CN103466558B - Method for separating sulfur from zinc sulfide concentrate - Google Patents
Method for separating sulfur from zinc sulfide concentrate Download PDFInfo
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- CN103466558B CN103466558B CN201310412138.8A CN201310412138A CN103466558B CN 103466558 B CN103466558 B CN 103466558B CN 201310412138 A CN201310412138 A CN 201310412138A CN 103466558 B CN103466558 B CN 103466558B
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- sulfur
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- zinc sulfate
- temperature
- zinc
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 119
- 239000011593 sulfur Substances 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000012141 concentrate Substances 0.000 title claims abstract description 40
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 34
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052984 zinc sulfide Inorganic materials 0.000 title claims abstract description 31
- 238000002386 leaching Methods 0.000 claims abstract description 75
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 42
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 42
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 42
- 238000001704 evaporation Methods 0.000 claims abstract description 31
- 230000008020 evaporation Effects 0.000 claims abstract description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004821 distillation Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 37
- 239000000243 solution Substances 0.000 description 35
- 239000005864 Sulphur Substances 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000002893 slag Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005188 flotation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for separating sulfur from zinc sulfide concentrate. The method comprises the following steps of: leaching zinc sulfide concentrate by utilizing sulfuric acid so as to obtain zinc sulfate leaching liquor; and evaporating the zinc sulfate leaching liquor so as to obtain sulfur-containing vapor, wherein the evaporation treatment is carried out under a condition that the temperature of the zinc sulfate leaching liquor is 125 DEG C-300 DEG C under the pressure of 10-25 Mpa. The method disclosed by the invention can be used for solving the problems that the grade of the sulfur extracted by adopting high-temperature distillation is low, the energy consumption is high; moreover, the grade of the separated sulfur can be obviously improved.
Description
Technical Field
The invention relates to the field of metallurgy, in particular to a method for separating sulfur from zinc sulfide concentrate.
Background
When the horizontal pressurized reaction kettle is used for treating zinc sulfide concentrate, a large amount of zinc is dissolved out and enters a zinc sulfate solution, and a large amount of sulfur enters a boiling slag phase in the form of elemental sulfur. In the actual production process, a large amount of sulfur wraps other impurity elements in the cooling process and enters slag, so that the sulfur grade is low, and sulfur-containing slag needs to be separated by sulfur flotation to generate sulfur concentrate. A large amount of zinc-containing liquid is generated during sulfur selection, a wet-process zinc electrolysis system is difficult to control, and in the operation process, the rapid bonding of elemental sulfur on a coil can occur due to the sharp drop of the temperature of the coil, so that the caking in a kettle is caused in severe cases. The temperature control in the pressure leaching process is too high, so that the viscosity of the elemental sulfur is increased sharply, the service life of lining bricks and cement in the autoclave is adversely affected, and the safe operation risk and the subsequent processing cost of the horizontal pressure reaction kettle are increased.
Therefore, the process of separating sulphur from zinc sulphide concentrate is in need of further improvement.
Disclosure of Invention
The present invention aims to solve at least one of the above technical problems to at least some extent or to at least provide a useful commercial choice. Therefore, the invention aims to provide a method for separating sulfur from zinc sulfide concentrate, which has simple process and easy implementation and can extract the sulfur with high purity.
In one aspect of the invention, the invention proposes a method of separating sulphur from zinc sulphide concentrate, the method comprising, according to an embodiment of the invention: leaching the zinc sulfide concentrate by using sulfuric acid so as to obtain zinc sulfate leachate; and evaporating the zinc sulfate leaching solution to obtain sulfur-containing water vapor, wherein the evaporation treatment is carried out under the condition that the temperature of the zinc sulfate leaching solution is controlled to be 125-300 ℃ under the pressure of 10-25 Mpa. Therefore, the problems of low grade, high energy consumption and the like of extracted sulfur in the prior art can be solved, and the purity of the sulfur is further improved.
In addition, the method for separating sulfur from zinc sulfide concentrate according to the above embodiment of the present invention may further have the following additional technical features:
according to the embodiment of the invention, the evaporation treatment is carried out under the condition that the temperature of the zinc sulfate leaching solution is controlled to be 160-250 ℃. Therefore, the sulfur produced in the pressure leaching process can be in the state of elemental sulfur, so that the evaporation efficiency of the sulfur in the zinc sulfate leaching solution is further improved.
According to the embodiment of the invention, the acidity of the zinc sulfate leaching solution is 25-65 g/L. Thereby preventing the sulfur produced in the leaching solution from being converted into SO4 2-So as to further improve the evaporation efficiency of sulfur in the zinc sulfate leaching solution.
According to the embodiment of the invention, the liquid-solid ratio of the zinc sulfate leaching solution is (5 mL: 1g) to (10 mL:1 g). Therefore, the effective evaporation amount of the zinc sulfate leaching solution in the pressure evaporation process can be ensured, so that the continuity of the sulfur distillation operation can be further ensured.
According to an embodiment of the invention, the method further comprises: cooling the sulfur-containing steam to obtain the sulfur.
According to the embodiment of the invention, the cooling treatment is carried out at the temperature of 25-65 ℃ and the pressure of 0.1-0.5 MPa. Thereby leading the sulfur-containing steam to be rapidly cooled so as to further improve the evaporation efficiency of the sulfur in the zinc sulfate leaching solution.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The following detailed description of the embodiments of the present invention is intended to be illustrative, and not to be construed as limiting the invention.
In the prior art, when a horizontal pressurized reaction kettle is adopted to treat zinc sulfide concentrate, a large amount of generated sulfur enters slag due to the fact that other impurity elements are wrapped in the slag in the cooling process, so that the sulfur grade is low, and sulfur concentrate is generated by the sulfur-containing slag through flotation separation. In the process of selecting sulfur from the sulfur concentrate leaching solution, the temperature of a pipe disc is sharply reduced to cause the sulfur to be bonded on the pipe disc, and in the serious process, the sulfur is caked in a kettle, and meanwhile, the control temperature in the pressure leaching process is too high, so that the safe operation risk and the subsequent processing cost of the pressure reaction kettle can be obviously increased.
To this end, in one aspect of the invention, the invention proposes a method of separating sulphur from zinc sulphide concentrate, the method comprising, according to an embodiment of the invention: leaching the zinc sulfide concentrate by using sulfuric acid so as to obtain zinc sulfate leachate; and evaporating the zinc sulfate leaching solution to obtain sulfur-containing water vapor, wherein the evaporation treatment is carried out under the condition that the temperature of the zinc sulfate leaching solution is controlled to be 125-300 ℃ under the pressure of 10-25 Mpa. According to the method, the zinc sulfide concentrate is leached under a high-temperature and high-pressure environment, the problems that the sulfur grade is low due to the fact that the horizontal reaction kettle wraps impurity elements in the process of treating the zinc sulfide concentrate, and the viscosity of the elemental sulfur is increased to cause in-kettle caking and the like can be effectively avoided, and the sulfur grade can be remarkably improved. The method can effectively solve the technical problems of complex subsequent flow, high energy consumption, low recovery rate of valuable metals and the like in the process of extracting the sulfur by adopting a conventional method, and can obviously improve the grade of the separated sulfur.
According to an embodiment of the present invention, the temperature of the zinc sulfate leaching solution evaporation treatment is not particularly limited, and according to an embodiment of the present invention, the evaporation treatment may be performed under a condition that the temperature of the zinc sulfate leaching solution is controlled to be 160 to 250 ℃. If the temperature is lower than 160 ℃, a large amount of sulfur dissolved out in the zinc sulfate leaching solution is converted into SO4 2-The evaporation amount of sulfur is reduced, the terminal acidity of the zinc sulfate leaching solution is increased, the neutralization cost of the subsequent process is increased, if the temperature is higher than 250 ℃, a large amount of sulfur in the solution is evaporated, and meanwhile, a large amount of aqueous solution is evaporated along with the evaporation of the sulfur, so that the liquid-solid ratio of the pressure kettle is disordered, the caking and the kettle caking of the pressure leaching kettle are easily caused, and the production accident is caused. Therefore, the temperature of the zinc sulfate leaching solution is controlled within the range of 160-250 ℃, so that the sulfur evaporation efficiency can be further improved.
According to an embodiment of the present invention, the acidity of the zinc sulfate leachate is not particularly limited, and according to an embodiment of the present invention, the acidity of the zinc sulfate leachate may be 25 to 65 g/L. If the acidity of the zinc sulfate leaching solution is lower than 25g/L, the zinc sulfide is not leached completely, so that a large amount of sulfur is left in leaching residues, the sulfur conversion rate is low, and the evaporation amount of the sulfur is influenced,if the acidity is higher than 65g/L, a large amount of sulfur dissolved out in the zinc sulfate leaching solution is converted into SO4 2-The end point acidity of the leaching solution is increased, and the neutralization cost of the subsequent process is increased. Therefore, the acidity of the zinc sulfate leaching solution is controlled within the range of 25-65 g/L, so that the sulfur evaporation efficiency is further improved.
According to an embodiment of the present invention, the liquid-solid ratio of the zinc sulfate leaching solution is not particularly limited, and according to an embodiment of the present invention, the liquid-solid ratio of the zinc sulfate leaching solution may be (5 mL: 1g) to (10 mL:1 g). If the liquid-solid ratio of the zinc sulfate leaching solution is lower than 5mL:1g, the acidity of the solution before leaching is required to be high, the solution viscosity is high in the leaching process, sulfur is wrapped easily to be unfavorable for sulfur evaporation, the sulfur evaporation amount is reduced, sulfur extraction is not favorable, equipment accidents are caused easily due to the fact that a mechanical stirring device is high in load, and if the liquid-solid ratio is higher than 10mL:1g, a large amount of sulfur is converted into SO4 2Entering the solution to participate in the leaching reaction, also resulting in a reduction in the amount of sulfur extracted. The liquid-solid ratio of the zinc sulfate leaching solution is controlled within the range of (5 mL: 1g) to (10 mL: 1g) so as to further improve the sulfur evaporation efficiency.
According to an embodiment of the present invention, the method for separating sulfur from zinc sulfide concentrate may further include: cooling the sulfur-containing water vapor to obtain sulfur. According to the embodiment of the invention, the closed device made of acid-resistant and temperature-resistant materials can be adopted to collect the sulfur-containing vapor, the temperature in the closed device is controlled to condense the sulfur-containing vapor, the sulfur in the sulfur-containing vapor is crystallized and separated out, and the vapor is liquefied into water which is further returned to the reaction kettle for evaporation treatment, so that the liquid-solid ratio of the zinc sulfate leaching solution can be further maintained, and the evaporation efficiency is further improved.
According to an embodiment of the present invention, the condition for cooling the sulfur-containing water vapor is not particularly limited, and according to an embodiment of the present invention, the cooling process may be performed at a temperature of 25 to 65 degrees celsius and a pressure controlled within a range of 0.1 to 0.5 Mpa. According to the specific example of the invention, when the pressure of the closed device exceeds 0.55MPa, the device is disassembled in time so as to recover the sulfur. If the cooling system high temperature (be higher than 65 ℃) will lead to the unable cooling formation solid-state sulphur of a large amount of sulphur steam, be unfavorable for the extraction of sulphur, if the cooling system low temperature (be less than 25 ℃), a large amount of sulphur steam turns into solid-state sulphur fast, lead to the sulphur moisture too high, if the cooling system high pressure (be higher than 0.5 Mpa) will lead to a large amount of sulphur steam to be in the boiling state for a long time simultaneously, be unfavorable for the form conversion of sulphur, if the cooling system low pressure (be less than 0.1 Mpa) will influence the conversion efficiency of sulphur, make gaseous sulphur turn into the time extension of solid-state sulphur, be unfavorable for the extraction of sulphur equally. Therefore, the sulfur-containing water vapor is condensed under the low-temperature and low-pressure cooling treatment condition, so that the condensation efficiency of the sulfur-containing water vapor can be remarkably improved, and the sulfur extraction efficiency is further improved.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
Performing pressure leaching treatment on the zinc sulfide concentrate, and controlling the liquid-solid ratio of sulfuric acid to the zinc sulfide concentrate in the leaching process to be 5mL:1g so as to ensure that the pressure leaching process has effective evaporation capacity; the method comprises the steps of controlling the temperature in the pressure leaching process to be 125 ℃, the pressure to be 10Mpa and the final acidity to be 25g/L, and distilling sulfur in zinc sulfate concentrate leachate to ensure that the sulfur exists in the form of elemental sulfur in the pressure leaching process and the produced sulfur is not oxidized into SO4 2-(ii) a The distilled sulfur-containing vapor is collected in a centralized manner by adopting a closed device, the temperature in the closed device is controlled to be 25 ℃, and the pressure is controlled to be within the range of 0.1-0.5 MPa, so that sulfur and vapor in the sulfur-containing vapor are condensed; when the pressure in the closed device exceeds 0.55MPa, the closed device is disassembled in time so as to recover the sulfur, and the grade of the obtained sulfur is 99.94 percent.
Example 2
Performing pressure leaching treatment on the zinc sulfide concentrate, and controlling the liquid-solid ratio of sulfuric acid to the zinc sulfide concentrate in the leaching process to be 10mL:1g so as to ensure that the pressure leaching process has effective evaporation capacity; controlling the temperature of the pressure leaching process to be 300 ℃, the pressure to be 25Mpa and the final acidity to be 65g/L, and distilling the sulfur in the zinc sulfate concentrate leaching solution to ensure that the sulfur exists in the form of elemental sulfur in the pressure leaching process and the produced sulfur is not oxidized into SO4 2-(ii) a The distilled sulfur-containing vapor is collected in a centralized manner by adopting a closed device, the temperature in the closed device is controlled to be 65 ℃, and the pressure in the closed device is controlled to be within the range of 0.1-0.5 MPa, so that sulfur and vapor in the sulfur-containing vapor are condensed; when the pressure in the closed device exceeds 0.55MPa, the closed device is disassembled in time so as to recover the sulfur, and the grade of the obtained sulfur is 99.93 percent.
Example 3
Performing pressure leaching treatment on the zinc sulfide concentrate, and controlling the liquid-solid ratio of sulfuric acid to the zinc sulfide concentrate in the leaching process to be 6.5mL:1g so as to ensure that the pressure leaching process has effective evaporation capacity; controlling the temperature of the pressure leaching process to be 175 ℃, the pressure to be 15Mpa and the final acidity to be 40g/L, and distilling the sulfur in the zinc sulfate concentrate leaching solution to ensure that the sulfur exists in the form of elemental sulfur in the pressure leaching process and the produced sulfur is not oxidized into SO4 2-(ii) a The method comprises the following steps of (1) adopting a closed device to intensively collect distilled sulfur-containing vapor, controlling the temperature in the closed device to be 35 ℃ and the pressure in the range of 0.1-0.5 MPa, so as to condense sulfur and vapor in the sulfur-containing vapor; when the pressure in the closed device exceeds 0.55MPa, the closed device is disassembled in time so as to recover the sulfur, and the grade of the obtained sulfur is 99.95 percent.
Example 4
The zinc sulfide concentrate is processed by pressure leachingControlling the liquid-solid ratio of sulfuric acid to zinc sulfide concentrate in the leaching process to be 8mL:1g so as to ensure that the pressure leaching process has effective evaporation capacity; controlling the temperature of the pressure leaching process to be 250 ℃, the pressure to be 20Mpa and the final acidity to be 50g/L, and distilling the sulfur in the zinc sulfate concentrate leaching solution to ensure that the sulfur exists in the form of elemental sulfur in the pressure leaching process and the produced sulfur is not oxidized into SO4 2-(ii) a The method comprises the following steps of (1) adopting a closed device to intensively collect distilled sulfur-containing vapor, controlling the temperature in the closed device to be 50 ℃ and the pressure in the range of 0.1-0.5 MPa, so as to condense sulfur and vapor in the sulfur-containing vapor; when the pressure in the closed device exceeds 0.55MPa, the closed device is disassembled in time so as to recover the sulfur, and the grade of the obtained sulfur is 99.945%.
Comparative example 1
Performing pressure leaching treatment on zinc sulfide concentrate, controlling the solid-to-solid ratio of sulfuric acid to the zinc sulfide concentrate in the leaching process to be 4mL:1g, controlling the temperature in the pressure leaching process to be 100 ℃, the pressure to be 5Mpa and the terminal acidity to be 20g/L, performing distillation treatment on sulfur in the zinc sulfide concentrate leachate, controlling the cooling temperature to be 20 ℃ and the cooling pressure to be 0.1-0.5 MPa, and performing concentrated collection on distilled sulfur-containing steam by adopting a closed device so as to condense the sulfur and the steam in the sulfur-containing steam; meanwhile, when the pressure in the closed device exceeds 0.55MPa, the closed device is timely disassembled, and sulfur is recovered, so that the grade of the obtained sulfur is 99.85%.
Comparative example 2
Performing pressure leaching treatment on zinc sulfide concentrate, controlling the solid-to-solid ratio of sulfuric acid to the zinc sulfide concentrate in the leaching process to be 15mL:1g, controlling the temperature in the pressure leaching process to be 350 ℃, the pressure to be 30Mpa and the terminal acidity to be 70g/L, performing distillation treatment on sulfur in the zinc sulfide concentrate leachate, controlling the cooling temperature to be 70 ℃ and the cooling pressure to be 0.1-0.5 MPa, and performing concentrated collection on distilled sulfur-containing steam by adopting a closed device so as to condense the sulfur and the steam in the sulfur-containing steam; meanwhile, when the pressure in the closed device exceeds 0.55MPa, the closed device is timely disassembled, and sulfur is recovered. The grade of the obtained sulfur is 98.35 percent.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (2)
1. A method for separating sulfur from zinc sulfide concentrate, comprising:
leaching the zinc sulfide concentrate by using sulfuric acid so as to obtain zinc sulfate leachate;
evaporating the zinc sulfate leaching solution to obtain sulfur-containing water vapor; and
cooling the sulfur-containing water vapor to obtain the sulfur,
wherein,
the evaporation treatment is carried out under the pressure of 10-25 MPa and the temperature of the zinc sulfate leaching solution is controlled to be 125-300 ℃,
the acidity of the zinc sulfate leaching solution is 25-65 g/L,
the liquid-solid ratio of the zinc sulfate leaching solution is (5 mL: 1g) to (10 mL: 1g),
the cooling treatment is carried out at a temperature of 25-65 ℃ and a pressure of 0.1-0.5 MPa.
2. The method according to claim 1, wherein the evaporation treatment is performed under the condition that the temperature of the zinc sulfate leaching solution is controlled to be 160-250 ℃.
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