CN113912095B - Precipitation desulfurization method for high-sulfur bauxite leaching solution - Google Patents
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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
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
- C01F7/47—Purification of aluminium oxide, aluminium hydroxide or aluminates of aluminates, e.g. removal of compounds of Si, Fe, Ga or of organic compounds from Bayer process liquors
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Abstract
The invention discloses a method for removing sulfur from a high-sulfur bauxite Bayer process leaching solution by precipitation, and belongs to the technical field of aluminum smelting. Placing high-sulfur bauxite leaching liquid in a U-shaped container, and taking out feed liquid connected to one end of a positive electrode after direct current is conducted for 5-6 hours; dissolving a precipitant in water according to the proportion of 5-50g/L, dripping the precipitant solution into the feed liquid, and stirring to fully precipitate; heating and boiling the obtained mixed solution for 0.5-1 hour, and continuously stirring; and cooling and filtering the heated solution, washing the precipitate with water to obtain sulfur-containing filter residues, and allowing the filtrate to enter a subsequent aluminum smelting process. The method disclosed by the invention is simple to operate, high in separation efficiency, and capable of reducing the subsequent treatment burden of the leached tail liquid and reducing the production cost.
Description
Technical Field
The invention relates to a precipitation desulfurization method for a high-sulfur bauxite leaching solution, and belongs to the technical field of aluminum smelting.
Background
With the increasing demand of China on metallic aluminum in recent years, the increasing of the output of aluminum oxide as a production raw material of aluminum becomes extremely critical, bauxite is a main mineral source of aluminum oxide, but the problem of larger sulfur content exists in bauxite, and when the bauxite is used for producing aluminum oxide, a large amount of S exists in sodium aluminate solution after the high-sulfur bauxite is leached by Bayer process 2- 、SO 3 2- 、S 2 O 3 2- The content of sulfur ions in the leaching solution is about 3g/L, so that the viscosity of the leaching solution is increased, and the production process of the alumina is affected, so that the yield of the alumina is reduced. In the immersion liquid environment, the main components of the immersion liquid are decomposed by sulfur ions and alkali to generate sodium sulfate, the metal is oxidized by thiosulfate to generate ferric hydroxide colloid, the solution viscosity is increased to reduce the separation and sedimentation speed of red mud, and the sulfite is converted into sulfate in the solution environment to increase the acidity of the immersion liquid to cause corrosion of production equipment.
In order to effectively remove sulfur in high-sulfur bauxite, improve the production efficiency of aluminum and save the production cost, patent (CN 105460962A) carries out desulfurization by adding barium hydroxide solution in the production process, but the added barium hydroxide is higher in quantity, the reagent consumption is higher, and the production cost is higher. In addition, the patent (CN 102897812A) adopts a method of activating and treating high-sulfur bauxite by a low-temperature roasting desulfurization method, and the mineral powder is introduced with hot air at 650-900 ℃ at 500-600 ℃ for desulfurization, so that the sulfur simple substance in the high-sulfur bauxite is changed into sulfur dioxide to realize sulfur removal, and the technology also treats tail gas sulfur dioxide, but has higher requirements on production environment, expensive production equipment and complex operation. There is also a patent (see patent CN102534189 a for details) that desulfurization is performed by microwave heating and roasting, but the environmental pollution caused by sulfur dioxide generated after roasting is a problem, and the subsequent process is complicated. Other bauxite immersion liquid desulfurization methods have the problems of large reagent amount, complicated steps, large environmental pollution and the like.
Disclosure of Invention
The invention aims to provide a precipitation desulfurization method for a high-sulfur bauxite leaching solution, which aims to solve the problem of high sulfur content in the bauxite leaching solution.
In order to achieve the above purpose, the invention adopts the following technical scheme:
(1) And placing the high-sulfur bauxite leaching liquid in a U-shaped container, respectively connecting graphite electrodes of direct current to two ends of the U-shaped container, and taking out the feed liquid connected to one end of the positive electrode after the two ends of the U-shaped container are electrified for 5-6 hours.
(2) Dissolving the precipitant in water according to the proportion of 5-50g/L, dripping the precipitant solution into the feed liquid, and stirring to fully precipitate.
(3) And (3) heating and boiling the mixed solution obtained in the step (2) for 0.5-1 hour, and stirring the mixed solution during heating, wherein the temperature is the actual environment temperature of the high-sulfur bauxite leaching solution.
(4) And cooling and filtering the heated solution, washing the precipitate with water to obtain sulfur-containing filter residues, retaining the first filtrate, and measuring sulfur ions in the solution.
Preferably, the direct current in step (1) of the present invention is 10-25V.
After the high-sulfur bauxite leaching liquid is connected with the electrode, the electrode is electrified for a period of time, the solution can be in different colors, the color close to the positive electrode is red and black, the color close to the negative electrode is light red, the red and black color of the positive electrode is taken as feed liquid, and the preferred feed liquid is 30-35% of the total volume of the high-sulfur bauxite leaching liquid.
Preferably, the precipitant used in the step (2) of the invention is one or more of calcium sulfate, calcium oxide, calcium fluoride, tricalcium phosphate, calcium acetate, calcium chloride, calcium hydroxide, magnesium carbonate, magnesium oxide, zinc sulfate and aluminum chloride which are mixed according to any proportion.
Preferably, the volume ratio of the precipitant solution to the feed solution in step (2) of the present invention is 1:1.
Preferably, the number of times of washing the precipitate in step (3) of the present invention is not less than 2.
The principle of the invention is as follows: the high-sulfur bauxite leaching liquid is a sulfur-containing compound colloid, after direct current is introduced, sulfur-containing charged ions in a sodium aluminate solution are enriched by utilizing the electrophoresis property of the colloid, reagents are added according to the solubility product difference between insoluble matters of sulfur to precipitate sulfur ions, and the solubility of insoluble sulfides is reduced by utilizing the influence of the homoionic effect on the solubility of the insoluble matters of sulfur to achieve the purpose of desulfurization.
The beneficial effects of the invention are as follows:
(1) According to the invention, through the addition of the precipitant, sulfur ions in the high-sulfur bauxite leaching tail liquid can be effectively precipitated, and the sulfur ion content in the sodium metaaluminate solution is reduced.
(2) The invention relates to a feed liquid pretreatment process flow, but the operation is simple and easy, and the cost is greatly saved; the used precipitant has the advantages of small dosage, low price, strong stability and low toxicity, is favorable for large-scale application, has a reaction temperature environment similar to the actual ore pulp leaching temperature, and is favorable for large-scale application.
The leachate of the invention enriches sulfur-containing ions through direct current, and the sulfur-containing precipitation is generated after the precipitator is added, so that the desulfurization effect can be efficiently and rapidly realized by the mutual cooperation of the sulfur-containing precipitation and the leaching solution.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the scope of the invention is not limited to the description.
Example 1
The embodiment adopts different precipitants and different concentrations for removing sulfur ions in the sodium aluminate solution after leaching the high-sulfur bauxite, and comprises the following steps:
(1) The leaching tail liquid of the high sulfur bauxite is treated by 25V direct current for 6 hours, and then the partial solution of the positive electrode is taken as feed liquid,
(2) Weighing different precipitants to prepare precipitant solution, dripping the precipitant solution into 1L of feed liquid, and stirring to form precipitate.
(3) Heating and boiling the precipitate for 0.5-1 hr, and stirring at proper time during heating.
(4) And cooling and filtering the heated solution, washing the precipitate twice to obtain sulfur-containing filter residues, and retaining the original filtrate to measure sulfur ions in the filtrate.
Measuring the original filtrate in the step (4) by using an iodine-sodium thiosulfate titration method, and calculating sulfur-containing ions (S) in the high-sulfur bauxite leaching tail liquid by using the difference of the reaction conditions of three ions and iodine 2- 、SO 3- 、S 2 O 3 2- ) Concentration; and (3) comparing the concentration of the sulfur-containing ions in the feed liquid (the calculation method is the same as that of the original filtrate), and calculating to obtain the removal rate of the sulfur-containing ions.
In this example, different precipitants are used to remove sulfur ions from the sodium aluminate solution after leaching the high sulfur bauxite, and the removal rates of the different precipitants to the sulfur ions are shown in table 1.
TABLE 1
As can be seen from Table 1, the selection of the precipitants has a great influence on the removal rate of sulfur ions, the concentration of the precipitants has a certain influence on the removal rate of sulfur ions, the concentration of some precipitants is high but the removal rate of sulfur ions is low, the concentration of some precipitants is low but the removal rate of sulfur ions is high, the determination is made according to the solubility product difference between sulfide precipitation and the added precipitants, after the solution of the precipitants is added into the feed liquid, a part of precipitants react with the sulfur ions in the feed liquid to directly form precipitation, and a part of precipitants use the same ion effect to reduce the solubility of the sulfur-containing precipitation and increase the precipitation amount.
Example 2
The embodiment adopts different concentrations of the same precipitant for removing sulfur ions in the sodium aluminate solution after leaching the high sulfur bauxite, and comprises the following steps:
(1) The leaching tail liquid of the high sulfur bauxite is treated by 25V direct current for 6 hours, and then the partial solution of the positive electrode is taken as feed liquid,
(2) The precipitant is weighed to prepare precipitant solutions with different concentrations, and the precipitant solutions are dripped into 1L of feed liquid and stirred to form precipitate.
(3) Heating and boiling the precipitate for 0.5-1 hr, and stirring at proper time during heating.
(4) And cooling and filtering the heated solution, washing the precipitate twice to obtain sulfur-containing filter residues, and retaining the original filtrate to measure sulfur ions in the filtrate.
Measuring the original filtrate in the step (4) by using an iodine-sodium thiosulfate titration method, and calculating sulfur-containing ions (S) in the high-sulfur bauxite leaching tail liquid by using the difference of the reaction conditions of three ions and iodine 2- 、SO 3- 、S 2 O 3 2- ) Concentration; and (3) comparing the concentration of the sulfur-containing ions in the feed liquid (the calculation method is the same as that of the original filtrate), and calculating to obtain the removal rate of the sulfur-containing ions.
This example uses different concentrations of the same precipitant for removal of sulfur ions from sodium aluminate solution after leaching of high sulfur bauxite, and the removal rates of sulfur ions from different concentrations of the same precipitant are shown in table 2.
TABLE 2
As can be seen from Table 2, the concentration of the precipitant has a great influence on the removal rate of sulfur ions, because the precipitant provides ions required for sulfur ion precipitation, the higher the concentration of sulfur ions in the feed liquid is, the higher the concentration of the precipitant ions to be provided is, and the precipitant ions react with each other to form precipitation, so that precipitation is not generated when the precipitation dissolution balance is reached, and the removal rate of sulfur ions reaches the highest.
Example 3
In the embodiment, whether the high-sulfur bauxite leaching solution is electrified or whether a precipitator is added for removing sulfur ions in the sodium aluminate solution after the high-sulfur bauxite leaching is adopted, and the method comprises the following steps of:
(1) Taking a part of the leaching tail liquid of the high-sulfur bauxite as a feed liquid after passing 25V direct current for 6 hours, and taking a part of the leaching tail liquid of the high-sulfur bauxite as a feed liquid after being not electrified
(2) Weighing a certain amount of precipitant to prepare a solution, dripping the solution into 1L of feed liquid or raw material liquid, stirring to form precipitate,
(3) Heating and boiling the precipitation liquid for 1 hour, and stirring timely during heating;
(4) And cooling and filtering the heated solution, washing the precipitate twice to obtain sulfur-containing filter residues, and retaining the original filtrate to measure sulfur ions in the filtrate.
Measuring the primary filtrate in the step (4) by using an iodine-sodium thiosulfate titration method, and calculating the concentration of sulfur-containing ions (S2-, SO3-, S2O 32-) in the high-sulfur bauxite leaching tail liquid by using the difference of the reaction conditions of three ions and iodine; and (3) comparing the concentration of the sulfur-containing ions in the feed liquid (the calculation method is the same as that of the original filtrate), and calculating to obtain the removal rate of the sulfur-containing ions.
In the embodiment, whether the high-sulfur bauxite leaching solution is electrified or not and whether a precipitator is added for removing sulfur ions in the sodium aluminate solution after the high-sulfur bauxite leaching is adopted, and the removal rate of the sulfur ions by the method is shown in a table 3.
TABLE 3 Table 3
As can be seen from table 3, the high-sulfur bauxite leaching solution is electrified only without adding a precipitant, so that the high-sulfur bauxite leaching solution has no better effect on removing sulfur ions; compared with the process of electrifying only, the process has the advantages that the removal rate of the sulfur ions is improved slightly by only adding the precipitant into the leaching solution, but the removal rate of the sulfur ions by electrifying the leaching solution and adding the precipitant is improved obviously, because the sulfur ions are enriched by electrifying the leaching solution, sulfide precipitation is formed by adding the precipitant after the concentration of the sulfur ions is increased, and the removal rate of the sulfur ions is improved obviously by the cooperation of the two components.
Example 4
The embodiment adopts a plurality of precipitants for sharing, is used for removing sulfur ions in sodium aluminate solution after leaching high sulfur bauxite, and comprises the following steps:
(1) The leaching tail liquid of the high sulfur bauxite is treated by 25V direct current for 6 hours, and then the partial solution of the positive electrode is taken as feed liquid,
(2) The precipitant is prepared into 5g/L solution, which is added into the feed liquid by drops, and the solution is stirred to form precipitate,
(3) Heating the precipitate for 1 hour, and stirring timely during heating;
(4) And cooling and filtering the heated solution, washing the precipitate twice to obtain sulfur-containing filter residues, and retaining the original filtrate to measure sulfur ions in the filtrate.
And (3) measuring the primary filtrate in the step (4) by using an iodine-sodium thiosulfate titration method, and calculating the concentration of sulfur-containing ions (S2-, SO3-, S2O 32-) in the high-sulfur bauxite leaching tail liquid by using the difference of the reaction conditions of the three ions and the iodine. And (3) comparing the concentration of the sulfur-containing ions in the feed liquid (the calculation method is the same as that of the original filtrate), and calculating to obtain the removal rate of the sulfur-containing ions.
In this example, various precipitants were used to remove sulfur ions from the sodium aluminate solution after leaching the high sulfur bauxite, and the removal rate of sulfur ions is shown in table 4.
TABLE 4 Table 4
As can be seen from Table 4, the leachate can be mixed with a plurality of precipitants to achieve a higher removal rate of sulfur ions, and the method utilizes the combined action of the precipitants, has less consumption of the precipitants and better removal effect of sulfur ions, and is an efficient and economical desulfurization method.
While the specific embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes may be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (4)
1. The precipitation desulfurization method of the high-sulfur bauxite leaching solution is characterized by comprising the following steps of:
(1) Placing the high-sulfur bauxite leaching solution in a U-shaped container, respectively inserting graphite electrodes at two ends of the U-shaped container, and introducing 10-25V direct current for 5-6 hours to take out anode end feed liquid;
(2) Dissolving a precipitant in water according to the proportion of 5-50g/L, dripping the precipitant solution into the feed liquid, and stirring to fully precipitate;
(3) Heating and boiling the mixed solution obtained in the step (2) for 0.5-1 hour, and stirring during heating;
(4) Cooling and filtering the heated solution, washing the precipitate with water to obtain sulfur-containing filter residues, and retaining the first filtrate;
the precipitants used in the step (2) are obtained by mixing a plurality of calcium sulfate, calcium oxide, calcium fluoride, tricalcium phosphate, calcium acetate, calcium chloride, calcium hydroxide, magnesium carbonate, magnesium oxide, zinc sulfate and aluminum chloride according to any proportion.
2. The method for precipitation desulfurization of high-sulfur bauxite leaching solution according to claim 1, wherein: the positive electrode end feed liquid taken out in the step (1) accounts for 30-35% of the total volume of the high-sulfur bauxite leaching liquid.
3. The method for precipitation desulfurization of high-sulfur bauxite leaching solution according to claim 1, wherein: in the step (2), the volume ratio of the precipitant solution to the feed liquid is 1:1.
4. The method for precipitation desulfurization of high-sulfur bauxite leaching solution according to claim 1, wherein: and (3) washing the precipitate with water for not less than 2 times.
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