System for purifying crude selenium by wet process

Abstract

The utility model discloses a system for purifying crude selenium by a wet method, and belongs to the technical field of crude selenium treatment equipment. The device comprises a size mixing tank, a leaching kettle, a plate-and-frame filter press, a leachate storage tank, a primary purification kettle, a primary purification filter tank, a secondary purification kettle, a secondary purification filter tank, a decomposition kettle, a decomposition filter tank, a wastewater storage tank and a sulfuric acid tank which are sequentially connected, the decomposition kettle is connected with a sulfuric acid tank, and the primary purification filter tank, the secondary purification filter tank and the decomposition filter tank are connected with a vacuum pump. The system for purifying the crude selenium by the wet method is simple in equipment configuration, suitable for purifying the crude selenium by the wet method, high in crude selenium purification treatment capacity and suitable for large-scale industrial production operation.

Description

Technical Field

[0001] The utility model belongs to the technical field of crude selenium processing equipment, and in particular relates to a system for wet-process purification of crude selenium. Background Art

[0002] The scattered element selenium is widely used in semiconductor, electronics, glass manufacturing, metallurgy, chemical industry, health care, bio-agriculture and other industries due to its good metallic properties. Refined selenium and high-purity selenium are mainly used to prepare new materials such as high-purity indium gallium selenide, zinc selenide, cadmium selenide, hydrogen selenide, and selenium compounds such as high-purity sodium selenite and sodium selenate. In recent years, with the rapid development of national strategic emerging materials and selenium-rich industries, the consumption of high-purity selenium has increased year by year, and the development trend and application prospects of high-purity selenium have become increasingly broad.

[0003] According to the crude selenium purification preparation method, the equipment for crude selenium purification mainly includes a vacuum distillation device and a regional smelting device. However, the above equipment has high requirements and small processing capacity and is not suitable for purification of crude selenium from large quantities of raw materials. Utility Model Content

[0004] In view of the above problems, the utility model provides a system for wet-process purification of crude selenium, which is suitable for wet-process purification of crude selenium, has simple equipment, large processing capacity and is suitable for mass production.

[0005] To achieve the above-mentioned purpose, the utility model provides a system for wet purification of crude selenium, comprising a slurry mixing tank 1, a leaching kettle 2, a plate and frame filter press 3, a leachate storage tank 4, a primary purification kettle 5, a primary purification filter tank 6, a secondary purification kettle 7, a secondary purification filter tank 8, a vacuum pump 9, a decomposition kettle 10, a decomposition filter tank 11, a wastewater storage tank 12 and a sulfuric acid tank 13;

[0006] The lower end outlet of the slurry mixing tank 1 is connected to the top inlet of the leaching kettle 2 through a delivery pump Ⅰ101 and a pipeline, the lower end outlet of the leaching kettle 2 is connected to the inlet of the plate and frame filter press 3 through a delivery pump Ⅱ201 and a pipeline, the outlet of the plate and frame filter press 3 is connected to the top inlet of the leachate storage tank 4 through a pipeline, the lower end outlet of the leachate storage tank 4 is connected to the top inlet of the primary purification kettle 5 through a delivery pump Ⅲ401 and a pipeline, the bottom outlet of the primary purification kettle 5 is located directly above the top inlet of the primary purification filter tank 6; the lower end outlet of the primary purification filter tank 6 is connected to the top inlet of the primary purification filter tank 6 through a delivery pump Ⅳ6 01, the pipeline is connected to the top inlet of the secondary purification kettle 7; the bottom outlet of the secondary purification kettle 7 is located just above the top inlet of the secondary purification filter tank 8; the lower outlet of the secondary purification filter tank 8 is connected to the top inlet of the decomposition kettle 10 through a delivery pump V801 and a pipeline; the bottom outlet of the decomposition kettle 10 is located just above the top inlet of the decomposition filter tank 11, and the top outlet is connected to the sulfuric acid tank 13 through a metering pump 1301 and a pipeline; the lower outlet of the decomposition filter tank 11 is connected to the top inlet of the wastewater storage tank 12 through a delivery pump VI1101 and a pipeline. As a further improvement of the present utility model, the system for wet purification of crude selenium also includes a vacuum pump 9, and the upper inlets of the primary purification filter tank 6, the secondary purification filter tank 8, and the decomposition filter tank 8 are connected to the vacuum pump 9 through a pipeline.

[0007] As a further improvement of the present invention, the lower end outlet of the wastewater storage tank 12 is discharged to the waste acid station through a delivery pump VII1201.

[0008] As a further improvement of the utility model, the slurry mixing tank 1, the leaching kettle 2, the leachate storage tank 4, the primary purification kettle 5, the secondary purification kettle 7, the decomposition kettle 10, the wastewater storage tank 12 and the sulfuric acid tank 13 are all provided with a radar level meter 14.

[0009] As a further improvement of the present invention, a hole filter plate with a pore size of 0.5 cm to 2 cm and a float type liquid level gauge are arranged inside the primary purification filter tank 6 and the secondary purification filter tank 8 .

[0010] As a further improvement of the present invention, the primary purification kettle 5, the secondary purification kettle 7 and the decomposition kettle 10 are all jacketed enamel reactors.

[0011] As a further improvement of the utility model, a discharge pipe is installed at the bottom outlet of the decomposition kettle 10, and a compression air duct is arranged on the side of the discharge pipe. The compression air duct is connected to the discharge pipe, and a valve is arranged on the compression air duct. The design of the compression air duct and the valve 1001 can prevent selenium from agglomerating and clogging the pipeline during the reaction process.

[0012] As a further improvement of the utility model, an atomizing nozzle 1002 is provided on the pipe connecting the decomposition kettle 10 and the sulfuric acid tank 13. The atomizing nozzle 1002 is located inside the decomposition kettle 10, so that sulfuric acid is sprayed into the decomposition kettle 10 in an atomized form, and the reaction is more uniform.

[0013] As a further improvement of the present invention, a tail gas outlet 1003 is provided at the top of the decomposition kettle 10 and connected to a tail gas treatment system.

[0014] As a further improvement of the present utility model, the delivery pump I101, delivery pump II201, delivery pump III401, delivery pump IV601, delivery pump V801, delivery pump VI1101, delivery pump VII1201 and metering pump 1301 can all be remotely controlled to be turned on and off.

[0015] The working principle of the system for wet purification of crude selenium:

[0016] Water is added to the slurry tank 1 and stirred, and crude selenium and leaching agent are added to the slurry tank 1 in turn. The slurried material is transported to the leaching kettle 2 for heating and leaching through the delivery pump I101. During the leaching process, the leaching agent converts the crude selenium into sodium selenosulfate solution, and then the leached slurry is transported to the plate and frame filter press 3 for filtration through the delivery pump II201. After filtration, the filter residue is bagged for treatment, and the filtrate enters the leaching liquid storage tank 4; the solution in the leaching liquid storage tank 4 is transported to the primary purification kettle 5 through the delivery pump III401, and the impurity arsenic in the leaching liquid is removed in the primary purification kettle. The solution after purification is filtered through the primary purification filter tank 6, and the filtered solution is pumped to the secondary purification kettle 7 through the delivery pump IV601, and lead is removed in the secondary purification kettle 7. The solution after secondary purification is filtered through the secondary purification filter tank 8, and the filtered solution is pumped to the decomposition kettle 10 through the delivery pump V801. The sulfuric acid tank 13 pumps sulfuric acid into the decomposition kettle 10, and the sulfuric acid reacts with the sodium selenosulfate solution to produce elemental selenium, thereby purifying selenium. After the reaction, the material is vacuum filtered through the decomposition filter tank 11, and the filtrate enters the wastewater storage tank 12. The filter residue is washed with water to obtain 99.9% refined selenium.

[0017] The beneficial effects of the utility model are embodied in that the system equipment for wet purification of crude selenium described in the utility model is simple in configuration, has a large processing capacity for purification of crude selenium, and is suitable for large-scale industrial production operations. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a schematic diagram of the structure of the system for wet purification of crude selenium described in the utility model.

[0019] Description of reference numerals:

[0020] 1-slurry mixing tank; 101-delivery pump I; 2-leaching kettle; 201-delivery pump II; 3-plate and frame filter press; 4-leachate storage tank; 401-delivery pump III; 5-primary purification kettle; 6-primary purification filter tank; 601-delivery pump IV; 7-secondary purification kettle; 8-secondary purification filter tank; 801-delivery pump V; 9-vacuum pump; 10-decomposition kettle; 1001-compressed air duct and valve; 1002-atomizing nozzle; 1003-exhaust pipeline; 11-decomposition filter tank; 1101-delivery pump VI; 12-waste liquid storage tank; 1201-delivery pump VII; 13-sulphuric acid tank; 1301-metering pump; 14-radar wave liquid level meter. DETAILED DESCRIPTION

[0021] In order to make the purpose, technical solution and advantages of the utility model clearer, the utility model is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the described embodiments are only part of the embodiments of the utility model, rather than all of the embodiments. In the absence of conflict, the embodiments in this application and the features in the embodiments can be combined with each other. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the utility model.

[0022] Example 1

[0023] like Figure 1 As shown, a system for wet purification of crude selenium includes a slurry mixing tank 1, a leaching kettle 2, a plate and frame filter press 3, a leaching liquid storage tank 4, a primary purification kettle 5, a primary purification filter tank 6, a secondary purification kettle 7, a secondary purification filter tank 8, a vacuum pump 9, a decomposition kettle 10, a decomposition filter tank 11, a wastewater storage tank 12 and a sulfuric acid tank 13.

[0024] The lower end outlet of the slurry mixing tank 1 is connected to the top inlet of the leaching kettle 2 through the delivery pump I101 and the pipeline in turn, the lower end outlet of the leaching kettle 2 is connected to the inlet of the plate and frame filter press 3 through the delivery pump II201 and the pipeline in turn, the outlet of the plate and frame filter press 3 is connected to the top inlet of the leachate storage tank 4 through the pipeline in turn, the lower end outlet of the leachate storage tank 4 is connected to the top inlet of the primary purification kettle 5 through the delivery pump III401 and the pipeline in turn, the bottom outlet of the primary purification kettle 5 is located directly above the top inlet of the primary purification filter tank 6; the lower end outlet of the primary purification filter tank 6 is connected to the top inlet of the secondary purification kettle 7 through the delivery pump IV601 and the pipeline; the bottom outlet of the secondary purification kettle 7 is located at the top of the secondary purification filter tank 8 The lower end outlet of the secondary purification filter tank 8 is connected to the top inlet of the decomposition kettle 10 through a delivery pump V801 and a pipeline; the bottom outlet of the decomposition kettle 10 is located directly above the top inlet of the decomposition filter tank 11, and the top inlet of the decomposition kettle 10 is connected to the sulfuric acid tank 13 through a metering pump 1301 and a pipeline; the lower end outlet of the decomposition filter tank 11 is connected to the top inlet of the wastewater storage tank 12 through a delivery pump VI1101 and a pipeline; the lower end outlet of the wastewater storage tank 12 is discharged to the dirty acid station through a delivery pump VII1201; the upper end inlets of the primary purification filter tank 6, the secondary purification filter tank 8, and the decomposition filter tank 8 are connected to the vacuum pump 9 through a pipeline, and the vacuum pump provides negative pressure to accelerate the filtration rate.

[0025] Radar level meters 14 are provided inside the slurry mixing tank 1, the leaching kettle 2, the leachate storage tank 4, the primary purification kettle 5, the secondary purification kettle 7, the decomposition kettle 10, the wastewater storage tank 12 and the sulfuric acid tank 13 for detecting the liquid level.

[0026] A perforated filter plate and a float type liquid level gauge are arranged inside the primary purification filter tank 6 and the secondary purification filter tank 8. The aperture size of the perforated filter plate can be selected according to actual needs. The aperture size of the perforated filter plate in this embodiment is 0.5 cm to 2 cm.

[0027] The bottom outlet of the decomposition kettle 10 is equipped with a discharge pipe, and a compressed air duct is arranged on the side of the discharge pipe. The compressed air duct is communicated with the discharge pipe, and a valve is arranged on the compressed air duct. The design of the compressed air duct and the valve 1001 can prevent the selenium agglomeration from blocking the pipeline during the reaction process. The sulfuric acid pipeline connected between the decomposition kettle 10 and the sulfuric acid tank 13 is provided with an atomizing nozzle 1002, and the atomizing nozzle 1002 is located inside the decomposition kettle 10, so that sulfuric acid is sprayed into the decomposition kettle 10 in an atomized form, and the reaction is more uniform. The top of the decomposition kettle 10 is provided with a tail gas outlet 1003, and the tail gas treatment system.

[0028] The primary purification kettle 5, the secondary purification kettle 7 and the decomposition kettle 10 are all jacketed enamel reactors.

[0029] The delivery pump I101, delivery pump II201, delivery pump III401, delivery pump IV601, delivery pump V801, delivery pump VI1101, delivery pump VII1201, and metering pump 1301 can all be remotely controlled to be turned on and off.

[0030] The principle of using the system for wet purification of crude selenium for conventional wet purification of crude selenium is:

[0031] Water is added to the slurry mixing tank 1 and stirred, and crude selenium and leaching agent (the leaching agent can be a commonly used agent in the art) are added to the slurry mixing tank 1 in turn. The slurried material is transported to the leaching kettle 2 for heating and leaching by the delivery pump I101. During the leaching process, the leaching agent converts the crude selenium into a sodium selenosulfate solution, and then the delivery pump II201 is used to transport the leached slurry to the plate and frame filter press 3 for filtration. After filtration, the filter residue is bagged for treatment, and the filtrate enters the leachate storage tank 4; the solution in the leachate storage tank 4 is delivered to the primary purification kettle 5 by the delivery pump III401. The primary purification kettle is provided with an arsenic removal agent (commonly used agents in the art, such as FeCl3, Na2S, etc.) to remove arsenic impurities in the leachate. The purified solution is passed through The primary purification filter tank 6 is filtered, and the filtered solution is pumped to the secondary purification kettle 7 through the delivery pump IV601. The secondary purification kettle 7 is provided with a lead removal agent and activated carbon (the lead removal agent can be a commonly used agent in this field, such as CaCl2, etc.) to remove lead. After the secondary purification, the solution is filtered through the secondary purification filter tank 8, and the filtered solution is pumped to the decomposition kettle 10 through the delivery pump V801. The sulfuric acid tank 13 pumps sulfuric acid into the decomposition kettle 10. The sulfuric acid reacts with the sodium selenosulfate solution to produce elemental selenium, thereby purifying the selenium. After the reaction, the material is vacuum filtered through the decomposition filter tank 11, and the filtrate enters the wastewater storage tank 12. The filter residue is washed with water to obtain 99.9% refined selenium, and the tail gas in the decomposition kettle 10 enters the tail gas treatment system through the tail gas outlet 1003.

[0032] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the utility model rather than to limit the protection scope of the utility model. Although the utility model is described in detail with reference to the preferred embodiments, ordinary technicians in this field should understand that the technical solution of the utility model can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the utility model.

Claims

1. A system for wet purification of crude selenium, characterized in that: It includes a slurry mixing tank, a leaching kettle, a plate and frame filter press, a leaching liquid storage tank, a primary purification kettle, a primary purification filter tank, a secondary purification kettle, a secondary purification filter tank, a decomposition kettle, a decomposition filter tank, a wastewater storage tank and a sulfuric acid tank; The lower outlet of the slurry mixing tank is connected to the top inlet of the leaching kettle through a delivery pump I and a pipeline, the lower outlet of the leaching kettle is connected to the inlet of the plate and frame filter press through a delivery pump II and a pipeline, the outlet of the plate and frame filter press is connected to the top inlet of the leachate storage tank through a pipeline, the lower outlet of the leachate storage tank is connected to the top inlet of the primary purification kettle through a delivery pump III and a pipeline, and the bottom outlet of the primary purification kettle is located directly above the top inlet of the primary purification filter tank; the lower outlet of the primary purification filter tank is connected to the top inlet of the secondary purification kettle through a delivery pump IV and a pipeline; the bottom outlet of the secondary purification kettle is located directly above the top inlet of the secondary purification filter tank; the lower outlet of the secondary purification filter tank is connected to the top inlet of the decomposition kettle through a delivery pump V and a pipeline; the bottom outlet of the decomposition kettle is located directly above the top inlet of the decomposition filter tank, and the top outlet is connected to the sulfuric acid tank through a metering pump and a pipeline; the lower outlet of the decomposition filter tank is connected to the top inlet of the wastewater storage tank through a delivery pump VI and a pipeline.

2. The system for wet purification of crude selenium according to claim 1, characterized in that: Radar level meters are arranged inside the slurry mixing tank, the leaching kettle, the leaching liquid storage tank, the primary purification kettle, the secondary purification kettle, the decomposition kettle, the sulfuric acid tank and the wastewater storage tank.

3. The system for wet purification of crude selenium according to claim 1, characterized in that: The primary purification filter tank and the secondary purification filter tank are provided with a hole filter plate and a float type liquid level gauge.

4. The system for wet purification of crude selenium according to claim 1, characterized in that: The primary purification kettle, secondary purification kettle and decomposition kettle are all jacketed enamel reactors.

5. The system for wet purification of crude selenium according to claim 1, characterized in that: The bottom outlet of the decomposition kettle is connected with a discharge pipe, and the side of the discharge pipe is connected with a compression air pipe, and a valve is arranged on the compression air pipe.

6. The system for wet purification of crude selenium according to claim 1, characterized in that: An atomizing nozzle is arranged on the pipeline connecting the decomposition kettle and the sulfuric acid tank, and the atomizing nozzle is located inside the decomposition kettle.

7. The system for wet purification of crude selenium according to claim 1, characterized in that: A tail gas outlet is arranged on the top of the decomposition kettle, and the tail gas outlet is connected to a tail gas treatment system.

8. The system for wet purification of crude selenium according to claim 1, characterized in that: The lower end outlet of the wastewater storage tank is discharged to the waste acid station through the delivery pump VII.

9. The system for wet purification of crude selenium according to claim 8, characterized in that: The delivery pump I, delivery pump II, delivery pump III, delivery pump IV, delivery pump V, delivery pump VI, delivery pump VII and metering pump can all be remotely controlled to be turned on and off.

10. The system for wet purification of crude selenium according to claim 1, characterized in that: It also includes a vacuum pump; the upper inlets of the primary purification filter tank, the secondary purification filter tank and the decomposition filter tank are connected to the vacuum pump through pipelines.

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