2022.
| Sample coding | Sample 15 | Sample 16 | Sample 17 | Sample 18 |
| Al 2 O 3 ％(wt％) | 99.893 | 99.893 | 99.901 | 99.879 |
| Fe 2 O 3 (wt％) | 0.011 | 0.010 | 0.010 | 0.010 |
| Na 2 O(wt％) | 0.055 | 0.045 | 0.045 | 0.050 |
| SiO 2 (wt％) | 0.011 | 0.012 | 0.014 | 0.011 |
| αAl 2 O 3 (wt％) | 94.3 | 95.4 | 94.6 | 94.9 |
| Grain size (mum) | 0.81 | 0.86 | 0.84 | 0.83 |
| Effective density (g/cm) 3 ) | 3.94 | 3.95 | 3.95 | 3.95 |
| Burning loss (wt%) | 0.03 | 0.04 | 0.03 | 0.05 |
TABLE 1
Samples 25-28 were subjected to chemical composition detection, grain size detection, effective density detection, and burn-off detection, the results of which are shown in Table 2.
TABLE 2
Samples 11-14 were subjected to chemical composition detection, grain size detection, effective density detection, and burning-off detection, and the results are shown in Table 3.
| Sample coding | Sample 11 | Sample 12 | Sample 13 | Sample 14 |
| Al 2 O 3 ％(wt％) | 99.882 | 99.903 | 99.893 | 99.922 |
| Fe 2 O 3 (wt％) | 0.012 | 0.009 | 0.011 | 0.011 |
| Na 2 O(wt％) | 0.020 | 0.024 | 0.020 | 0.021 |
| SiO 2 (wt％) | 0.016 | 0.014 | 0.016 | 0.016 |
| αAl 2 O 3 (wt％) | 92.0 | 93.8 | 95.5 | 93.6 |
| Grain size (mum) | 0.85 | 0.80 | 0.83 | 0.81 |
| Effective density (g/cm) 3 ) | 3.93 | 3.93 | 3.93 | 3.94 |
| Burning loss (wt%) | 0.07 | 0.05 | 0.06 | 0.03 |
TABLE 3 Table 3
Samples 21-24 were subjected to chemical composition detection, grain size detection, effective density detection, and burning-off detection, and the results are shown in Table 4.
| Sample coding | Sample 21 | Sample 22 | Sample 23 | Sample 24 |
| Al 2 O 3 ％(wt％) | 99.905 | 99.924 | 99.888 | 99.91 |
| Fe 2 O 3 (wt％) | 0.009 | 0.012 | 0.010 | 0.014 |
| Na 2 O(wt％) | 0.020 | 0.020 | 0.020 | 0.023 |
| SiO 2 (wt％) | 0.016 | 0.014 | 0.012 | 0.023 |
| αAl 2 O 3 (wt％) | 92.7 | 94.1 | 93.4 | 93.0 |
| Grain size (mum) | 0.85 | 0.77 | 0.80 | 0.85 |
| Effective density (g/cm) 3 ) | 3.94 | 3.94 | 3.95 | 3.95 |
| Burning loss (wt%) | 0.05 | 0.03 | 0.07 | 0.03 |
TABLE 4 Table 4
Samples 31-34 were subjected to chemical composition detection, grain size detection, effective density detection, and burning-off detection, and the results are shown in Table 5.
TABLE 5
Samples 41-44 were subjected to chemical composition detection, grain size detection, effective density detection, and burning-off detection, and the results are shown in Table 6.
| Sample coding | Sample 41 | Sample 42 | Sample 43 | Sample 44 |
| Al 2 O 3 ％(wt％) | 99.911 | 99.911 | 99.902 | 99.893 |
| Fe 2 O 3 (wt％) | 0.009 | 0.009 | 0.015 | 0.010 |
| Na 2 O(wt％) | 0.036 | 0.036 | 0.030 | 0.018 |
| SiO 2 (wt％) | 0.014 | 0.014 | 0.013 | 0.029 |
| αAl 2 O 3 (wt％) | 94.0 | 94.5 | 94.5 | 95.1 |
| Grain size (mum) | 0.82 | 0.83 | 0.84 | 0.85 |
| Effective density (g/cm) 3 ) | 3.95 | 3.95 | 3.94 | 3.96 |
| Burning loss (wt%) | 0.03 | 0.03 | 0.04 | 0.05 |
TABLE 6
Various embodiments of the present application may exist in a range format; it should be understood that the description in a range format is merely for convenience and brevity and should not be interpreted as a rigid limitation on the scope of the application. It is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In this application, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present application, the terms "include", "comprise", "comprising" and the like mean "including but not limited to". Moreover, 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. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other like elements in a process, method, article or apparatus that comprises the element. Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. For the association relation of more than three association objects described by the "and/or", it means that any one of the three association objects may exist alone or any at least two of the three association objects exist simultaneously, for example, for a, and/or B, and/or C, any one of the A, B, C items may exist alone or any two of the A, B, C items exist simultaneously or three of the three items exist simultaneously. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the low-sodium microcrystalline alpha-alumina is characterized by comprising the following steps of:
providing an alumina raw material, and mixing the alumina raw material with hydrated pulp to obtain first pulp;
adding a first acid agent for dissolving sodium oxide into the first slurry to obtain a second slurry;
filtering and washing the second slurry to obtain a first filter cake;
calcining the first filter cake at a preset temperature, and cooling to obtain an alumina intermediate;
mixing the alumina intermediate with hydrated slurry to obtain second slurry;
stirring, filtering and washing the second slurry to obtain a second filter cake;
drying the second filter cake to obtain the low-sodium microcrystalline alpha-alumina.
2. The method for producing low-sodium microcrystalline α -alumina according to claim 1, wherein the alumina raw material is mixed with a hydrated slurry, and wherein the mass of water for the slurry is 2 to 5 times that of the alumina raw material.
3. The method for producing low-sodium microcrystalline α -alumina according to claim 1, wherein the first acid agent is at least one of acetic acid, oxalic acid, and hydrochloric acid.
4. The method for producing low-sodium microcrystalline α -alumina according to claim 1, wherein the second slurry is filtered and washed, and wherein the mass of washing water is not more than 3 times the mass of solids in the second slurry.
5. The method for producing low-sodium microcrystalline α -alumina according to claim 1, wherein the predetermined temperature is 1200 to 1600 ℃.
6. The method of preparing low sodium microcrystalline α -alumina according to claim 1, wherein the alumina intermediate is combined with a hydrated slurry, and a second acid agent is added.
7. The method for producing low-sodium microcrystalline α -alumina according to claim 6, wherein the second acid agent is carbon dioxide.
8. The method for producing low-sodium microcrystalline α -alumina according to claim 1, wherein the mass of the slurry water used for the hydration of the alumina intermediate is 2 to 5 times that of the alumina intermediate.
9. The method for producing low-sodium microcrystalline α -alumina according to claim 1, wherein the stirring time is 0.2 to 2 hours.
10. The method for producing low-sodium microcrystalline α -alumina according to claim 1, wherein the second slurry is stirred, filtered, and washed, wherein the mass of the washing water is not more than 3 times the solid content in the second slurry.
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