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CN118127342B - A method for wet desulfurization of sulfur-containing bauxite - Google Patents

A method for wet desulfurization of sulfur-containing bauxite Download PDF

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CN118127342B
CN118127342B CN202410559497.4A CN202410559497A CN118127342B CN 118127342 B CN118127342 B CN 118127342B CN 202410559497 A CN202410559497 A CN 202410559497A CN 118127342 B CN118127342 B CN 118127342B
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bauxite
autoclave
sulfur
sulfuric acid
acid solution
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CN118127342A (en
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谢锋
王明理
白云龙
王伟
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Northeastern University China
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Northeastern University China
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Abstract

本发明提供了一种含硫铝土矿湿法脱硫的方法,其步骤包括:将铝土矿与PH在1~5的硫酸溶液加入高压釜内胆中;将高压釜密封后排出釜胆内的空气;设定目标加热温度,加热与搅拌得到铝土矿与硫酸溶液的混合物料;达到目标加热温度时,向高压釜内胆内持续通入氧气保温进行氧化浸出反应;混合物料氧化浸出反应完成后降温取出釜胆内的浆液;对浆液过滤、洗涤、烘干得到脱硫的铝土矿。本发明提供的一种含硫铝土矿湿法脱硫的方法,流程短、成本低、绿色环保且脱硫效率高,完全能够降低含硫铝土矿中的硫含量,从而提高铝土矿的综合利用率。

The present invention provides a method for wet desulfurization of sulfur-containing bauxite, the steps of which include: adding bauxite and a sulfuric acid solution with a pH of 1 to 5 into an autoclave; sealing the autoclave and discharging the air in the autoclave; setting a target heating temperature, heating and stirring to obtain a mixture of bauxite and sulfuric acid solution; when the target heating temperature is reached, continuously introducing oxygen into the autoclave to keep the temperature for oxidation leaching reaction; after the oxidation leaching reaction of the mixture is completed, cooling and taking out the slurry in the autoclave; filtering, washing and drying the slurry to obtain desulfurized bauxite. The present invention provides a method for wet desulfurization of sulfur-containing bauxite, which has a short process, low cost, is green and environmentally friendly, and has high desulfurization efficiency, and can completely reduce the sulfur content in sulfur-containing bauxite, thereby improving the comprehensive utilization rate of bauxite.

Description

Wet desulfurization method for sulfur-containing bauxite
Technical Field
The invention relates to the technical field of bauxite processing, in particular to a wet desulfurization method for sulfur-containing bauxite.
Background
With the reduction of ore resources, research on high-sulfur and difficult-to-treat sedimentary ores is urgent. Production practice finds that the dissolution rate of the aluminum minerals of the deposit ore is poor, and the sulfur of the deposit ore has great harm to production. The existing desulfurization methods include a roasting desulfurization method, a desulfurizing agent addition desulfurization method, a microbial desulfurization method, a floatation desulfurization method and the like.
The roasting desulfurization method has the advantages that the roasting temperature is high, and in addition, the condition that SO 2 is concentrated on the surface of mineral powder easily occurs in the roasting process, SO that the 'under-burning' or 'over-burning' problem is caused. The microbial desulfurization method has high requirements on the growth environment of microorganisms, including temperature, ph value and the like, which require accurate control of the microorganisms in the operation process, and has complex operation and high cost. The desulfurizing agent adding desulfurizing method and the floating desulfurizing method respectively need to use a large amount of desulfurizing agents and floating agents in the desulfurizing process, so that the production cost is greatly increased, the operation condition requirement is high, and the environment pollution is relatively large.
Therefore, a new process for desulfurizing bauxite, which is short in flow, low in cost and environment-friendly, is needed at present so as to reduce the sulfur content in sulfur-containing bauxite ore and further improve the comprehensive utilization rate of bauxite.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a wet desulfurization method for sulfur-containing bauxite, which has the advantages of short flow, low cost, environmental protection and high desulfurization efficiency, so as to reduce the sulfur content in the sulfur-containing bauxite and further improve the comprehensive utilization rate of the bauxite.
In order to solve the technical problems, the invention provides a wet desulfurization method for sulfur-containing bauxite, which comprises the following steps:
Adding bauxite and sulfuric acid solution with pH of 1-5 into an autoclave liner;
sealing the autoclave and discharging air in the autoclave liner;
setting a target heating temperature, heating and stirring to obtain a mixed material of bauxite and sulfuric acid solution;
when the target heating temperature is reached, continuously introducing oxygen into the inner container of the high-pressure kettle for heat preservation to perform oxidation leaching reaction;
after the mixed material is subjected to the oxidation leaching reaction, cooling and taking out slurry in the kettle liner;
Filtering, washing and drying the slurry to obtain the desulfurized bauxite.
Further, the bauxite is bauxite with the granularity of 32-37 mu m formed after grinding.
Further, the mass of sulfuric acid in the sulfuric acid solution is 1.63 g/1t bauxite to 16300g/1t bauxite, and the liquid-solid ratio of the sulfuric acid solution to the bauxite is 500:10 to 500:400.
Preferably, the sulfuric acid mass in the sulfuric acid solution is 163.3g/1t bauxite, and the liquid-solid ratio of the sulfuric acid solution to bauxite is 500:150.
Further, the target heating temperature is 80-240 ℃.
Preferably, the target heating temperature is 150 ℃.
Further, the heat preservation time is 60 min-180 min.
Preferably, the time for the incubation is 120 min.
Further, the oxygen partial pressure is kept at 0.1 MPa-0.8 Mpa after oxygen is continuously introduced into the autoclave liner.
Preferably, the partial pressure of oxygen is maintained at 0.5Mpa after the continuous introduction of oxygen into the autoclave liner.
According to the method for desulfurizing the sulfur-containing bauxite by the wet method, the sulfuric acid solution with the pH of 1-5 is used as the desulfurizing solution for desulfurizing the bauxite, and the acidity of the sulfuric acid solution is low, so that the influence of Fe (OH) 3 precipitation covering layer generated on the surface of the bauxite on the contact of the sulfuric acid solution and minerals in the process of desulfurizing the bauxite can be avoided, the leaching desulfurization efficiency can be influenced, and the oxygen potential of the introduced oxygen can be fully ensured to improve the desulfurizing effect on the sulfur-containing bauxite.
In addition, in the wet desulfurization method for the sulfur-containing bauxite, in the oxidation leaching reaction process of continuously introducing oxygen into the mixed material of the bauxite and the sulfuric acid solution, the desulfurization rate of the sulfur-containing bauxite and the aluminum dissolution rate in the ore after desulfurization can be improved to the greatest extent by controlling the dosage of sulfuric acid, the liquid-solid ratio of the mixed material, the reaction temperature and the heat preservation time of the oxidation leaching and the partial pressure of the introduced oxygen. For bauxite with sulfur content not higher than 2%, the desulfurization rate can reach more than 50%; for bauxite with sulfur content of 2-3%, the desulfurization rate can reach more than 65%; for bauxite with sulfur content more than 3%, the desulfurization rate can reach 80%. The aluminum dissolution rate in the desulfurized bauxite is 5% or less.
Meanwhile, according to the wet desulfurization method for the sulfur-containing bauxite, provided by the invention, only oxygen is continuously introduced into the mixed material of the bauxite and the sulfuric acid solution, the bauxite is subjected to oxidative leaching for a preset time at a target temperature, and then slurry is filtered, washed and dried to obtain the desulfurized bauxite, so that the process is simple, and the desulfurization flow is short. In addition, the used raw materials are simple and easy to obtain, the process cost is low, and the environment is protected.
Drawings
FIG. 1 is a flow chart of a method for wet desulfurization of sulfur-containing bauxite provided in an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a desulfurizing device in the wet desulfurizing method for bauxite containing sulfur according to the embodiment of the present invention.
Detailed Description
Referring to fig. 1, the method for wet desulfurization of sulfur-containing bauxite provided by the embodiment of the invention comprises the following steps:
Step 1) adding bauxite and sulfuric acid solution with pH value of 1-5 into an autoclave liner.
The bauxite is sedimentary bauxite of Guangxi Zhuang autonomous region, the bauxite is not weathered, the phase composition of the bauxite is complex, the sulfur content of the ore is high, the sulfur element of the bauxite mainly exists in the form of associated sulfide ore, and the associated sulfide ore is mainly pyrite. The mineral composition of the composite material mainly comprises 65 to 75 percent of diaspore, less than 0.5 percent of gibbsite, 20 to 25 percent of chlorite and clay mineral, less than 0.5 percent of muscovite, 2to 3 percent of anatase, a small amount of limonite and the like.
Referring to fig. 2, the desulfurization device for wet desulfurization of bauxite containing sulfur of the invention comprises a reaction kettle, an oxygen and nitrogen supply steel bottle connected with the reaction kettle, and a reaction kettle controller connected with the reaction kettle, wherein the reaction kettle is provided with a stirrer and a pressure gauge which are respectively used for stirring materials in the reaction kettle and detecting air pressure in the reaction kettle in real time, and meanwhile, the reaction kettle is also connected with a cooling device which is used for cooling a stirring bearing of the stirrer and cooling the reaction kettle by cooling water. Wherein, as a specific embodiment of the invention, the reaction kettle is a KCFD1-10 high-pressure reaction kettle, the maximum volume of the reaction kettle is 1000 mL, the maximum pressure is 6.0 MPa, the reaction kettle is connected by adopting a flange, and the reaction kettle is heated by an external electric furnace, and the limit temperature is 300 ℃.
In order to facilitate the subsequent oxidative leaching, the sulfur-containing bauxite requires a grinding treatment of the bauxite to a bauxite powder having a particle size of 32 μm to 37 μm prior to loading into the autoclave.
When the initial sulfuric acid consumption is gradually increased, the desulfurization rate of the sulfur-containing bauxite is increased, the pH value of the solution after the reaction is gradually reduced, and the dissolution amount of Al 2O3 is increased. Therefore, increasing the initial sulfuric acid consumption is beneficial to removing sulfur in the sulfur-containing bauxite, the oxidation-reduction equilibrium potential of oxygen under the acidic condition is larger, and the sulfur in the bauxite is more easily oxidized. However, increasing the sulfuric acid consumption increases the concentration of residual acid in the solution, which not only puts higher demands on the reaction equipment, but also increases the cost of neutralizing the acidic wastewater, so that the quality of the sulfuric acid in the sulfuric acid solution is controlled to be 1.63 g/1-16300 g/1t bauxite.
When the liquid-solid ratio is reduced, the desulfurization rate of the sulfur-containing bauxite is slightly reduced from a high level, the pH value is gradually reduced, and the dissolution amount of Al 2O3 is increased. Therefore, increasing the liquid-solid ratio can lead to the reduction of the desulfurization effect in the sulfur-containing bauxite, and simultaneously can increase the residual acid content of the treated liquid, so that the pH of the solution is reduced, and the dissolution amount of Al 2O3 is increased after the concentration of sulfuric acid in unit volume is increased, thereby increasing the treatment cost. Therefore, the liquid-solid ratio of the sulfuric acid solution to bauxite is controlled to be 500:10-500:400.
In a specific embodiment of the present invention, in order to control the dissolution amount of Al 2O3 in treated bauxite to 5% or less and to maintain the desulfurization rate to 80% or more, the sulfuric acid mass in the sulfuric acid solution is controlled to 163.3g/1t bauxite, and the liquid-solid ratio of the sulfuric acid solution to bauxite is controlled to 500:150.
And 2) slowly shaking the autoclave liner, covering the autoclave liner, uniformly sealing the autoclave liner with force, opening a nitrogen steel cylinder, introducing nitrogen into the autoclave liner, flushing the autoclave liner, and discharging air in the sealed autoclave liner.
Step 3) setting a target heating temperature, and heating and stirring to obtain a mixed material of bauxite and sulfuric acid solution. Specifically, a temperature controller is started, the experimental target temperature is set, the mixture of bauxite and sulfuric acid solution is heated, then a stirrer is started to stir the mixture of bauxite and sulfuric acid solution, the rotating speed is controlled at a set value, and meanwhile, stirring shaft cooling water of a cooling device is started to cool a stirring bearing.
Since S in sulfur-containing bauxite is mainly in the form of FeS 2 in bauxite minerals, feS 2 generates S, H 2SO4 and Fe 3+ according to formula 1 or formula 2 when high sulfur bauxite is subjected to pressure oxidation treatment, and the generated H 2SO4 reduces the pH of the desulfurization solution, so that Al 2O3 in bauxite is gradually dissolved in the solution, and Al 2O3 is dissolved.
(1)
(2)
When the desulfurization temperature is gradually increased, the removal rate of S in the treated bauxite is gradually increased, the pH value is gradually reduced, and the dissolution amount of Al 2O3 is increased. And, because the melting point of elemental sulfur is 119 ℃, when the reaction temperature exceeds the melting point of sulfur, the generated sulfur is liquid elemental sulfur, the melted liquid sulfur has poor viscosity and fluidity, and the adhesion of surrounding minerals reduces the reaction area, resulting in a reduction in desulfurization rate. Therefore, increasing the reaction temperature during desulfurization is advantageous for removing S in high-sulfur bauxite, reducing the residual sulfur content in slag components, but increasing the acidity of the treated solution increases the dissolution rate of Al 2O3. Therefore, the target heating temperature is set to 80 to 240 ℃.
In one embodiment of the present invention, the target heating temperature is preferably controlled to 150 ℃ in order to control the dissolution amount of Al 2O3 in the treated bauxite to 5% or less and to maintain the desulfurization rate to 80% or more.
And 4) continuously introducing oxygen into the autoclave liner through an oxygen steel cylinder when the target heating temperature reaches 80-240 ℃, and adjusting the pressure of the autoclave to a required value, wherein the pressure P Total (S) of the autoclave is the sum of the pressure P Oxygen gas of the oxygen and the pressure P Steam generation of water vapor in the autoclave. The oxidation leaching reaction is carried out according to a preset heat preservation time, and the reaction temperature in the autoclave is maintained by cooling water by a cooling device and electric heating in the heat preservation process, so that the fluctuation range of the reaction temperature in the autoclave is controlledWithin 2 ℃.
When oxygen is continuously introduced into the autoclave, when the partial pressure of oxygen is gradually increased, the desulfurization rate of the sulfur-containing bauxite is gradually increased, but basically kept unchanged after the desulfurization rate is increased to a certain value, the pH value is gradually reduced, and the dissolution amount of Al 2O3 is increased. Therefore, the improvement of the oxygen partial pressure during desulfurization is beneficial to the S removal in the high-sulfur bauxite, reduces the residual sulfur content in slag components, but increases the acidity of the treated solution, thereby increasing the dissolution amount of Al 2O3. After the oxygen partial pressure is increased, the concentration of dissolved oxygen in the solution is increased, and the concentration of the reactant is increased, so that the forward movement of the reaction balance of the associated mineral pyrite is facilitated, and the oxidation rate of elemental sulfur is improved. In addition, in the pyrite pressure oxidation process, along with the generation of elemental sulfur, the increase of oxygen partial pressure can further oxidize the elemental sulfur into sulfate, and the dispersion of product sulfur can be fast to a certain extent. Therefore, after continuously introducing oxygen into the autoclave liner, the oxygen partial pressure was maintained at 0.1MPa to 0.8Mpa.
In a specific embodiment of the present invention, in order to control the dissolution amount of Al 2O3 in treated bauxite to 5% or less and to maintain the desulfurization rate to 80% or more, oxygen is continuously introduced into the autoclave liner and then the oxygen partial pressure is maintained at 0.5Mpa.
When the heat preservation time is increased, the desulfurization rate of the sulfur-containing bauxite is increased, the sulfur-containing bauxite basically keeps unchanged after the desulfurization rate is increased to a certain degree, the pH value is gradually reduced, and the dissolution quantity of Al 2O3 is increased. Therefore, the prolonging of the heat preservation time is beneficial to improving the desulfurization rate of the sulfur bauxite, but the heat preservation time of heating is controlled to be 60 min-180 min in consideration of the comprehensive desulfurization effect and time cost.
In one embodiment of the present invention, the heating time is controlled to be 120min in order to control the dissolution amount of Al 2O3 in the treated bauxite to 5% or less and to maintain the desulfurization rate to 80% or more.
And 5) stopping heating and closing an air inlet of the autoclave after the oxidation leaching reaction reaches the target time, dismantling auxiliary devices such as a transmission device, a temperature measuring device and a speed measuring device of the desulfurization device, introducing cooling water to cool the autoclave, and opening an air outlet of the autoclave to completely discharge the gas in the autoclave liner after the temperature in the autoclave is reduced to below 50 ℃. Then opening the kettle cover, taking out the kettle liner, and filtering out leached slurry in the high-pressure kettle liner by adopting a vacuum pump.
And 6) filtering the slurry, repeatedly washing filter residues, cooling to room temperature, and putting the filter residues into a drying oven for drying to obtain the desulfurized bauxite.
The method for wet desulfurization of sulfur-containing bauxite provided by the invention is further described below by referring to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. 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
(1) Adding the grinded bauxite powder with the granularity of 35 mu m into an autoclave liner, adding a sulfuric acid solution with the PH of 3 into the autoclave liner according to the adding amount of the bauxite with the sulfuric acid mass of 163 g/1t in the sulfuric acid solution, and controlling the liquid-solid ratio of the mixed materials to be 500:100.
(2) Slowly shaking the autoclave liner, covering the autoclave liner with a cover, uniformly sealing the autoclave liner with force, then opening a nitrogen steel bottle, introducing nitrogen into the autoclave to flush the autoclave liner, and discharging air in the sealed autoclave liner.
(3) And starting a temperature controller, setting the target heating temperature to be 100 ℃, starting to heat the mixture of the bauxite and the sulfuric acid solution, starting a stirrer to stir the mixture of the bauxite and the sulfuric acid solution, controlling the rotating speed to be a set value, and simultaneously starting stirring shaft cooling water of a cooling device to cool a stirring bearing.
(4) When the target heating temperature reaches 100 ℃, oxygen is continuously introduced into the inner container of the high-pressure kettle through an oxygen steel bottle, and the oxygen partial pressure in the high-pressure kettle is adjusted to be 0.6 MPa. The preset heat preservation time is 120min, the oxidation leaching reaction is carried out, and meanwhile, the reaction temperature in the autoclave is maintained by cooling water and electric heating by a cooling device in the heat preservation process, so that the fluctuation range of the reaction temperature in the autoclave is controlledWithin 2 ℃.
(5) After the oxidation leaching reaction reaches 120 min, stopping heating and closing the air inlet of the autoclave, dismantling the transmission device, the temperature measuring device, the speed measuring device and other auxiliary devices of the desulfurization device, introducing cooling water to cool the autoclave, and opening the air outlet of the autoclave to completely discharge the gas in the kettle liner after the temperature in the autoclave is reduced to below 50 ℃. Then opening the kettle cover, taking out the kettle liner, and filtering out leached slurry in the high-pressure kettle liner by adopting a vacuum pump.
(6) Filtering the slurry, repeatedly washing filter residues, cooling to room temperature, and drying the filter residues in a drying oven to obtain the desulfurized bauxite.
The pH of the solution after the reaction, the sulfur removal rate of bauxite after desulfurization and the dissolution rate of Al 2O3 in this example are shown in Table 1.
TABLE 1
Examples PH after reaction S Removal rate /% Al2O3 Amount of dissolution /%
Example 1 5.78 82.26 3.72
Example 2 4.56 86.36 4.26
Example 3 1.05 85.56 2.77
Example 4 0.68 88.61 3.12
Example 5 0.75 86.47 4.08
From the data of the PH of the solution after reaction, the sulfur removal rate of the bauxite after desulfurization, the dissolution rate of Al 2O3 and the like in the table 1, the wet desulfurization method for the sulfur-containing bauxite provided by the embodiment of the invention can greatly reduce the sulfur content in the sulfur-containing bauxite, and obtain a good desulfurization effect, thereby improving the comprehensive utilization rate of the bauxite.
Example 2
(1) Adding the ground bauxite powder with the granularity of 32 mu m into an autoclave liner, adding a sulfuric acid solution with the PH of 1 into the autoclave liner according to the addition amount of the bauxite with the sulfuric acid mass of 16.3 g/1t in the sulfuric acid solution, and controlling the liquid-solid ratio of the mixed materials to be 500:200.
(2) Slowly shaking the autoclave liner, covering the autoclave liner with a cover, uniformly sealing the autoclave liner with force, then opening a nitrogen steel bottle, introducing nitrogen into the autoclave to flush the autoclave liner, and discharging air in the sealed autoclave liner.
(3) And starting a temperature controller, setting the target heating temperature to be 80 ℃, starting to heat the mixture of the bauxite and the sulfuric acid solution, starting a stirrer to stir the mixture of the bauxite and the sulfuric acid solution, controlling the rotating speed to be a set value, and simultaneously starting stirring shaft cooling water of a cooling device to cool a stirring bearing.
(4) When the target heating temperature reaches 80 ℃, oxygen is continuously introduced into the inner container of the high-pressure kettle through an oxygen steel bottle, and the oxygen partial pressure in the high-pressure kettle is adjusted to be 0.8 MPa. The preset heat preservation time is 180 min, the oxidation leaching reaction is carried out, and meanwhile, the reaction temperature in the autoclave is maintained by cooling water and electric heating by a cooling device in the heat preservation process, so that the fluctuation range of the reaction temperature in the autoclave is controlledWithin 2 ℃.
(5) After the oxidation leaching reaction reaches 180 min, stopping heating and closing the air inlet of the autoclave, dismantling the transmission device, the temperature measuring device, the speed measuring device and other auxiliary devices of the desulfurization device, introducing cooling water to cool the autoclave, and opening the air outlet of the autoclave to completely discharge the gas in the kettle liner after the temperature in the autoclave is reduced to below 50 ℃. Then opening the kettle cover, taking out the kettle liner, and filtering out leached slurry in the high-pressure kettle liner by adopting a vacuum pump.
(6) Filtering the slurry, repeatedly washing filter residues, cooling to room temperature, and drying the filter residues in a drying oven to obtain the desulfurized bauxite.
The pH of the solution after the reaction, the sulfur removal rate of bauxite after desulfurization and the dissolution rate of Al 2O3 in this example are shown in Table 1.
From the data of the PH of the solution after reaction, the sulfur removal rate of the bauxite after desulfurization, the dissolution rate of Al 2O3 and the like in the table 1, the wet desulfurization method for the sulfur-containing bauxite provided by the embodiment of the invention can greatly reduce the sulfur content in the sulfur-containing bauxite, and obtain a good desulfurization effect, thereby improving the comprehensive utilization rate of the bauxite.
Example 3
(1) Adding the ground bauxite powder with the granularity of 37 mu m into an autoclave liner, adding a sulfuric acid solution with the PH of 5 into the autoclave liner according to the adding amount of 1630g/1t bauxite in the sulfuric acid solution, and controlling the liquid-solid ratio of the mixed materials to be 500:400.
(2) Slowly shaking the autoclave liner, covering the autoclave liner with a cover, uniformly sealing the autoclave liner with force, then opening a nitrogen steel bottle, introducing nitrogen into the autoclave to flush the autoclave liner, and discharging air in the sealed autoclave liner.
(3) And starting a temperature controller, setting the target heating temperature to 240 ℃, starting to heat the mixture of the bauxite and the sulfuric acid solution, starting a stirrer to stir the mixture of the bauxite and the sulfuric acid solution, controlling the rotating speed to be a set value, and simultaneously starting stirring shaft cooling water of a cooling device to cool a stirring bearing.
(4) When the target heating temperature reaches 240 ℃, oxygen is continuously introduced into the inner container of the autoclave through an oxygen steel bottle, and the oxygen partial pressure in the autoclave is adjusted to be 0.4 MPa. The preset heat preservation time is 60 min, the oxidation leaching reaction is carried out, and meanwhile, the reaction temperature in the autoclave is maintained by cooling water and electric heating of a cooling device in the heat preservation process, so that the fluctuation range of the reaction temperature in the autoclave is controlledWithin 2 ℃.
(5) After the oxidation leaching reaction reaches 60 minn, stopping heating and closing the air inlet of the autoclave, dismantling the transmission device, the temperature measuring device, the speed measuring device and other auxiliary devices of the desulfurization device, introducing cooling water to cool the autoclave, and opening the air outlet of the autoclave to completely discharge the gas in the kettle liner after the temperature in the autoclave is reduced to below 50 ℃. Then opening the kettle cover, taking out the kettle liner, and filtering out leached slurry in the high-pressure kettle liner by adopting a vacuum pump.
(6) Filtering the slurry, repeatedly washing filter residues, cooling to room temperature, and drying the filter residues in a drying oven to obtain the desulfurized bauxite.
The pH of the solution after the reaction, the sulfur removal rate of bauxite after desulfurization and the dissolution rate of Al 2O3 in this example are shown in Table 1.
From the data of the PH of the solution after reaction, the sulfur removal rate of the bauxite after desulfurization, the dissolution rate of Al 2O3 and the like in the table 1, the wet desulfurization method for the sulfur-containing bauxite provided by the embodiment of the invention can greatly reduce the sulfur content in the sulfur-containing bauxite, and obtain a good desulfurization effect, thereby improving the comprehensive utilization rate of the bauxite.
Example 4
(1) Adding the grinded bauxite powder with the granularity of 36 mu m into an autoclave liner, adding a sulfuric acid solution with the PH of 1-5 into the autoclave liner according to the adding amount of the bauxite with the sulfuric acid mass of 163.3 in the sulfuric acid solution, and controlling the liquid-solid ratio of the mixed materials to be 500:150.
(2) Slowly shaking the autoclave liner, covering the autoclave liner with a cover, uniformly sealing the autoclave liner with force, then opening a nitrogen steel bottle, introducing nitrogen into the autoclave to flush the autoclave liner, and discharging air in the sealed autoclave liner.
(3) And starting a temperature controller, setting the target heating temperature to be 150 ℃, starting to heat the mixture of the bauxite and the sulfuric acid solution, starting a stirrer to stir the mixture of the bauxite and the sulfuric acid solution, controlling the rotating speed to be a set value, and simultaneously starting stirring shaft cooling water of a cooling device to cool a stirring bearing.
(4) When the target heating temperature reaches 150 ℃, oxygen is continuously introduced into the inner container of the high-pressure kettle through an oxygen steel bottle, and the oxygen partial pressure in the high-pressure kettle is adjusted to be 0.5 MPa. The preset heat preservation time is 120 min, the oxidation leaching reaction is carried out, and meanwhile, the reaction temperature in the autoclave is maintained by cooling water and electric heating by a cooling device in the heat preservation process, so that the fluctuation range of the reaction temperature in the autoclave is controlledWithin 2 ℃.
(5) After the oxidation leaching reaction reaches 120 min, stopping heating and closing the air inlet of the autoclave, dismantling the transmission device, the temperature measuring device, the speed measuring device and other auxiliary devices of the desulfurization device, introducing cooling water to cool the autoclave, and opening the air outlet of the autoclave to completely discharge the gas in the kettle liner after the temperature in the autoclave is reduced to below 50 ℃. Then opening the kettle cover, taking out the kettle liner, and filtering out leached slurry in the high-pressure kettle liner by adopting a vacuum pump.
(6) Filtering the slurry, repeatedly washing filter residues, cooling to room temperature, and drying the filter residues in a drying oven to obtain the desulfurized bauxite.
The pH of the solution after the reaction, the sulfur removal rate of bauxite after desulfurization and the dissolution rate of Al 2O3 in this example are shown in Table 1.
From the data of the PH of the solution after reaction, the sulfur removal rate of the bauxite after desulfurization, the dissolution rate of Al 2O3 and the like in the table 1, the wet desulfurization method for the sulfur-containing bauxite provided by the embodiment of the invention can greatly reduce the sulfur content in the sulfur-containing bauxite, and obtain a good desulfurization effect, thereby improving the comprehensive utilization rate of the bauxite.
Example 5
(1) Adding the ground bauxite powder with the granularity of 34 mu m into an autoclave liner, adding a sulfuric acid solution with the PH of 1-5 into the autoclave liner according to the adding amount of 1630g/1t bauxite in the sulfuric acid solution, and controlling the liquid-solid ratio of the mixed materials to be 500:300.
(2) Slowly shaking the autoclave liner, covering the autoclave liner with a cover, uniformly sealing the autoclave liner with force, then opening a nitrogen steel bottle, introducing nitrogen into the autoclave to flush the autoclave liner, and discharging air in the sealed autoclave liner.
(3) And starting a temperature controller, setting the target heating temperature to be 200 ℃, starting to heat the mixture of the bauxite and the sulfuric acid solution, starting a stirrer to stir the mixture of the bauxite and the sulfuric acid solution, controlling the rotating speed to be a set value, and simultaneously starting stirring shaft cooling water of a cooling device to cool a stirring bearing.
(4) When the target heating temperature reaches 200 ℃, oxygen is continuously introduced into the inner container of the high-pressure kettle through an oxygen steel bottle, and the oxygen partial pressure in the high-pressure kettle is adjusted to be 0.3 MPa. The preset heat preservation time is 90 min, the oxidation leaching reaction is carried out, and meanwhile, the reaction temperature in the autoclave is maintained by cooling water and electric heating of a cooling device in the heat preservation process, so that the fluctuation range of the reaction temperature in the autoclave is controlledWithin 2 ℃.
(5) After the oxidation leaching reaction reaches 90 min, stopping heating and closing the air inlet of the autoclave, dismantling the transmission device, the temperature measuring device, the speed measuring device and other auxiliary devices of the desulfurization device, introducing cooling water to cool the autoclave, and opening the air outlet of the autoclave to completely discharge the gas in the kettle liner after the temperature in the autoclave is reduced to below 50 ℃. Then opening the kettle cover, taking out the kettle liner, and filtering out leached slurry in the high-pressure kettle liner by adopting a vacuum pump.
(6) Filtering the slurry, repeatedly washing filter residues, cooling to room temperature, and drying the filter residues in a drying oven to obtain the desulfurized bauxite.
The pH of the solution after the reaction, the sulfur removal rate of bauxite after desulfurization and the dissolution rate of Al 2O3 in this example are shown in Table 1.
From the data of the PH of the solution after reaction, the sulfur removal rate of the bauxite after desulfurization, the dissolution rate of Al 2O3 and the like in the table 1, the wet desulfurization method for the sulfur-containing bauxite provided by the embodiment of the invention can greatly reduce the sulfur content in the sulfur-containing bauxite, and obtain a good desulfurization effect, thereby improving the comprehensive utilization rate of the bauxite.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications and equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and all such modifications and equivalents are intended to be encompassed in the scope of the claims of the present invention.

Claims (6)

1. A method for wet desulfurization of sulfur-containing bauxite, comprising the steps of:
adding bauxite and sulfuric acid solution with pH value of 1-5 into an autoclave liner;
sealing the autoclave and discharging air in the autoclave liner;
Setting the target heating temperature to 80-240 ℃, heating and stirring to obtain a mixed material of bauxite and sulfuric acid solution;
when the target heating temperature is reached, continuously introducing oxygen into the inner container of the high-pressure kettle for heat preservation to perform oxidation leaching reaction;
after the mixed material is subjected to the oxidation leaching reaction, cooling and taking out slurry in the kettle liner;
filtering, washing and drying the slurry to obtain desulfurized bauxite;
Wherein the mass of sulfuric acid in the sulfuric acid solution is 1.63 g/1t bauxite to 16300g/1t bauxite, and the liquid-solid ratio of the sulfuric acid solution to the bauxite is 500:10 to 500:400;
the heat preservation time is 60 min-180 min;
The oxygen partial pressure is kept between 0.1 MPa and 0.8MPa after oxygen is continuously introduced into the autoclave liner.
2. The method for wet desulfurization of sulfur-containing bauxite according to claim 1, characterized in that: the bauxite is bauxite with granularity of 32-37 mu m formed after grinding.
3. The method for wet desulfurization of sulfur-containing bauxite according to claim 1, characterized in that: the mass of sulfuric acid in the sulfuric acid solution is 163.3g/1t bauxite, and the liquid-solid ratio of the sulfuric acid solution to the bauxite is 500:150.
4. The method for wet desulfurization of sulfur-containing bauxite according to claim 1, characterized in that: the target heating temperature was 150 ℃.
5. The method for wet desulfurization of sulfur-containing bauxite according to claim 1, characterized in that: the time of the heat preservation is 120 min.
6. The method for wet desulfurization of sulfur-containing bauxite according to claim 1, characterized in that: and after continuously introducing oxygen into the autoclave liner, the oxygen partial pressure is kept at 0.5MPa.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734698A (en) * 2009-09-08 2010-06-16 东北大学 Method for preparing aluminum oxide from aluminiferous material
CN107986309A (en) * 2017-10-31 2018-05-04 昆明理工大学 A kind of process for sulfur removal with high-sulfur bauxite production aluminium oxide

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1347556A (en) * 1963-02-16 1963-12-27 North American Coal Corp Process for preparing aluminum sulphate from residual pickling liquor and aluminum ore
US3890425A (en) * 1974-03-21 1975-06-17 Southwire Co Redox treatment of alunite ore
CN109554540A (en) * 2018-12-26 2019-04-02 湖南柿竹园有色金属有限责任公司 A kind of method of bismuth concentrate wet underwater welding bismuth
CN212610834U (en) * 2020-07-03 2021-02-26 沈阳鑫博工业技术股份有限公司 High-sulfur bauxite dry-process desulfurization device

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734698A (en) * 2009-09-08 2010-06-16 东北大学 Method for preparing aluminum oxide from aluminiferous material
CN107986309A (en) * 2017-10-31 2018-05-04 昆明理工大学 A kind of process for sulfur removal with high-sulfur bauxite production aluminium oxide

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