CN112010266A - Method for preparing sodium sulfide by melting reduction of industrial sodium sulfate - Google Patents
Method for preparing sodium sulfide by melting reduction of industrial sodium sulfate Download PDFInfo
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- CN112010266A CN112010266A CN202010773152.0A CN202010773152A CN112010266A CN 112010266 A CN112010266 A CN 112010266A CN 202010773152 A CN202010773152 A CN 202010773152A CN 112010266 A CN112010266 A CN 112010266A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/24—Preparation by reduction
- C01B17/26—Preparation by reduction with carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to the technical field of sodium sulfide preparation, and discloses a method for preparing sodium sulfide by melting and reducing industrial sodium sulfate. The method comprises the following steps: (1) mixing industrial sodium sulfate and a reducing agent, and then carrying out ball milling to obtain a mixture with the fineness of less than or equal to 200 meshes; (2) adding the mixture obtained in the step (1) into a medium frequency induction converting furnace, heating to a molten state, blowing mixed gas for converting reduction, reducing molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out of the medium frequency induction converting furnace; (3) pouring and molding the molten sodium sulfide poured out in the step (2); wherein, in the step (1), the mass ratio of the industrial sodium sulfate to the reducing agent is 1: 0.4-1. The method takes industrial sodium sulfate as a raw material, adds a reducing agent, adopts an all-fire method to melt and reduce the industrial sodium sulfate into sodium sulfide, is simple and environment-friendly, has small corrosion to equipment, and prepares the sodium sulfide with high purity, and the content of the sodium sulfide reaches more than 90 percent by weight.
Description
Technical Field
The invention relates to the technical field of sodium sulfide preparation, in particular to a method for preparing sodium sulfide by melting and reducing industrial sodium sulfate.
Background
At present, the vanadium extraction process mainly comprises a sodium vanadium extraction process and a calcium vanadium extraction process, and the sodium vanadium extraction process is relatively mature, high in vanadium yield and low in cost, but can generate a large amount of industrial sodium sulfate in the production process, so that the comprehensive utilization difficulty is high, and the environmental protection pressure of enterprises is high.
The Panzhihua vanadium plant of Panzhi vanadium-titanium company adopts sodium treatment vanadium extraction process, and the industrial sodium sulfate produced every year is above 7 ten thousand tons. At present, most of industrial sodium sulfate generated by treatment in a stockpiling treatment mode (rainproof and anti-seepage treatment) is adopted; a small part of the sodium sulfide is sold to peripheral enterprises for producing sodium sulfide (by adopting a short-kiln coal-based reduction process), the content of the produced sodium sulfide is about 50-55 wt%, and the sodium sulfide is mainly sold to the colored ore dressing enterprises around Yunnan as an ore dressing agent.
The sodium sulfide prepared by reducing industrial sodium sulfate serving as a raw material provides better raw material selection for the fields of printing and dyeing, chemical industry and colored mineral separation, but the problems that the process is complex, the purity of the obtained sodium sulfide is not high, the pollution to the environment is large, the corrosion to equipment is serious, the energy consumption is large and the like exist when the sodium sulfide is prepared by adopting a water immersion process and the industrial sodium sulfate serving as the raw material in the prior art.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a method for preparing sodium sulfide by melting and reducing industrial sodium sulfate.
In order to achieve the above object, the present invention provides a method for preparing sodium sulfide by reducing industrial sodium sulfate, comprising the steps of:
(1) mixing industrial sodium sulfate and a reducing agent, and then carrying out ball milling to obtain a mixture with the fineness of less than or equal to 200 meshes;
(2) adding the mixture obtained in the step (1) into a medium frequency induction converting furnace, heating to a molten state, blowing mixed gas for converting reduction, reducing molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out of the medium frequency induction converting furnace;
(3) pouring and molding the molten sodium sulfide poured out in the step (2);
wherein, in the step (1), the mass ratio of the industrial sodium sulfate to the reducing agent is 1: 0.4-1.
Preferably, in the step (1), the industrial sodium sulfate is a byproduct of a sodium-modified vanadium extraction process; more preferably, the content of sodium sulfate in the industrial sodium sulfate is 95 wt% or more.
Preferably, in the step (1), the reducing agent is coal powder or coke powder; further preferably, the ash content in the coal dust is less than 8 wt%, and the ash content in the coke dust is less than 10 wt%.
Preferably, in the step (2), the medium-frequency induction converting furnace comprises a feeding device, a smoke dust collecting device, an induction coil, a heating body, a sliding water gap and a converting gun; the heating body is of a cylindrical structure with an opening at the upper end, and the induction coil is arranged on the outer wall of the heating body in a surrounding manner; the smoke dust collecting device is of an umbrella-shaped structure and is arranged above the heating body; the feeding device and the converting gun penetrate through the smoke dust collecting device to the inside of the heating body, and the sliding water gap is arranged at the bottom of the heating body; wherein the diameter of the smoke dust collecting device is larger than that of the heating body.
Preferably, the heating body is made of graphite.
Preferably, the specific operation of step (2) is: and (2) adding the mixture obtained in the step (1) into a heating body through a feeding device, starting an induction coil to heat so as to change industrial sodium sulfate into molten sodium sulfate, blowing mixed gas by using a blowing gun to carry out blowing reduction, reducing the molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out through a sliding water gap.
Preferably, the feeding device and the converting gun can move up and down, and the converting gun does not directly contact with the molten sodium sulfate.
Preferably, in the step (2), the medium-frequency induction heating temperature is 900-.
Preferably, in the step (2), the mixed gas is nitrogen and compressed air; wherein the volume ratio of the nitrogen to the compressed air is 1: 0.5-2.
Preferably, the upper end of the smoke dust collecting device is sequentially connected with a fan and an alkali liquor absorption tower through pipelines, and waste gas from the smoke dust collecting device is conveyed to the alkali liquor absorption tower through the fan for absorption treatment.
The method takes the industrial sodium sulfate with the content of more than 95 weight percent as a raw material, adds a reducing agent, takes a medium-frequency induction converting furnace as a reducing device, blows nitrogen and compressed air, adopts the full-fire method to melt and reduce the industrial sodium sulfate into sodium sulfide, and can absorb the generated waste gas with little pollution to the environment. The method is simple and environment-friendly, has small corrosion to equipment, and the prepared sodium sulfide has high purity, and the content is more than 90%.
Drawings
FIG. 1 is a process flow diagram according to the present invention;
FIG. 2 is a schematic cross-sectional view of a medium frequency induction converting furnace according to the present invention.
Description of the reference numerals
1 feeding device and 2 smoke dust collecting device
3 induction coil 4 heating body
5 slide gate 6 converting gun
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for preparing sodium sulfide by reducing industrial sodium sulfate in a molten state, which has a process flow diagram shown in figure 1 and comprises the following steps:
(1) mixing industrial sodium sulfate and a reducing agent, and then carrying out ball milling to obtain a mixture with the fineness of less than or equal to 200 meshes;
(2) adding the mixture obtained in the step (1) into a medium frequency induction converting furnace, heating to a molten state, blowing mixed gas for converting reduction, reducing molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out of the medium frequency induction converting furnace;
(3) and (3) pouring and molding the molten sodium sulfide poured out in the step (2).
Wherein, in the step (1), the mass ratio of the industrial sodium sulfate to the reducing agent is 1: 0.4-1.
In the method, industrial sodium sulfate is a byproduct of a sodium-treatment vanadium extraction process, the content of the main component sodium sulfate reaches over 95 weight percent, and the industrial sodium sulfate also contains impurities such as ammonium sulfate and the like.
According to the method, the industrial sodium sulfate is changed into a molten state by adopting a full fire method in the medium-frequency induction converting furnace, then the molten state sodium sulfate is changed into the molten state sodium sulfide by blowing reduction, the molten state viscosity of the sodium sulfate is different from that of the molten state of the sodium sulfide, and the reduction end point can be judged by observing the viscosity of the melt. The method is simple and environment-friendly to operate, and the obtained sodium sulfide is high in purity.
In the method of the present invention, in the step (1), the reducing agent is pulverized coal or coke powder. Preferably, the ash content in the coal dust is less than 8 wt%, and the ash content in the coke dust is less than 10 wt%. In a particular embodiment, the coal fines may be anthracite fines.
The method of the invention uses low ash content coal powder or coke powder as a reducing agent, adopts a converter-like steelmaking mode, changes industrial sodium sulfate into a molten state by adopting a total fire method in a medium-frequency induction converting furnace, realizes direct reduction of the molten state, forms a power stirring function by blowing nitrogen and compressed air, accelerates the reaction rate, leads carbon in the mixture to react with oxygen by the intervention of oxygen, generates heat, makes up the deficiency of medium-frequency induction heating, leads the carbon monoxide formed by the reaction to be more reduced by sodium sulfate, and has full thermodynamic and kinetic conditions.
In the method, in the step (1), the mass ratio of the industrial sodium sulfate to the reducing agent is 1: 0.4-1. In a specific embodiment, the mass ratio of the industrial sodium sulfate to the reducing agent may be 1: 0.4, 1: 0.5, 1: 0.6, 1: 0.7, 1: 0.8, 1: 0.9 or 1: 1.
in the method of the invention, in the step (1), the thickness of the mixed material is less than or equal to 200 meshes. Preferably, the thickness of the mixture is 200-250 meshes.
In the method of the invention, in the step (2), the schematic sectional structure of the medium frequency induction converting furnace is shown in fig. 2, and the medium frequency induction converting furnace comprises a feeding device 1, a smoke dust collecting device 2, an induction coil 3, a heating body 4, a sliding water gap 5 and a converting gun 6; the heating body 4 is of a cylindrical structure with an opening at the upper end, and the induction coil 3 is arranged on the outer wall of the heating body 4 in a surrounding manner; the smoke dust collecting device 2 is of an umbrella-shaped structure and is arranged above the heating body 4; the feeding device 1 and the converting gun 6 penetrate through the smoke dust collecting device 2 to the inside of the heating body 4, and the sliding water gap 5 is arranged at the bottom of the heating body 4.
In the method according to the invention, the diameter of the soot collecting device 2 is greater than the diameter of the heating body 4. Preferably, a gap is left between the bottom of the smoke collecting device 2 and the top of the heating body 4.
In the method of the present invention, the heating body 4 is made of graphite.
In the method, the induction coil 3 provides heat for melting and reduction of industrial sodium sulfate, the feeding device 1 is used for feeding the mixed material into the heating body 4, the heating body 4 can be heated through the induction coil 3 to heat the mixed material, the sliding water gap 5 is used for discharging reduced sodium sulfide, and the converting gun 6 is used for blowing the mixed gas into the molten sodium sulfate to perform converting reduction.
In the method of the present invention, the specific operation of step (2) is: adding the mixture obtained in the step (1) into a heating body 4 through a feeding device 1, starting an induction coil 3 to heat so as to change industrial sodium sulfate into molten sodium sulfate, blowing mixed gas by using a blowing gun 6 to carry out blowing reduction, reducing the molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out through a sliding water gap 5.
In the method of the present invention, the charging device 1 and the converting lance 6 can be moved up and down, and the converting lance 6 is not in direct contact with molten sodium sulfate.
In the method of the present invention, in the step (2), the temperature of the medium frequency induction heating is 900-. In specific embodiments, the temperature of the medium frequency induction heating may be 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃ or 1300 ℃.
In the method of the present invention, in the step (2), the mixed gas is nitrogen and compressed air; wherein the volume ratio of the nitrogen to the compressed air is 1: 0.5-2. In particular embodiments, the volume ratio of nitrogen to compressed air may be 1: 0.5, 1: 0.6, 1: 0.7, 1: 0.8, 1: 0.9, 1: 1. 1: 1.2, 1: 1.4, 1: 1.5, 1: 1.7, 1: 1.9 or 1: 2.
in the method, waste gas is generated in the blowing reduction process, so that the upper end of the smoke dust collecting device 2 is sequentially connected with a fan and an alkali liquor absorption tower through a pipeline, and the waste gas from the smoke dust collecting device 2 is conveyed to the alkali liquor absorption tower through the fan for absorption treatment.
In the method of the present invention, in step (3), the casting molding is performed on a sheet casting machine.
The method takes the industrial sodium sulfate with the content of more than 95 weight percent as a raw material, adds a reducing agent into the raw material, takes a medium-frequency induction converting furnace as reducing equipment, adopts the full-fire method to melt and reduce the industrial sodium sulfate into sodium sulfide, and can absorb the generated waste gas with little pollution to the environment. The method is simple and environment-friendly, has small corrosion to equipment, and the prepared sodium sulfide has high purity.
Compared with the traditional method, the method of the invention has the following advantages:
(1) the method is a full fire method process, does not need a water immersion process, and has less corrosion to equipment;
(2) the method is simple and feasible to operate, and can prepare high-purity sodium sulfide with the content of more than 90 weight percent;
(3) compared with a wet process, the method has small environmental influence, mainly generates absorbable waste gas, and does not generate waste water and waste residue.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
Examples 1 to 3
(1) Mixing industrial sodium sulfate (which is a byproduct of a sodium-treatment vanadium extraction process) with a reducing agent, and then carrying out ball milling to obtain a mixture with the fineness of less than or equal to 200 meshes;
(2) adding the mixture obtained in the step (1) into a medium frequency induction converting furnace, heating to a molten state, blowing mixed gas for converting reduction, reducing molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out of the medium frequency induction converting furnace;
(3) pouring and molding the molten sodium sulfide poured out in the step (2);
in the step (2), specifically, a schematic sectional structure diagram of the intermediate frequency induction converting furnace is shown in fig. 2, and the intermediate frequency induction converting furnace includes a feeding device 1, a smoke dust collecting device 2, an induction coil 3, a heating body 4, a sliding water gap 5 and a converting gun 6; the heating body 4 is of a cylindrical structure with an opening at the upper end, and the induction coil 3 is arranged on the outer wall of the heating body 4 in a surrounding manner; the smoke dust collecting device 2 is of an umbrella-shaped structure and is arranged above the heating body 4; the feeding device 1 and the converting gun 6 penetrate through the smoke dust collecting device 2 to the inside of the heating body 4, and the sliding water gap 5 is arranged at the bottom of the heating body 4; the diameter of the smoke dust collecting device 2 is larger than that of the heating body 4; the heating body 4 is made of graphite.
The specific operation steps of the medium-frequency induction converting furnace are as follows: adding the mixture obtained in the step (1) into a heating body 4 through a feeding device 1, starting an induction coil 3 to heat so as to change industrial sodium sulfate into molten sodium sulfate, blowing mixed gas by using a blowing gun 6 to carry out blowing reduction, reducing the molten sodium sulfate into molten sodium sulfide, pouring the molten sodium sulfide out through a sliding water gap 5, carrying out casting molding on a casting machine, collecting waste gas generated in the blowing reduction through a smoke dust collecting device 2, and conveying the waste gas to an alkali liquor absorption tower through a fan to carry out absorption treatment; wherein the feeding device 1 and the converting gun 6 can move up and down, and the converting gun 6 is not in direct contact with molten sodium sulfate.
Specific parameter settings of purity of industrial sodium sulfate, reducing agent, content of ash of the reducing agent, mass ratio of industrial sodium sulfate to the reducing agent, fineness of the mixed material, heating temperature, and volume ratio of nitrogen gas to compressed air in examples 1 to 3 are shown in table 1.
TABLE 1
Comparative example 1
Sodium sulfide was prepared according to the method of example 2, except that in step (1), the mass ratio of industrial sodium sulfate to coke powder was 1: 0.2.
comparative example 2
Sodium sulfide was prepared according to the method of example 2, except that in step (1), the mass ratio of industrial sodium sulfate to coke powder was 1: 2.2.
comparative example 3
Sodium sulfide was prepared according to the method of example 3, except that in step (2), the induction coil was started and heated to a temperature of 800 ℃.
Test example 1
The contents of sodium sulfide prepared according to the methods of examples 1 to 3 and comparative examples 1 to 3 were measured, and the results are shown in Table 1.
TABLE 1
It can be seen from the results in table 1 that sodium sulfide with higher purity can be successfully prepared by the method of the present invention.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for preparing sodium sulfide by melting and reducing industrial sodium sulfate is characterized by comprising the following steps:
(1) mixing industrial sodium sulfate and a reducing agent, and then carrying out ball milling to obtain a mixture with the fineness of less than or equal to 200 meshes;
(2) adding the mixture obtained in the step (1) into a medium frequency induction converting furnace, heating to a molten state, blowing mixed gas for converting reduction, reducing molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out of the medium frequency induction converting furnace;
(3) pouring and molding the molten sodium sulfide poured out in the step (2);
wherein, in the step (1), the mass ratio of the industrial sodium sulfate to the reducing agent is 1: 0.4-1.
2. The method according to claim 1, wherein in step (1), the industrial sodium sulfate is a byproduct of a sodium-modified vanadium extraction process;
preferably, the content of sodium sulfate in the industrial sodium sulfate is 95 wt% or more.
3. The method according to claim 1 or 2, wherein in step (1), the reducing agent is pulverized coal or coke powder; preferably, the ash content in the coal dust is less than 8 wt%, and the ash content in the coke dust is less than 10 wt%.
4. The method according to claim 1, characterized in that in step (2), the medium frequency induction converting furnace comprises a charging device (1), a smoke collecting device (2), an induction coil (3), a heating body (4), a sliding gate nozzle (5) and a converting gun (6);
the heating body (4) is of a cylindrical structure with an opening at the upper end, and the induction coil (3) is arranged on the outer wall of the heating body (4) in a surrounding manner;
the smoke dust collecting device (2) is of an umbrella-shaped structure and is arranged above the heating body (4);
the feeding device (1) and the converting gun (6) penetrate through the smoke dust collecting device (2) to the inside of the heating body (4), and the sliding water gap (5) is arranged at the bottom of the heating body (4);
wherein the diameter of the smoke dust collecting device (2) is larger than that of the heating body (4).
5. Method according to claim 4, characterized in that said heating body (4) is of graphite material.
6. The method according to claim 4, wherein the specific operation of step (2) is: adding the mixture obtained in the step (1) into a heating body (4) through a feeding device (1), starting an induction coil (3) to heat so as to change industrial sodium sulfate into molten sodium sulfate, blowing mixed gas by using a blowing gun (6) to carry out blowing reduction, reducing the molten sodium sulfate into molten sodium sulfide, and pouring the molten sodium sulfide out through a sliding water gap (5).
7. A method according to claim 4 or 6, characterized in that the feeding device (1) and the blow lance (6) are movable up and down and that the blow lance (6) is not in direct contact with the molten sodium sulphate.
8. The method as claimed in claim 1, wherein in step (2), the medium frequency induction heating temperature is 900-1300 ℃.
9. The method according to claim 1 or 6, wherein in the step (2), the mixed gas is nitrogen and compressed air;
wherein the volume ratio of the nitrogen to the compressed air is 1: 0.5-2.
10. The method according to claim 4, characterized in that the upper end of the smoke dust collecting device (2) is connected with a fan and a lye absorption tower in turn through pipelines, and the waste gas from the smoke dust collecting device (2) is conveyed to the lye absorption tower through the fan for absorption treatment.
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Cited By (4)
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| CN114132901A (en) * | 2021-11-17 | 2022-03-04 | 重庆长能环境科技有限公司 | Method for preparing sodium sulfide from SDS desulfurization slag and product thereof |
| CN115784168A (en) * | 2022-12-14 | 2023-03-14 | 攀钢集团攀枝花钢铁研究院有限公司 | Process and method for continuously preparing sodium sulfide by directly reducing sodium sulfate with fuel gas |
| CN116425121A (en) * | 2023-05-22 | 2023-07-14 | 南风化工(运城)集团有限公司 | Sodium sulfide production method |
| WO2024040703A1 (en) * | 2022-08-24 | 2024-02-29 | 湖南福尔程环保科技有限公司 | Resource utilization method for crude sodium sulfate |
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