阅读说明：本技术 一种锌冶炼高硫渣中元素硫晶化转型调控装置及其方法 (Device and method for regulating and controlling crystallization transformation of element sulfur in high-sulfur slag in zinc smelting ) 是由 陈永明 常聪 李云 代杰 胡方圆 向长柳 何静 杨声海 于 2020-08-11 设计创作，主要内容包括：本发明公开了一种锌冶炼高硫渣中元素硫晶化转型调控装置,包括加热器、循环泵和晶化转型反应釜,所述晶化转型反应釜为立式结构,所述晶化转型反应釜一侧下端设置有出料口,一侧上端设置有溢流口,顶部为进料口,所述循环泵安装在所述加热器的加热器入口与所述晶化转型反应釜的溢流口之间的管道上,所述加热器出口与所述晶化转型反应釜的进料口之间通过循环管相连；所述加热器入口的一侧端还设置有新料进入口。还公布了其晶化转型调控方法。本发明通过晶化转型调控与转化,实现单质硫晶体的可控生长和迁移聚合,为后续单质硫的空化解离和浮选提硫创造有利条件。(The invention discloses a device for regulating and controlling crystallization transformation of element 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 hole, 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 hole, 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 hole 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. Also discloses a crystallization transformation regulation and control method thereof. The invention realizes the controllable growth and migration polymerization of the elemental sulfur crystal through the crystallization transformation regulation and transformation, and creates favorable conditions for the subsequent cavitation dissociation and flotation sulfur extraction of the elemental sulfur.)

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 1, 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 the 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.

9. A method for regulating and controlling crystallization transformation of element sulfur in zinc smelting high-sulfur slag is characterized by comprising 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.

10. The method for regulating, controlling and recovering the crystallization transformation of the elemental sulfur in the zinc smelting high-sulfur slag according to claim 9, characterized in that: 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.

Technical Field

The invention belongs to the technical field of wet metallurgy, and particularly relates to a device and a method for regulating and controlling crystallization transformation of elemental sulfur in zinc smelting high-sulfur slag.

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.

Disclosure of Invention

In order to solve the technical problems, the invention provides a device and a method for regulating and controlling the crystallization transformation of elemental sulfur in high-sulfur slag in zinc smelting.

In order to solve the technical problems, the invention adopts the following technical scheme:

the invention 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 hole, 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 provided with a feed hole, the circulating pump is arranged on a pipeline between the 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 hole of the crystallization transformation reaction kettle through a; 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 invention has the beneficial technical effects that:

according to the device for regulating and controlling the crystallization transformation of the elemental sulfur in the high-sulfur slag in the zinc smelting, the heater and the crystallization transformation reaction kettle are used in a combined manner, the solubility of the elemental sulfur in the ore pulp of the high-sulfur slag is greatly increased under the heating action of the heater, the solubility of the elemental sulfur is reduced under the cooling action of the jacket at the periphery of the crystallization transformation reaction kettle, a supersaturated solution is formed to precipitate sulfur crystals, and finally, the elemental sulfur with uniform particle size and good floatability can be obtained, so that a foundation is laid for the subsequent cavitation dissociation and flotation sulfur extraction of the elemental sulfur. 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 invention is further illustrated in the following description with reference to the drawings.

FIG. 1 is a schematic structural diagram 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.