CN212687567U - Crystallization transformation regulation and control device for element sulfur in high-sulfur slag in zinc smelting - Google Patents
Crystallization transformation regulation and control device for element sulfur in high-sulfur slag in zinc smelting Download PDFInfo
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- CN212687567U CN212687567U CN202021660547.1U CN202021660547U CN212687567U CN 212687567 U CN212687567 U CN 212687567U CN 202021660547 U CN202021660547 U CN 202021660547U CN 212687567 U CN212687567 U CN 212687567U
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Abstract
The utility model discloses an elemental sulfur crystallization transformation regulation and control device in zinc smelting high-sulfur slag, which comprises a heater, a circulating pump and a crystallization transformation reaction kettle, wherein the crystallization transformation reaction kettle is of a vertical structure, the lower end of one side of the crystallization transformation reaction kettle is provided with a discharge port, the upper end of one side is provided with an overflow port, the top of the crystallization transformation reaction kettle is a feed port, the circulating pump is arranged on a pipeline between the heater inlet of the heater and the overflow port of the crystallization transformation reaction kettle, and the outlet of the heater is connected with the feed port of the crystallization transformation reaction kettle through a circulating pipe; and a new material inlet is also arranged at one side end of the heater inlet. The utility model discloses a crystallization transformation regulation and control and conversion realize the controllable growth and the migration polymerization of elemental sulfur crystal, carry sulphur for the cavitation dissociation and the flotation of follow-up elemental sulfur and create the advantage.
Description
Technical Field
The utility model belongs to the technical field of hydrometallurgy, especially, relate to a zinc is smelted elemental sulphur crystallization transformation and regulation and control device in high sulfur sediment.
Background
Zinc exists mainly in sulfide form in nature, and sulfide ores of zinc mainly include sphalerite and high-iron sphalerite. The zinc smelting process of zinc sulfide concentrate is divided into a pyrometallurgical process and a zinc hydrometallurgy process, wherein the mainstream zinc hydrometallurgy process comprises the conventional zinc hydrometallurgy (roasting-leaching-purifying-electrowinning) and a direct leaching process (oxygen pressure/normal pressure leaching-purifying-electrowinning). A large amount of SO is generated in the roasting process of the conventional wet zinc smelting process2The flue gas has the problems of long process flow, difficult sale and storage of sulfuric acid, serious environmental pollution and the like. The direct zinc leaching process eliminates the process of oxidizing roasting, sulfur in zinc concentrate is oxidized into elemental sulfur to enter acid leaching slag, and SO is avoided2The flue gas pollution is particularly suitable for production enterprises which are located remotely and have difficulty in selling sulfuric acid. The method can well treat the zinc concentrate containing high iron, lead and silicon which is unfavorable for zinc smelting, and the zinc recovery rate is up to more than 97 percent.
There are many methods for recovering elemental sulfur from zinc directly leached high-sulfur slag, and there are mainly physical methods such as a high-pressure decantation method, a vacuum distillation method, a flotation-hot filtration method and the like, and chemical methods such as a xylene leaching method, an ammonium sulfide leaching method, a tetrachloroethylene leaching method and the like, wherein the physical methods are applied in actual production, but all the physical methods have defects in sulfur recovery application. The high-pressure decantation equipment is expensive, and the quality of the produced sulfur is not high; although the sulfur produced by the vacuum distillation method has high purity, the equipment is complex and the production cost is high; the flotation-heat filtration method has simple process and low production cost, is suitable for large-scale industrial production, but has low direct sulfur yield. Therefore, the technical problems of controllable growth and migration polymerization of elemental sulfur crystal phase, high-efficiency separation of the elemental sulfur and other mineral phases, and improvement of the direct yield of the elemental sulfur in the flotation-hot filtration process flow need to be solved urgently.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides an element sulphur crystallization transformation regulation and control device in high sulphur sediment is smelted to zinc through crystallization transformation regulation and control and conversion, realizes the controllable growth and the migration polymerization of elemental sulphur crystal, carries sulphur creation advantage for the cavitation dissociation and the flotation of follow-up elemental sulphur.
In order to solve the technical problem, the utility model adopts the following technical scheme:
the utility model relates to a device for regulating and controlling crystallization transformation of elemental sulfur in zinc smelting high-sulfur slag, which comprises a heater, a circulating pump and a crystallization transformation reaction kettle, wherein the crystallization transformation reaction kettle is of a vertical structure, the lower end of one side of the crystallization transformation reaction kettle is provided with a discharge port, the upper end of one side of the crystallization transformation reaction kettle is provided with an overflow port, the top of the crystallization transformation reaction kettle is a feed port, the circulating pump is arranged on a pipeline between a heater inlet of the heater and the overflow port of the crystallization transformation reaction kettle, and an outlet of the heater is connected with the feed port of the crystallization transformation reaction kettle through a circulating pipe; and a new material inlet is also arranged at one side end of the heater inlet.
Furthermore, a central descending pipe is arranged in the crystallization transformation reaction kettle, a steam outlet is formed in the upper part of the central descending pipe, and a mesh separator is arranged on the inner side of the steam outlet.
Further, the diameter of the crystallization transformation reaction kettle is gradually reduced from top to bottom.
Furthermore, a peripheral jacket for introducing a cooling medium or a heating medium is arranged on the peripheral side of the crystallization transformation reaction kettle.
Furthermore, the flow direction of the peripheral jacket is from bottom to top, a refrigerant is introduced under normal working conditions, a jacket inlet of the peripheral jacket is used for feeding the refrigerant into the peripheral jacket, and the jacket inlet is used for cooling the high-sulfur slag ore pulp to below 120 ℃ so as to generate supersaturation and separate out crystals in the crystallization transformation reaction kettle, wherein the jacket inlet of the peripheral jacket is lower than the jacket outlet.
Furthermore, an adjusting valve for controlling the overflow speed of ore pulp is arranged at the overflow port of the crystallization transformation reaction kettle.
Furthermore, when the heater works, steam enters the heat exchange pipeline of the heater through the steam inlet at the side end of the heater, is cooled after heat transfer to form condensed water, and is discharged through the condensed water outlet.
Further, the working temperature of the heater is 120-155 ℃, and the pressure is 200-550 KPa.
A method for regulating and controlling crystallization transformation of element sulfur in zinc smelting high-sulfur slag comprises the following steps:
A. heating and dissolving process: heating the high-sulfur slag in a heater to obtain ore pulp with good melt flowability;
B. the material conveying process comprises the following steps: the molten high-sulfur slag ore pulp flows to a material inlet of the crystallization transformation reaction kettle through a circulating pipe and enters the inner side of the crystallization transformation reaction kettle through a central descending pipe; the gas is discharged through a steam outlet, and the entrained high-sulfur slag small particles are blocked by a mesh separator and fall into a central descending pipe of the crystallization transformation reaction kettle;
C. and (3) crystallization transformation process: controlling the high-sulfur slag ore pulp within a certain acidity and stirring speed range, cooling to below 120 ℃ under the cooling action of a jacket at the periphery of a crystallization transformation reaction kettle to obtain a supersaturated solution, separating out elemental sulfur crystal crystals, settling and falling into a grading leg at the bottom of the reaction kettle, and carrying out particle size grading to obtain a final product with uniform particle size.
D. The external circulation process is as follows: and (4) enabling the insufficiently grown fine grains and the insufficiently transformed high-sulfur slag ore pulp to flow out through an overflow port in the upper part of the reaction kettle, returning to the step A under the action of a circulating pump, mixing with a new material, and starting the next circulation.
Further, the acidity of the high-sulfur slag ore pulp is 70-100 g/L; the conversion temperature in the crystallization transformation reaction kettle is 80-119 ℃, and the stirring speed is 100-600 r/min.
Further, the high-sulfur slag includes, but is not limited to, leaching slag produced by processing zinc sulfide concentrate by pressure oxygen leaching and atmospheric oxygen leaching.
Compared with the prior art, the utility model discloses a beneficial technological effect:
the utility model provides an elemental sulphur crystallization transformation regulation and control device in high sulphur sediment is smelted to zinc, jointly use heater and crystallization transformation reation kettle, heating effect through the heater, the solubility of elemental sulphur greatly increases in making high sulphur sediment ore pulp, and the solubility of elemental sulphur reduces under the peripheral cooling effect that presss from both sides the cover of crystallization transformation reation kettle, form supersaturated solution and appear sulphur crystal, finally can obtain the particle diameter evenly, the elemental sulphur that floatability can be good, it establishes the basis to carry sulphur for the cavitation dissociation and the flotation of follow-up elemental sulphur. The crystallization transformation device can greatly improve the crystal transformation efficiency of elemental sulfur in the high-sulfur slag, and is centralized in layout and less in occupied area; crystals with larger and uniform particle size can be produced.
Drawings
The present invention will be further explained with reference to the following description of the drawings.
FIG. 1 is a schematic structural view of a device for controlling crystallization transformation of elemental sulfur in high-sulfur slag from zinc smelting according to the present invention;
description of reference numerals: 1-a circulating pump; 2-a circulation pipe; 3-a fresh material inlet; 4-jacket inlet; 5-crystallization transformation reaction kettle; 6-discharging port; 7-a peripheral jacket; 8-central down tube; 9-jacket outlet; 10-a feed inlet; 11-a mesh separator; 12-a steam outlet; 13-an overflow port; 14-a regulating valve; 15-heater outlet; 16-a steam inlet; 17-a heater; 18-a condensate outlet; 19-heater inlet.
Detailed Description
As shown in figure 1, the device for regulating and controlling the crystallization transformation of elemental sulfur in the zinc smelting high-sulfur slag comprises a heater 17, a circulating pump 2 and a crystallization transformation reaction kettle 5, wherein a feed inlet 10, a discharge outlet 6 and an overflow port 13 are arranged on the crystallization transformation reaction kettle 5, the circulating pump 1 is arranged on a circulating pipe 2 between a heater inlet 19 of the heater 17 and the overflow port 13 of the crystallization transformation reaction kettle 5, and a heater outlet 15 is connected with the feed inlet 10 of the crystallization transformation reaction kettle through the circulating pipe 2; one side end of the heater inlet 19 is provided with a fresh material inlet port 3. The inside central down pipe 8 that is equipped with of crystallization transformation reation kettle 5, the upper portion of central down pipe 8 is steam outlet 12, steam outlet 12 inboard is equipped with netted separator 11, and the end of central down pipe 8 extends to the bottom that is close to in crystallization transformation reation kettle 5 to be less than the discharge gate 6 position. The periphery of the crystallization transformation reaction kettle 5 is also provided with a peripheral jacket 7, a refrigerant (or a heating medium) can be introduced into the peripheral jacket 7, the flow direction of the refrigerant (or the heating medium) is downward inlet and upward outlet, the refrigerant is introduced under the normal working condition, a jacket inlet 4 is used for conveying the refrigerant into the peripheral jacket and is used for cooling the high-sulfur slag ore pulp to below 120 ℃, so that the high-sulfur slag ore pulp generates supersaturation and crystals are separated out in the crystallization transformation reaction kettle, and the jacket inlet 4 is lower than the jacket outlet 9. An overflow port 13 of the crystallization transformation reaction kettle 5 is provided with an adjusting valve 14 for controlling the overflow speed of ore pulp. When the heater 17 works, steam enters the heat exchange pipeline of the heater through the steam inlet 16 at the side end of the steam, is cooled after heat is transferred to form condensed water, and is discharged through the condensed water outlet 18. The working temperature of the heater is 120-155 ℃, and the pressure is 200-550 KPa.
The crystallization transformation method adopting the device comprises the following steps:
A. heating and dissolving process: heating the high-sulfur slag in a heater to obtain ore pulp with good melt flowability;
B. the material conveying process comprises the following steps: the molten high-sulfur slag ore pulp flows to a material inlet of the crystallization transformation reaction kettle through a circulating pipe and enters the inner side of the crystallization transformation reaction kettle through a central descending pipe; the gas is discharged through a steam outlet, and the entrained high-sulfur slag small particles are blocked by a mesh separator and fall into a central descending pipe of the crystallization transformation reaction kettle;
C. and (3) crystallization transformation process: controlling the high-sulfur slag ore pulp within a certain acidity and stirring speed range, cooling to below 120 ℃ under the cooling action of a jacket at the periphery of a crystallization transformation reaction kettle to obtain a supersaturated solution, separating out elemental sulfur crystal crystals, settling and falling into a grading leg at the bottom of the reaction kettle, and carrying out particle size grading to obtain a final product with uniform particle size.
D. The external circulation process is as follows: and (4) enabling the insufficiently grown fine grains and the insufficiently transformed high-sulfur slag ore pulp to flow out through an overflow port in the upper part of the reaction kettle, returning to the step A under the action of a circulating pump, mixing with a new material, and starting the next circulation.
The invention is illustrated by the following specific examples.
Example 1
Heating the high-sulfur slag in a heater to obtain high-sulfur slag pulp, entering the inner side of a crystallization transformation reaction kettle through a circulating pipe and a central descending pipe of the crystallization transformation reaction kettle, cooling the crystallization transformation reaction kettle to 85 ℃ under the cooling action of a peripheral jacket, stirring at a stirring speed of 500r/min by a stirring paddle, and obtaining a transformation product with uniform particle size by directional crystallization transformation in the crystallization transformation reaction kettle, wherein the acidity of the high-sulfur slag pulp is 90 g/L.
And (4) conclusion: the particle size distribution of the elemental sulfur particles is 2-120 μm, and the volume median diameter d (0.5) is 36 μm.
Example 2
Heating the high-sulfur slag in a heater to obtain high-sulfur slag pulp, feeding the high-sulfur slag pulp into the inner side of a crystallization transformation reaction kettle through a circulating pipe and a central descending pipe of the crystallization transformation reaction kettle, cooling the crystallization transformation reaction kettle to 100 ℃ under the cooling action of a peripheral jacket, stirring the high-sulfur slag pulp at a stirring speed of 100r/min and the acidity of 75g/L by a stirring paddle, and performing directional crystallization transformation in the crystallization transformation reaction kettle to finally obtain a transformation product with uniform granularity.
And (4) conclusion: the particle size distribution of the elemental sulfur particles is 5-110 μm, and the volume median diameter d (0.5) is 30 μm.
Example 3
Heating the high-sulfur slag in a heater to obtain high-sulfur slag pulp, entering the inner side of a crystallization transformation reaction kettle through a circulating pipe and a central descending pipe of the crystallization transformation reaction kettle, cooling the crystallization transformation reaction kettle to 110 ℃ under the cooling action of a peripheral jacket, stirring at a stirring speed of 250r/min by a stirring paddle, and obtaining a transformation product with uniform particle size by directional crystallization transformation in the crystallization transformation reaction kettle, wherein the acidity of the high-sulfur slag pulp is 80 g/L.
And (4) conclusion: the particle size distribution of the elemental sulfur particles is 5-145 μm, and the volume median diameter d (0.5) ═ 41 μm through the measurement of a particle size analyzer.
The above-mentioned embodiments are only intended to describe the preferred embodiments of the present invention, but not to limit the scope of the present invention, and those skilled in the art should also be able to make various modifications and improvements to the technical solution of the present invention without departing from the spirit of the present invention, and all such modifications and improvements are intended to fall within the scope of the present invention as defined in the appended claims.
Claims (8)
1. The utility model provides an element sulphur crystallization transformation regulation and control device in zinc smelting high sulfur sediment which characterized in that: the crystallization transformation reaction kettle is of a vertical structure, a discharge port is arranged at the lower end of one side of the crystallization transformation reaction kettle, an overflow port is arranged at the upper end of one side of the crystallization transformation reaction kettle, a feed port is arranged at the top of the crystallization transformation reaction kettle, the circulating pump is arranged on a pipeline between an inlet of the heater and the overflow port of the crystallization transformation reaction kettle, and an outlet of the heater is connected with the feed port of the crystallization transformation reaction kettle through a circulating pipe; and a new material inlet is also arranged at one side end of the heater inlet.
2. The device for regulating and controlling the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 1, characterized in that: the crystallization transformation reaction kettle is internally provided with a central down pipe, the upper part of the central down pipe is a steam outlet, and the inner side of the steam outlet is provided with a mesh separator.
3. The device for regulating and controlling the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 1, characterized in that: the diameter of the crystallization transformation reaction kettle is gradually reduced from top to bottom.
4. The device for regulating and controlling the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 1, characterized in that: and a peripheral jacket for introducing a refrigerant or a heating medium is arranged on the peripheral side of the crystallization transformation reaction kettle.
5. The device for regulating and controlling the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 4, characterized in that: the flow direction of the peripheral jacket is from bottom to top, a refrigerant is introduced under the normal working condition, a jacket inlet of the peripheral jacket is used for conveying the refrigerant into the peripheral jacket, and the jacket inlet is used for cooling the high-sulfur slag ore pulp to below 120 ℃ so as to generate supersaturation and separate out crystals in the crystallization transformation reaction kettle, wherein the jacket inlet of the peripheral jacket is lower than a jacket outlet.
6. The device for regulating and controlling the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 1, characterized in that: and an adjusting valve for controlling the overflow speed of ore pulp is arranged at the overflow port of the crystallization transformation reaction kettle.
7. The device for regulating and controlling the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 1, characterized in that: when the heater works, steam enters the heat exchange pipeline of the heater through the steam inlet at the side end of the heater, is cooled after heat transfer to form condensed water, and is discharged through the condensed water outlet.
8. The device for regulating and controlling the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 1, characterized in that: the working temperature of the heater is 155 ℃ and the pressure is 200 KPa and 550 KPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111874870A (en) * | 2020-08-11 | 2020-11-03 | 中南大学 | Device and method for regulating and controlling crystallization transformation of element sulfur in high-sulfur slag in zinc smelting |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111874870A (en) * | 2020-08-11 | 2020-11-03 | 中南大学 | Device and method for regulating and controlling crystallization transformation of element sulfur in high-sulfur slag in zinc smelting |
| CN111874870B (en) * | 2020-08-11 | 2023-08-18 | 中南大学 | Device and method for regulating and controlling element sulfur crystallization transformation in zinc smelting high-sulfur slag |
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