CN114560484B - Method for producing low-sodium alumina by electrodialysis method - Google Patents
Method for producing low-sodium alumina by electrodialysis method Download PDFInfo
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- CN114560484B CN114560484B CN202210343202.0A CN202210343202A CN114560484B CN 114560484 B CN114560484 B CN 114560484B CN 202210343202 A CN202210343202 A CN 202210343202A CN 114560484 B CN114560484 B CN 114560484B
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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
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/422—Electrodialysis
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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
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
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- 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
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Abstract
The invention relates to the technical field of alumina production, in particular to a method for producing low-sodium alumina by an electrodialysis method. The method comprises the steps of roasting aluminum hydroxide obtained by an electrodialysis device to obtain low-sodium aluminum oxide, wherein the electrodialysis device comprises an anode chamber and a cathode chamber which are positioned at two sides and an anion exchange membrane which is clamped between the anode chamber and the cathode chamber; the electrodialysis comprises the following steps: sodium aluminate solution is added into a cathode chamber, alkaline buffer solution without sodium ions is added into an anode chamber, and direct current is applied between an anode and a cathode to carry out electrodialysis. Compared with the cation exchange membrane, the aluminum hydroxide crystallization environment does not contain sodium ions, so that the sodium oxide content in the roasted aluminum oxide is below 0.05%, the catalytic activity of the aluminum oxide is improved, the cost is saved, the preparation process is energy-saving and environment-friendly, and the environment is protected.
Description
Technical Field
The invention relates to the technical field of alumina production, in particular to a method for producing low-sodium alumina by an electrodialysis method.
Background
The industrial production technology of alumina mainly includes an aluminum alkoxide hydrolysis method, a crystallization pyrolysis method and a Bayer process. Wherein, the vast majority of the world's Al 2 O 3 And the metal aluminum is prepared from purified bauxite by Bayer process. Al is prepared by the traditional Bayer process 2 O 3 The technological principle is that bauxite is firstly ground, then dissolved by alkali solution NaOH, the impurities are separated and washed, and the filtrate sodium aluminate solution is used as mother liquor, and Al (OH) is produced by seed precipitation or carbon precipitation 3 And (3) separating and washing the crystal, and drying and roasting the product to obtain the alumina. In the above process, al (OH) 3 The crystals are directly precipitated in the sodium aluminate solution, and a large amount of sodium ions are contained in the solution and can be attached to Al (OH) 3 An intergranular base is generated in the crystal lattice. Sodium ions are well-known poisons for the acidity of alumina surfaces, which exchange for hydroxyl groups on the alumina surface, weakening or poisoning the strongest lewis acid sites.
In view of the above problems, if there is a suitable method, in Al (OH) 3 In the course of the crystallization process, the crystal is formed,separating aluminate and sodium ions is expected to reduce sodium ion content in alumina produced by Bayer process, increase surface strong acidity and improve reactivity of alumina. The membrane separation method has the characteristics of high efficiency, low energy consumption, environment friendliness and the like, so the method is worthy of reference and use. Currently, membrane separation, including electrodialysis, diffusion dialysis, etc., is mainly performed on multivalent metal hydroxides as solids from alkali metal hydroxides or another multivalent metal hydroxide. For example, alkali metal hydroxide etchants that etch aluminum and aluminum alloys, require purification and recovery, and U.S. patent No. 5141610 reports treatment by electrodialysis, in which OH in the waste stream is present during operation - Generating oxygen by ion electrolysis or H by reaction with electrodes + Neutralizing ions to generate water; sodium ions migrate through the cation exchange membrane to the cathode compartment and react with OH generated by electrolysis of water in the cathode compartment - The ions are combined to generate NaOH to be recovered; hydrolyzing the aluminate plasma in a reaction chamber to generate solid precipitate such as aluminum hydroxide; and intermittently extracting the solution in the reaction chamber, separating the precipitate such as aluminum hydroxide by cooling, crystallizing, filtering and the like, and returning the solution to continue the electrodialysis experiment. The method has high recovery rate of alkali and aluminum, but the obtained aluminum hydroxide sodium content is still high, sodium ions are removed through a cation membrane, but residues are inevitably remained in an anode chamber, so that the sodium ions are attached in aluminum hydroxide crystals.
Aiming at separating aluminate and sodium ions in Bayer mother liquor in the alumina production process, china patent CN104016388A discloses a separation method of alkaline feed liquor in the alumina production, wherein sodium hydroxide and sodium metaaluminate in the alkaline feed liquor are separated through electrodialysis, and the sodium hydroxide and the sodium metaaluminate in the alkaline feed liquor are subjected to membrane separation before seed crystal is introduced, so that the energy consumption in the subsequent seed crystal precipitation process can be reduced, the time is shortened, and the yield of aluminum hydroxide is improved; in addition, the purity of the alkali in the mother liquor can be improved, and the recycling of the alkali is facilitated. Chinese CN113044863a discloses a method for increasing the decomposition rate of seed crystals in alumina production, which uses electrodialysis technology to decompose sodium aluminate solution in cooperation with seed crystals in the seed crystal decomposition procedure, and the chest effect of electrodialysis and seed crystal decomposition decomposes sodium aluminate solution into high caustic ratio solution and aluminum hydroxide crystals and breaks away from the non-decomposed sodium aluminate solution, so that the non-decomposed sodium aluminate solution can be maintained at a lower caustic ratio level, thereby ensuring rapid progress of seed crystal decomposition, improving the decomposition efficiency and the decomposition rate. However, the ion exchange membranes in the electrolytic cells involved in the above process are all cation exchange membranes, and sodium ions are basically migrated from the sodium aluminate solution to the cathode chamber under the action of electric field force, so that the content of the obtained sodium ions in the alumina is still high.
Disclosure of Invention
The invention aims to solve the technical problems: provides a method for producing low-sodium alumina by an electrodialysis method, and aims to solve the problems of over-high sodium content in alumina produced by a Bayer process and the like.
In view of the shortcomings of the prior art, one of the purposes of the invention is to provide a method for producing low-sodium alumina by an electrodialysis method, so that the content of sodium oxide in the low-sodium alumina is less than or equal to 0.05%.
The technical scheme of the invention is as follows:
the present invention provides a method for producing low sodium alumina by an electrodialysis method, which comprises calcining aluminum hydroxide obtained by an electrodialysis device comprising an anode compartment and a cathode compartment and an anion exchange membrane sandwiched between the anode compartment and the cathode compartment;
the electrodialysis comprises the following steps: sodium aluminate solution is added into a cathode chamber, alkaline buffer solution without sodium ions is added into an anode chamber, and direct current is applied between an anode and a cathode to carry out electrodialysis.
Preferably, the alkaline buffer solution free of sodium ions comprises a mixture of aqueous ammonia and nitric acid or ammonium nitrate, preferably a mixture of aqueous ammonia and nitric acid.
Preferably, the volume ratio of the ammonia water to the nitric acid is 0.03 to 3, preferably 0.03 to 1, more preferably 0.1 to 0.25.
Preferably, the concentration of the sodium aluminate solution is 0.5-1.5mol/L.
Preferably, the voltage of the direct current is 8-20V, preferably 14-20V.
Preferably, the electrodialysis time is 4-12 hours.
The invention also provides the low-sodium aluminum oxide prepared by the method, wherein the weight percentage content of sodium oxide in the low-sodium aluminum oxide is less than or equal to 0.05 percent.
The invention has the beneficial effects that:
1. compared with the traditional process for producing alumina by using a thermochemical method, the method provided by the invention adopts an electrodialysis method to produce low-sodium alumina, and the preparation process is energy-saving and environment-friendly and is environment-friendly and recyclable;
2. compared with the method adopting a cation exchange membrane, the method does not contain sodium ions in the crystallization environment of the aluminum hydroxide, so that the sodium oxide content in the roasted aluminum oxide is below 0.05%, the catalytic activity of the aluminum oxide is improved, and the cost is saved.
Drawings
FIG. 1 is a schematic diagram of an electrodialysis apparatus of example 1.
Detailed Description
In order to make the purposes, technical schemes and technical effects of the embodiments of the present invention more clear, the technical schemes in the embodiments of the present invention are clearly and completely described. The embodiments described below are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art without the benefit of the teachings of this invention, are intended to be within the scope of the invention.
At present, the hydrothermal treatment method is used for removing sodium from aluminum oxide, and the intermediate semi-finished product has the problems of high water content, further drying in later period, large equipment investment, long flow, high energy consumption and the like. In order to solve the technical problems, the invention provides a method for producing low-sodium alumina by an electrodialysis method, which is characterized in that aluminate and sodium ions are separated by electrodialysis, then the aluminate undergoes a precipitation reaction in a buffer solution without sodium ions to generate aluminum hydroxide, then the aluminum hydroxide is roasted to prepare the low-sodium alumina, and the filtered sodium aluminate solution can be recycled.
In one embodiment of the present invention, a method for producing low sodium alumina by an electrodialysis method comprises calcining aluminum hydroxide obtained by an electrodialysis device comprising anode and cathode compartments on both sides and an anion exchange membrane sandwiched between the anode and cathode compartments;
the electrodialysis comprises the following steps: sodium aluminate solution is added into a cathode chamber, alkaline buffer solution without sodium ions is added into an anode chamber, and direct current is applied between an anode and a cathode to carry out electrodialysis.
In the electrodialysis process, under the action of direct current, aluminate ions and hydroxide ions in the cathode chamber migrate through the anion exchange membrane and enter the anode chamber, so that sodium ions and aluminate ions in the cathode chamber are separated. Sodium ions in the cathode chamber cannot pass through the anion exchange membrane to enter the anode chamber due to positive charge. The total result is that aluminate is enriched in the anode chamber, aluminum hydroxide precipitate is generated under the environment with proper pH, and sodium ions in the cathode chamber and hydroxide generated by electrolysis are combined to produce sodium hydroxide, so that no sodium ions are generated in the crystallization environment of aluminum hydroxide, and the purity of aluminum oxide is improved.
The invention also provides the low-sodium alumina produced by the method, wherein the weight percentage content of sodium oxide in the low-sodium alumina is less than or equal to 0.05 percent.
The method for producing low sodium alumina by the electrodialysis of the present invention will be specifically described by way of specific examples.
The raw materials and equipment sources used in the inventive examples and comparative examples are shown in Table 1.
Table 1 inventive and comparative examples use raw materials and equipment sources
| Using raw materials or apparatus | Content of | Model number | Sources or manufacturers |
| Sodium aluminate | 500g | CP | Shanghai test |
| Nitric acid | 500mL | AR | Western style flower |
| Ammonia water | 500mL | AR | Shanghai test |
| XRF | / | S8TIGER | BRUKER |
| XRD | / | X'Pert3 | PAN |
Example 1
The electrodialysis device shown in fig. 1, which is used in this embodiment, is composed of an anode chamber and a cathode chamber which are respectively located at two sides, and an anion exchange membrane which is sandwiched between the anode chamber and the cathode chamber; shan Zhangyin ion exchange membrane has an effective area of 2.0cm 2 The spacing between the anode or cathode and the anion exchange membrane was 4cm, respectively. The anion exchange membrane is made of Sanceno Co., ltdThe provided anion exchange membrane with the model of fumasep-3-20 adopts pure titanium electrodes as an anode and a cathode.
The anode chamber and the cathode chamber are connected in series, the anode chamber is filled with an alkaline buffer solution without sodium ions, the alkaline buffer solution without sodium ions is ammonia water and dilute nitric acid aqueous solution, the volume ratio of the ammonia water to the dilute nitric acid is 0.03, the concentration of the ammonia water is 13.38mol/L, and the concentration of the dilute nitric acid is 14.4mol/L; the cathode chamber was charged with sodium aluminate solution at a concentration of 0.746mol/L, and the volumes of the sodium ion-free alkaline buffer solution and the sodium aluminate solution were 50mL. And controlling the voltage at 14V, continuously generating white aluminum hydroxide precipitate in an anode chamber in the experimental process, filtering an alkaline buffer solution after running for 4 hours to obtain 0.06g of aluminum hydroxide precipitate, obtaining 1.54% of aluminum hydroxide, and roasting the aluminum hydroxide to obtain the low-sodium aluminum oxide.
The XRD method is adopted to measure the aluminum hydroxide as Bayerite crystal form.
The sodium oxide content per 500mg of low sodium alumina was analyzed by XRF using the melt-sampling method and the results are shown in Table 2.
Example 2
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, the difference from example 1 being that the volume ratio of ammonia to dilute nitric acid was 0.11, and the alkaline buffer solution was filtered to give 0.11g of aluminum hydroxide precipitate, the yield of aluminum hydroxide being 2.82%.
The aluminum hydroxide was measured as the Boehmite crystal form by XRD.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Example 3
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, the difference from example 1 being that the volume ratio of ammonia to dilute nitric acid was 0.2, and the alkaline buffer solution was filtered to give 0.14g of aluminum hydroxide precipitate, with an aluminum hydroxide yield of 3.59%.
The aluminum hydroxide was measured as the Boehmite crystal form by XRD.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Example 4
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, the difference from example 1 being that the volume ratio of ammonia to dilute nitric acid was 0.25, and the alkaline buffer solution was filtered to give 0.13g of aluminum hydroxide precipitate, the yield of aluminum hydroxide being 3.33%.
The aluminum hydroxide was amorphous as measured by XRD.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Example 5
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, the difference from example 1 being that the volume ratio of ammonia to dilute nitric acid was 0.76, and the alkaline buffer solution was filtered to give 0.03g of aluminum hydroxide precipitate, with an aluminum hydroxide yield of 0.77%.
The aluminum hydroxide was amorphous as measured by XRD.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Example 6
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, with the difference that the control voltage was 20V, and the alkaline buffer solution was filtered to give 0.13g of aluminum hydroxide precipitate, with an aluminum hydroxide yield of 3.33%.
The aluminum hydroxide was measured as the Boehmite crystal form by XRD.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Example 7
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, with the difference from example 3 in that the control voltage was 8V, and the alkaline buffer solution was filtered to give 0.03g of aluminum hydroxide precipitate, with an aluminum hydroxide yield of 0.77%.
The aluminum hydroxide was measured as the Boehmite crystal form by XRD.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Example 8
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, differing from example 3 in that the control voltage was 14V, the run time was 8 hours, and the alkaline buffer solution was filtered to give 0.14g of aluminum hydroxide precipitate, with a yield of 3.59%.
The aluminum hydroxide was measured as the Boehmite crystal form by XRD.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Example 9
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, differing from example 3 in that the control voltage was 14V, the run time was 12 hours, and the alkaline buffer solution was filtered to give 0.16g of aluminum hydroxide precipitate, with a yield of 4.10% aluminum hydroxide.
The XRD method is adopted to measure the aluminum hydroxide as Bayerite crystal form.
The sodium oxide content of the low sodium alumina was measured by XRF and the results are shown in table 2.
Comparative example 1
50mL of 0.746mol/L sodium aluminate solution is measured and added into 50mL of alkaline buffer solution without sodium ions, the alkaline buffer solution without sodium ions is ammonia water and dilute nitric acid aqueous solution, the volume ratio of the ammonia water to the dilute nitric acid is 0.2, the concentration of the ammonia water is 13.38mol/L, and the concentration of the dilute nitric acid is 14.4mol/L. The alkaline buffer solution was filtered to obtain 0.95g of aluminum hydroxide precipitate, the yield of aluminum hydroxide was 24.36%, and then the aluminum hydroxide was calcined to obtain low sodium alumina.
The XRD method is adopted to measure the aluminum hydroxide as Bayerite crystal form.
The sodium oxide content of the alumina was measured by XRF and the results are shown in table 2.
Comparative example 2
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, with the difference from example 1 that the volume ratio of ammonia to dilute nitric acid was 3.29, and no precipitation of aluminum hydroxide was obtained.
Comparative example 3
The electrodialysis apparatus of example 1 was used to produce low sodium alumina, with the difference from example 1 that 50mL of dilute nitric acid was introduced into the anode compartment, and no precipitation of aluminum hydroxide was obtained.
TABLE 2 sodium oxide content in alumina
As can be seen from Table 2, the sodium oxide content of the low-sodium alumina prepared in examples 1 to 9 of the present invention is 0.015 to 0.023%, which is less than 0.05%; comparative example 1 the sodium oxide content of the low sodium alumina obtained without electrodialysis was 0.089% or more than 0.05%. From the viewpoint of the yield of aluminum hydroxide obtained in examples 1 to 5, the yield of aluminum hydroxide is higher when the volume ratio of ammonia water to nitric acid is 0.03 to 0.25, and the yield of aluminum hydroxide is higher when the volume ratio of ammonia water to nitric acid is 0.1 to 0.25; the results of comparative examples 2 and 3 show that when the volume ratio of ammonia water to nitric acid is 0 or 3.29, no aluminum hydroxide precipitate can be formed, and thus low sodium alumina cannot be produced; from the results of the aluminum hydroxide production in examples 3 and 6 to 7, the aluminum hydroxide production was higher at a voltage of 14 to 20V in electrodialysis.
In summary, the invention adopts the anion exchange membrane single-compartment electrodialysis method to prepare the low-sodium alumina, and compared with the cation exchange membrane, the invention does not contain sodium ions in the crystallization environment of the aluminum hydroxide, so that the sodium oxide content in the roasted alumina is below 0.05 percent, the catalytic activity of the alumina is improved, the cost is saved, the preparation process is energy-saving and environment-friendly, and the environment is protected.
The above description is not intended to limit the invention in any way, but is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (6)
1. A method for producing low-sodium alumina by an electrodialysis method, characterized in that it comprises calcining aluminum hydroxide obtained by an electrodialysis device comprising an anode compartment and a cathode compartment and an anion exchange membrane sandwiched between the anode compartment and the cathode compartment;
the electrodialysis comprises the following steps: adding sodium aluminate solution into a cathode chamber, adding alkaline buffer solution without sodium ions into an anode chamber, and applying direct current between an anode and a cathode to carry out electrodialysis;
wherein the alkaline buffer solution without sodium ions is a mixture containing ammonia water and nitric acid; the volume ratio of the ammonia water to the nitric acid is 0.1-0.25; the voltage of the direct current is 14-20V.
2. The method according to claim 1, wherein the concentration of the aqueous ammonia is 10 to 15mol/L and the concentration of the nitric acid is 10 to 20mol/L.
3. The method according to claim 1, characterized in that the concentration of the sodium aluminate solution is 0.5-1.5mol/L.
4. The method according to claim 2, characterized in that the concentration of the sodium aluminate solution is 0.5-1.5mol/L.
5. The method according to any one of claims 1-4, wherein the electrodialysis time is 4-12 hours.
6. A low sodium alumina prepared by the method of any one of claims 1-5, wherein the low sodium alumina has a sodium oxide content of less than or equal to 0.05 wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2815628C1 (en) * | 2023-11-30 | 2024-03-19 | Федеральное государственное автономное образовательное учреждение высшего образования Сибирский федеральный университет | Method of processing weakly alkaline aluminate solutions of alumina production |
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| CN104016388A (en) * | 2014-06-12 | 2014-09-03 | 合肥工业大学 | Separation method of alkaline liquid in production of alumina |
| CN104211098A (en) * | 2014-09-22 | 2014-12-17 | 合肥工业大学 | Device and method for electrodialysis and electrolysis electrodialysis integrated processing of alkaline feed liquid in aluminium oxide production |
| CN109650683A (en) * | 2017-10-10 | 2019-04-19 | 广东科达洁能股份有限公司 | A kind of method and system recycling calcium and aluminium from Aluminum sludge |
| CN113993817A (en) * | 2019-04-18 | 2022-01-28 | 内斯特化学有限责任公司 | High purity alumina by electrodialysis |
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| CN104211098A (en) * | 2014-09-22 | 2014-12-17 | 合肥工业大学 | Device and method for electrodialysis and electrolysis electrodialysis integrated processing of alkaline feed liquid in aluminium oxide production |
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