CN113502392A - Automatic solid-liquid separation device and method for wet smelting - Google Patents
Automatic solid-liquid separation device and method for wet smelting Download PDFInfo
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- CN113502392A CN113502392A CN202111052596.6A CN202111052596A CN113502392A CN 113502392 A CN113502392 A CN 113502392A CN 202111052596 A CN202111052596 A CN 202111052596A CN 113502392 A CN113502392 A CN 113502392A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
- G01N2001/1418—Depression, aspiration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses an automatic solid-liquid separation device and method for hydrometallurgy, wherein the device comprises a pre-pretreatment module, a primary sampling module and a secondary sampling module; the front preprocessing module comprises a front sample cup, and a front sample tube is arranged at the bottom of the front sample cup; a front sample sending pipe, a front liquid level sensor and a reagent adding unit are arranged in the front sample cup; the primary sampling module comprises a primary sample cup and a filtering unit, and the filtering unit is positioned in the primary sample cup; a primary sampling tube is arranged at the bottom of the primary sample cup, the other end of the primary sampling tube is communicated with the front sample feeding tube, a primary sample feeding tube is arranged in the primary sample cup, and one end of the primary sample feeding tube is positioned at the upper part of the primary sample cup; the secondary sampling module comprises a secondary sample cup, a secondary sampling tube and a waste liquid tube, one end of the secondary sampling tube is connected with the other end of the primary sample feeding tube, the other end of the secondary sampling tube is located in the secondary sample cup, and one end of the waste liquid tube is connected with the bottom of the secondary sample cup. The invention has the advantages of high automation degree, high separation efficiency and the like.
Description
Technical Field
The invention mainly relates to the technical field of wet smelting, in particular to an automatic solid-liquid separation device and method for wet smelting.
Background
The non-ferrous metal smelting industry in China is a typical process industry and has the characteristics of various types, complicated raw material sources, complex process, long process, harsh working condition and environment and the like, smelting production is a process of gradually enriching main metals and gradually removing impurity metals, and a zinc hydrometallurgy water sample generally has the characteristics of high temperature, easiness in crystallization, large solid content, corrosion before filter pressing and the like. The smelting liquid has the characteristics of complex ions, high salinity and easy crystallization, and the realization of rapid and high-precision online detection is an industrial problem. At present, sampling and solid-liquid separation in the production process of zinc hydrometallurgy generally adopt timing manual sampling, manual solid-liquid separation and manual assay, wherein inspection data is reported in about 2 hours, and then field operators adjust production process parameters according to manual assay results and experience, so that the concentration of impurity metal ions in metallurgical feed liquid output by each process is kept within a specified range.
For traditional manual sampling and solid-liquid separation, the following defects and drawbacks exist:
1. the manual sampling and the solid-liquid separation time are long, and the samples are easy to be confused.
2. Personnel demand is many, increases the human cost of enterprise.
3. The labor intensity is high, the workers are easy to fatigue and relax, and mistakes are easy to make.
4. The environment is poor, and potential safety hazards and occupational hazards exist.
In the process of realizing the patent application, the applicant of the patent finds that the blockage of a pipeline caused by crystallization and scaling is the biggest difficult problem in solid-liquid separation, automatic sampling and automatic detection and analysis. In the first step of analyzing the crystal components, the crystal slag components of the domestic main wet-process zinc smelting plant are systematically sampled and analyzed, and the X-ray diffraction results are shown in figure 1.
In FIG. 1, the curve A is the X-ray diffraction of the calcium-magnesium slag from the immersion chute of the A plant, hereinafter referred to as XRD analysis result. And (3) carrying out suction filtration on the zinc sulfate solution, naturally drying, and then directly carrying out XRD analysis on the obtained slag sample. As can be seen, the main component of the crystallization slag is basic zinc sulfate (ZnSO)4∙3(Zn(OH)2)∙5H2O) and calcium sulfate dihydrate (CaSO)4∙2H2O)。
In FIG. 1, the curve B is the XRD analysis result of the calcium-magnesium slag in the leaching process liquid chute of the B plant. The main component of the crystallization slag is basic zinc sulfate (ZnSO) obtained by analysis of a map4∙3(Zn(OH)2)∙5H2O) and calcium sulfate dihydrate (CaSO)4∙2H2O), the crystal slag has the same component as the crystal slag of the Tatzia smelting plant, but the content of the calcium sulfate dihydrate is higher than that of the A plant.
In FIG. 1, the C curve is the XRD analysis result of the zinc hydrometallurgy calcium crystal slag in the C plant. The main component of the crystallization slag is basic zinc sulfate (ZnSO)4∙3(Zn(OH)2)∙5H2O) and calcium sulfate dihydrate (CaSO)4∙2H2O) and containing minor amounts of other heavy metal impurities.
In FIG. 1, the curve D is the XRD analysis result of the site crystallized slag in the D plant. The analysis result shows that the main components of the crystallization slag are basic zinc sulfate and calcium sulfate dihydrate, which indicates that other insoluble matters such as calcium sulfate dihydrate and basic zinc sulfate are formed in the production process.
The analysis shows that the main component of the crystallized slag from the middle leaching solution to the new solution section of almost all zinc smelters is basic zinc sulfate (ZnSO)4∙3(Zn(OH)2)∙5H2O) and calcium sulfate dihydrate (CaSO)4∙2H2O)。
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the problems in the prior art, the invention provides the automatic solid-liquid separation device and method for hydrometallurgy, which have high automation degree.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
an automatic solid-liquid separation device for hydrometallurgy comprises a pre-pretreatment module, a primary sampling module and a secondary sampling module;
the pre-pretreatment module comprises a pre-sample cup, the bottom of the pre-sample cup is provided with a pre-sample pipe, and the pre-sample pipe is provided with a pre-sample pump; a front sample sending pipe, a front liquid level sensor and a reagent adding unit are arranged in the front sample cup;
the primary sampling module comprises a primary sample cup and a filtering unit, and the filtering unit is positioned in the primary sample cup and is used for dividing the primary sample cup into an upper part and a lower part; a primary sampling tube is arranged at the bottom of the primary sample cup, the other end of the primary sampling tube is communicated with the preposed sample feeding tube, a primary sampling pump is arranged on the primary sampling tube, a primary sample feeding tube and a primary liquid level sensor are arranged in the primary sample cup, one end of the primary sample feeding tube is positioned at the upper part of the primary sample cup, the primary sample feeding tube is provided with the primary sample feeding pump, and the primary liquid level sensor is positioned at the upper part of the primary sample cup;
the secondary sampling module includes secondary appearance cup, secondary sampling tube and waste liquid pipe, the one end of secondary sampling tube links to each other with the other end of once sending the appearance pipe, and the other end of secondary sampling tube is located secondary appearance cup, the one end of waste liquid pipe links to each other with the bottom of secondary appearance cup.
As a further improvement of the above technical solution:
the secondary sampling module still includes the cleaning unit, the cleaning unit includes scale removal pipe and pickling pipe, the one end of scale removal pipe and pickling pipe all links to each other with the bottom of secondary appearance cup.
And a secondary liquid level sensor is arranged in the secondary sample cup.
The primary sampling module further comprises a cleaning assembly, the cleaning assembly comprises an upper water inlet pipe and a lower water inlet pipe, and an upper water inlet valve is arranged on the upper water inlet pipe; and a lower water inlet valve and a pressure sensor are arranged on the lower water inlet pipe, and a high-pressure spraying flusher is arranged at the lower part of the lower water inlet pipe, close to the filtering unit, of the primary sample cup.
The filtering unit is a filtering belt.
The invention also discloses a separation method based on the automatic solid-liquid separation device for hydrometallurgy, which comprises the following steps:
s01, pre-sampling: a front sampling pump of the front preprocessing module rotates forwards, and a water sample enters a front sampling cup from a chute through a front sampling pipe; when the prepositive liquid level sensor detects a high-level signal, the prepositive sampling is finished;
s02, settling: a reagent adding unit adds a flocculating agent into the preposed sample cup for sedimentation, and the next step is carried out after the sedimentation is finished;
s03, filter pressing and sampling: the primary sampling pump of the primary sampling module rotates forwards, the sample liquid of the preposed sample cup enters the primary sample cup through the preposed sample conveying pipe and the primary sampling pipe of the primary sampling module and then enters the primary sample cup through the bottom of the primary sample cup, and the filtering unit filters the sample liquid; when the primary liquid level sensor detects a high-level signal, the filter-pressing sampling is finished, and the next step is carried out;
s04, sample sending: the primary sample feeding pump of the primary sampling module rotates positively, and the primary sample cup is subjected to filter pressing by the filter unit to obtain sample liquid at the upper part, and the sample liquid enters the secondary sample cup of the secondary sampling module through the primary sample feeding pipe and the secondary sampling pipe to be sampled.
As a further improvement of the above technical solution:
after step S04, a cleaning process is further included, specifically:
injecting cleaning water into a front sample cup of the front pretreatment module, reversely rotating a front sampling pump, and cleaning the front sample cup and a front sampling pipe by the cleaning water from top to bottom; injecting cleaning water into a primary sample cup of the primary sampling module, reversely rotating a primary sampling pump, and cleaning the primary sample cup, a primary sampling pipe and a preposed sample conveying pipe from top to bottom by the cleaning water;
injecting cleaning water into a primary sample cup of the primary sampling module, enabling a primary sample conveying pump to rotate forwards, and cleaning the primary sample conveying pipe and a secondary sampling pipe by the cleaning water; the cleaning water of the secondary sample cup is discharged through the waste liquid pipe;
a front sample pump of the front pretreatment module is reversed, and the front sample cup and the front sample tube are emptied; and injecting cleaning water into the lower part of the primary sample cup of the primary sampling module, reversely rotating the primary sampling pump, and cleaning the primary sample cup and the primary sampling tube from bottom to top by the cleaning water.
After the cleaning process, the method also comprises an acid washing process:
and adding pickling solution or descaling agent into the secondary sample cup, reversely rotating the primary sample feeding pump of the primary sampling module, enabling the pickling solution or descaling agent of the secondary sample cup to enter the primary sample cup through the secondary sampling tube and the primary sample feeding tube, beginning to soak the filtering unit and the pipeline, and entering a standby state after the pickling is finished.
Before step S01, a preprocessing process is further included, specifically:
when the secondary sampling module starts triggering: discharging residual liquid of the secondary sample cup through a waste liquid pipe;
a primary sample feeding pump of the primary sampling module rotates forwards, and residual liquid on the upper part of the filtering unit of the primary sample cup is discharged to a secondary sample cup of the secondary sampling module through a primary sample feeding pipe and a secondary sampling pipe of the secondary sampling module;
a primary sampling pump of the primary sampling module is reversed, and residual liquid at the lower part of the filtering unit in the primary sample cup is reversely discharged to a front sample cup of the front pretreatment module through a primary sampling pipe and a front sample conveying pipe of the front pretreatment module;
and (3) reversely rotating a front sampling pump of the front pretreatment module, reversely discharging residual liquid of the front sampling cup to a sampling chute through a front sampling pipe, and ending the reverse discharging process.
After the reverse drainage process is finished, the front liquid level sensor detects a low-level signal and then starts rinsing, and the method specifically comprises the following steps: a front sample pump of the front pretreatment module rotates forwards, a water sample enters a front sample cup from a chute through a front sample pipe, and after the rinsing is finished, the rinsing is started to discharge reversely; the specific process of rinsing and back discharging is as follows: the preposed sampling pump of the preposed preprocessing module is reversed, the water sample after being rinsed is reversely discharged to the chute from the preposed sampling cup through the preposed sampling pipe, and the preposed sampling is started after the rinsing and reverse discharging are finished.
Compared with the prior art, the invention has the advantages that:
the sample liquid sedimentation, filter pressing and sampling are realized through the mutual matching of the pre-pretreatment module, the primary sampling module and the secondary sampling module, the whole process is automatically completed, and the automation degree is high.
The invention cleans before sampling, and washes with water and acid after sampling, which can solve the problem of crystal blockage and prolong the reliable operation time of the device. The invention can also be suitable for corrosive working condition sites.
The invention can adapt to the liquid before filter pressing, can carry out sampling detection in the whole process, and enables the water sample to be detected after pretreatment to meet the requirement of GB/T1914-2017 on rapid filter paper of chemical analysis filter paper so as to have consistency with the water sample detected in a laboratory.
The invention produces a relatively small amount of waste liquid. For example, the water sample for solid-liquid separation of cobalt detection is 2-10 ml, the reagent is 2-5 ml, and the waste liquid generated in one time is not more than 25 ml. Such waste streams may enter a factory laboratory waste collection system. The invention can recycle the waste liquid, such as solid-liquid separation of cadmium detection, and mercury in the waste liquid is recycled by a special recycling device. The invention can classify and process waste liquid and cleaning liquid, wherein the waste liquid enters a factory laboratory waste liquid recovery system, the cleaning liquid enters a production system and returns from a sampling point without influencing the system balance.
Drawings
FIG. 1 is an X-ray diffraction result diagram of the components of the crystallized slag of the prior wet-process zinc smelter.
Fig. 2 is a schematic structural diagram of an embodiment of the apparatus of the present invention.
FIG. 3 is a schematic structural diagram of a pre-processing module according to an embodiment of the present invention.
Fig. 4 is a schematic structural diagram of a one-time sampling module according to an embodiment of the present invention.
Fig. 5 is a schematic structural diagram of a sub-sampling module according to an embodiment of the present invention.
FIG. 6 is a flow chart of a method of the present invention in an embodiment.
Illustration of the drawings: 1. a front sample cup; 2. a sampling tube is arranged in front; 3. a front sampling pump; 4. a pre-level sensor; 5. a pre-pump; 6. a front water inlet valve; 7. a front water inlet pipe; 8. a sample sending pipe is arranged in front; 9. a front external pipe; 10. a reagent freezer; 11. cleaning the water tank; 12. a preposed overflow port; 13. a chute; 14. a primary sample cup; 15. a primary sampling tube; 16. a primary sampling pump; 17. a filter belt; 18. clamping a hoop; 19. a primary liquid level sensor; 20. a primary sample conveying pipe; 21. a primary sample feeding pump; 22. a lower water inlet pipe; 23. a water inlet valve; 24. a pressure sensor; 25. a high pressure spray washer; 26. an upper water inlet pipe; 27. an upper water inlet valve; 28. a primary overflow port; 29. a secondary sample cup; 30. a secondary pump; 31. a pickling valve; 33. secondary external connection pipe; 34. a waste liquid pipe; 35. a descaling pipe; 36. pickling the tube; 37. a secondary liquid level sensor; 38. a secondary sampling tube; 39. a way of instrument sampling tube; 40. b path of instrument sampling tube; 41. a spare instrument sampling tube; 42. and a secondary overflow port.
Detailed Description
The invention is further described below with reference to the figures and the specific embodiments of the description.
As shown in fig. 2, the automatic solid-liquid separation device for hydrometallurgy of the embodiment comprises a pre-pretreatment module, a primary sampling module and a secondary sampling module;
the pre-pretreatment module comprises a pre-sample cup 1, a pre-sample tube 2 is arranged at the bottom of the pre-sample cup 1, and a pre-sample pump 3 is arranged on the pre-sample tube 2; a front sample sending pipe 8, a front liquid level sensor 4 and a reagent adding unit are arranged in the front sample cup 1;
the primary sampling module comprises a primary sample cup 14 and a filtering unit, wherein the filtering unit is positioned inside the primary sample cup 14 and is used for dividing the primary sample cup 14 into an upper part and a lower part; a primary sampling tube 15 is arranged at the bottom of the primary sample cup 14, the other end of the primary sampling tube 15 is communicated with the front sample feeding tube 8, a primary sampling pump 16 is arranged on the primary sampling tube 15, a primary sample feeding tube 20 and a primary liquid level sensor 19 are arranged in the primary sample cup 14, one end of the primary sample feeding tube 20 is positioned at the upper part of the primary sample cup 14, a primary sample feeding pump 21 is arranged on the primary sample feeding tube 20, and the primary liquid level sensor 19 is positioned at the upper part of the primary sample cup 14;
the secondary sampling module comprises a secondary sample cup 29, a secondary sampling tube 38 and a waste liquid tube 34, wherein one end of the secondary sampling tube 38 is connected with the other end of the primary sample feeding tube 20, the other end of the secondary sampling tube 38 is positioned in the secondary sample cup 29, and one end of the waste liquid tube 34 is connected with the bottom of the secondary sample cup 29.
In an embodiment, as shown in fig. 3, a front water inlet pipe 7 is further disposed on the top of the front sample cup 1 for injecting cleaning water into the front sample cup 1, a front water inlet valve 6 is disposed on the front water inlet pipe 7, one end of the front water inlet pipe 7 is disposed in the chute 13, and the other end is disposed in the front sample cup 1.
In one embodiment, as shown in FIG. 3, the reagent unit of the pre-treatment module comprises a pre-extension pipe 9, and the pre-pump 5 is disposed on the pre-extension pipe 9 and connected to the reagent refrigerator 10 or the wash water tank 11. In addition, a front overflow port 12 is provided at the upper part of the front sample cup 1.
In a specific embodiment, as shown in fig. 4, the primary sampling module further includes a cleaning assembly, the cleaning assembly includes an upper water inlet pipe 26 and a lower water inlet pipe 22, the upper water inlet pipe 26 is provided with an upper water inlet valve 27; the lower water inlet pipe 22 is provided with a lower water inlet valve 23 and a pressure sensor 24, and the lower water inlet pipe 22 is provided with a high-pressure spray flusher 25 at the lower part of the primary sample cup 14 close to the filtering unit. Wherein the filtering unit is a filtering belt 17 which is fixed in the primary sample cup 14 through a fast-assembling clamp 18. The upper part of the other primary sample cup 14 is provided with a primary overflow port 28.
In one embodiment, as shown in fig. 5, a secondary liquid level sensor 37, a path a instrument sampling tube 39, a path B instrument sampling tube 40 and a spare instrument sampling tube 41 are arranged in the secondary sample cup 29; the bottom of the secondary sample cup 29 is provided with a secondary external pipe 33, the secondary external pipe 33 is provided with a secondary pump 30, the secondary pump 30 is connected with a cleaning unit, and specifically comprises a descaling pipe 35 and an acid washing pipe 36, one end of the descaling pipe 35 and one end of the acid washing pipe 36 are both connected with the bottom of the secondary sample cup 29 through the secondary pump 30, wherein the descaling pipe 35 and the acid washing pipe 36 are provided with acid washing valves 31 (pinch valves, two pipelines are sleeved inside); the pickling pipe 36 and the waste liquid pipe 34 are provided with a descaling valve 32 (a pinch valve, two pipelines are sleeved inside); the upper part of the secondary sample cup 29 is provided with a secondary overflow port 42.
In a specific embodiment, the front water inlet valve 6, the lower water inlet valve 23, the upper water inlet valve 27, the pickling valve 31 and the descaling valve 32 all adopt non-contact type pinch valves; the preposed sampling pump 3, the preposed pump 5, the primary sample feeding pump 21 and the secondary pump 30 all adopt non-contact peristaltic pumps, and the primary sampling pump 16 adopts a non-contact peristaltic variable frequency pump.
In one embodiment, the pre-treatment module and the primary sampling module are installed in the vicinity of the chute position during installation, and the installation principle is that the installation of equipment is convenient and the sampling pipeline is preferably less than 5 meters. The secondary sampling module is positioned in an independent equipment room of a hydrometallurgy factory, usually, a detection instrument is positioned in the equipment room, and a sample conveying pipeline from the secondary sampling module to the detection instrument is required to be arranged to be shortened as much as possible. In addition, the execution time of each step in the solid-liquid separation process can be set on an upper computer.
As shown in FIG. 6, the invention also discloses a separation method based on the automatic hydrometallurgy solid-liquid separation device, which comprises the following steps:
s01, pre-sampling: a front sampling pump 3 of the front preprocessing module rotates forwards, and a water sample enters a front sample cup 1 from a chute 13 through a front sample pipe 2; when the prepositive liquid level sensor 4 detects a high-level signal, the prepositive sampling is finished;
s02, settling: a reagent adding unit adds a flocculating agent into the preposed sample cup 1 for sedimentation, and the next step is carried out after the sedimentation is finished;
s03, filter pressing and sampling: a primary sampling pump 16 of the primary sampling module rotates forwards, sample liquid of the front sample cup 1 passes through the front sample sending pipe 8 and the primary sampling pipe 15 of the primary sampling module and then enters the primary sample cup 14 through the bottom of the primary sample cup 14, and the filtering unit filters the sample liquid; when the primary liquid level sensor 19 detects a high-level signal, the filter-pressing sampling is finished, and the next step is carried out;
s04, sample sending: the primary sample feeding pump 21 of the primary sampling module rotates forwards, the primary sample cup 14 is subjected to filter pressing by the filter unit to obtain sample liquid at the upper part, and the sample liquid enters the secondary sample cup 29 of the secondary sampling module through the primary sample feeding pipe 20 and the secondary sampling pipe 38 for sampling.
In an embodiment, after step S04, a cleaning process is further included, specifically:
injecting cleaning water into a front sample cup 1 of the front pretreatment module, reversely rotating a front sampling pump 3, and cleaning the front sample cup 1 and a front sampling pipe 2 by the cleaning water from top to bottom; injecting cleaning water into a primary sample cup 14 of the primary sampling module, reversely rotating a primary sampling pump 16, and cleaning the primary sample cup 14, a primary sampling pipe 15 and a preposed sample conveying pipe 8 from top to bottom by the cleaning water;
injecting cleaning water into a primary sample cup 14 of the primary sampling module, rotating a primary sample conveying pump 21 forwards, and cleaning the primary sample conveying pipe 20 and a secondary sampling pipe 38 by the cleaning water; the washing water of the secondary sample cup 29 is discharged through the waste liquid pipe 34;
a front sampling pump 3 of the front pretreatment module is reversed, and the front sampling cup 1 and the front sampling tube 2 are emptied; the lower part of a primary sample cup 14 of a primary sampling module is injected with cleaning water, a primary sampling pump 16 is reversed, the cleaning water cleans the primary sample cup 14 and a primary sampling tube 15 from bottom to top, and after the cleaning process, the acid cleaning process is carried out:
adding pickling solution or descaling agent into the secondary sample cup 29, reversely rotating the primary sample feeding pump 21 of the primary sampling module, enabling the pickling solution or descaling agent of the secondary sample cup 29 to enter the primary sample cup 14 through the secondary sampling pipe 38 and the primary sample feeding pipe 20, beginning to soak the filtering unit and the pipeline, and entering a standby state after pickling is finished.
In an embodiment, before step S01, a preprocessing process is further included, specifically:
when the secondary sampling module starts triggering: discharging the residual liquid in the secondary sample cup 29 through a waste liquid pipe 34;
the primary sample feeding pump 21 of the primary sampling module rotates positively, and residual liquid on the upper part of the filtering unit of the primary sample cup 14 is discharged to the secondary sample cup 29 of the secondary sampling module through the primary sample feeding pipe 20 and the secondary sampling pipe 38 of the secondary sampling module;
a primary sampling pump 16 of the primary sampling module reverses, and residual liquid at the lower part of the filtering unit in the primary sample cup 14 is reversely discharged to a front sample cup 1 of the front pretreatment module through a primary sampling pipe 15 and a front sample feeding pipe 8 of the front pretreatment module;
leading pretreatment module's leading sampling pump 3 reversal, through leading sampling pipe 2 back drainage to sample chute 13 with the residual liquid of leading appearance cup 1, after the back drainage flow, then start the rinse when leading level sensor 4 detects low level signal, specifically is: a front sampling pump 3 of the front preprocessing module rotates forwards, a water sample enters a front sample cup 1 from a chute 13 through a front sample pipe 2, and after the rinsing is finished, the rinsing is started to discharge reversely; the specific process of rinsing and back discharging is as follows: the preposed sampling pump 3 of the preposed preprocessing module is reversed, the moistened water sample is reversely discharged to the chute 13 from the preposed sampling cup 1 through the preposed sampling pipe 2, and the preposed sampling is started after the moistening and reverse discharging are finished.
The sample liquid sedimentation, filter pressing and sampling are realized through the mutual matching of the pre-pretreatment module, the primary sampling module and the secondary sampling module, the whole process is automatically completed, and the automation degree is high.
The invention cleans before sampling, and washes with water and acid after sampling, which can solve the problem of crystal blockage and prolong the reliable operation time of the device. The invention can also be suitable for corrosive working condition sites.
The invention can adapt to the liquid before filter pressing, can carry out sampling detection in the whole process, and enables the water sample to be detected after pretreatment to meet the requirement of GB/T1914-2017 on rapid filter paper of chemical analysis filter paper so as to have consistency with the water sample detected in a laboratory.
The invention produces a relatively small amount of waste liquid. For example, the water sample for solid-liquid separation of cobalt detection is 2-10 ml, the reagent is 2-5 ml, and the waste liquid generated in one time is not more than 25 ml. Such waste streams may enter a factory laboratory waste collection system. The invention can recycle the waste liquid, such as solid-liquid separation of cadmium detection, and mercury in the waste liquid is recycled by a special recycling device. The invention can classify and process waste liquid and cleaning liquid, wherein the waste liquid enters a factory laboratory waste liquid recovery system, the cleaning liquid enters a production system and returns from a sampling point without influencing the system balance.
The process of the invention is described in further detail below with reference to a specific example:
1. waiting for starting: the secondary sampling module is periodically and circularly started and triggers the pre-preprocessing module and the primary sampling module to be started;
2. starting reverse drainage: when the secondary sampling module starts triggering: the descaling valve 32 of the secondary sampling module is opened, the secondary pump 30 is reversed, and the residual liquid in the secondary sample cup 29 is discharged from the waste liquid pipe 34;
the primary sample feeding pump 21 of the primary sampling module rotates positively, and residual liquid on the upper part of the filter belt 17 of the primary sample cup 14 is discharged to the secondary sample cup 29 of the secondary sampling module through the primary sample feeding pipe 20 and the secondary sampling pipe 38 of the secondary sampling module;
a primary sampling pump 16 of the primary sampling module reversely rotates to reversely discharge residual liquid at the lower part of a filter belt 17 in a primary sample cup 14 to a front sample cup 1 of the front pretreatment module through a primary sampling pipe 15 and a front sample sending pipe 8 of the front pretreatment module;
a preposed sampling pump 3 of the preposed pretreatment module reversely rotates, residual liquid of a preposed sample cup 1 is reversely discharged to a sampling chute 13 through a preposed sampling pipe 2, and when the reverse discharge process is finished, a preposed liquid level sensor 4 starts rinsing when detecting a low-level signal;
3. rinsing: a front sampling pump 3 of the front preprocessing module rotates forwards, a water sample enters a front sample cup 1 from a chute 13 through a front sample pipe 2, and after the rinsing is finished, the rinsing is started to discharge reversely;
4. rinsing and back discharging: the actions of the rinsing and back-discharging process and the rinsing process are opposite, a preposed sampling pump 3 of the preposed pretreatment module is reversed, a rinsed water sample is back-discharged from the preposed sample cup 1 to the chute 13 through the preposed sample pipe 2, and the preposed sampling is started after the rinsing and back-discharging process is finished;
5. pre-sampling: a front sampling pump 3 of the front preprocessing module rotates forwards, and a water sample enters a front sample cup 1 from a chute 13 through a front sample pipe 2; when the prepositive liquid level sensor 4 detects a high-level signal, the prepositive sampling is finished, and the sedimentation is started;
6. and (3) settling: the prepositive pump 5 of the prepositive pretreatment module is reversed, and the flocculating agent enters the prepositive sample cup 1 from the reagent refrigerator 10; wherein, the flocculating agent is added according to the sedimentation efficiency of the on-site water sample; starting filter pressing sampling after the sedimentation is finished;
7. filter pressing and sampling: a primary sampling pump 16 of the primary sampling module rotates forwards, supernatant of the front sample cup 1 enters a primary sample cup 14 from a front sample sending pipe 8 and a primary sampling pipe 15 of the primary sampling module, and when a primary liquid level sensor 19 detects a high-level signal, filter-pressing sampling is finished, and sample sending is started; otherwise, the pre-preprocessing module jumps to the 9 th step of reverse discharging original sample, and informs the secondary sampling module to jump to the last step of standby;
during the filter-pressing sampling process, a PID control method or a sectional control method is adopted for pressure monitoring alarm, when the pressure sensor 24 detects that the pressure is higher than the standard pressure (the pressure of the primary sample cup 14 during normal filter-pressing sampling), the primary sampling pump 16 operates at a reduced speed, and when the pressure sensor 24 detects that the pressure is higher than the alarm pressure (the pressure of the primary sample cup 14 is increased by the blockage of the filter belt 17), the alarm is stopped.
8. Sample feeding and rinsing:
sample feeding: a primary sample feeding pump 21 of the primary sampling module rotates positively, and the primary sample cup 14 is subjected to filter pressing by a filter belt 17 to obtain supernatant on the upper part, and the supernatant enters a secondary sample cup 29 of the secondary sampling module from a primary sample feeding pipe 20 and a secondary sampling pipe 38;
rinsing: the secondary pump 30 of the secondary sampling module is reversed, the descaling valve 32 is opened, and the sampled water in the secondary sample cup 29 is discharged from the waste pipe 34. When the secondary liquid level sensor 37 detects a high-level signal, the sample feeding and the reverse discharging rinsing are finished, the sampling of the instrument is waited, and the reverse discharging original sample is started after the sampling of the instrument is finished;
9. reversely discharging the original sample, reversely rotating a front sampling pump 3 of the front preprocessing module, reversely rotating a primary sampling pump 16 of the primary sampling module and reversely rotating a primary sample feeding pump 21, and reversely discharging the water samples of a secondary sample cup 29 of the secondary sampling module, a primary sample cup 14 of the primary sampling module and a front sample cup 1 of the front preprocessing module to a chute 13;
10. cleaning, the cleaning process is divided into four processes:
the first time of cleaning the sample cup is from top to bottom: a front water inlet valve 6 of the front pretreatment module is opened, a front sampling pump 3 is reversed, and tap water cleans a front sampling cup 1 and a front sampling pipe 2 from top to bottom; the upper water inlet valve 27 of the primary sampling module is opened, the primary sampling pump 16 is reversed, and tap water cleans the primary sample cup 14, the primary sampling tube 15 and the preposed sample conveying tube 8 from top to bottom;
the upper water inlet valve 27 of the primary sampling module is opened, the primary sample feeding pump 21 rotates forwards, and tap water is used for cleaning the primary sample feeding pipe 20 and the secondary sampling pipe 38; the secondary pump 30 is reversed, the descaling valve 32 is opened, and the cleaning water of the secondary sample cup 29 is discharged from the waste liquid pipe 34;
cleaning the sample cup for the second time from bottom to top: a front sampling pump 3 of the front pretreatment module is reversed, and the front sampling cup 1 and the front sampling tube 2 are emptied; a lower water inlet valve 23 of the primary sampling module is opened, the primary sampling pump 16 is reversed, and tap water cleans the primary sample cup 14 and the primary sampling tube 15 from bottom to top;
the third time of cleaning the sample cup is consistent with the first time of cleaning the sample cup from top to bottom;
11. acid washing: the secondary pump 30 of the secondary sampling module rotates positively, and the pickling solution or the descaling agent enters the secondary sample cup 29 from the pickling pipe 36 or the descaling pipe 35 through the secondary external connecting pipe 33; the primary sample feeding pump 21 of the primary sampling module is reversed, the pickling solution of the secondary sample cup 29 enters the primary sample cup 14 from the secondary sampling pipe 38 and the primary sample feeding pipe 20, the secondary pump 30 stops after the filter belt 17 is immersed, the filter belt 17 and the pipeline begin to be soaked, and the pickling solution enters a standby state after the pickling is finished;
12. standby: and waiting for the periodic cycle starting of the secondary sampling module and triggering to enter the waiting starting.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (10)
1. An automatic solid-liquid separation device for hydrometallurgy is characterized by comprising a pre-pretreatment module, a primary sampling module and a secondary sampling module;
the pre-pretreatment module comprises a pre-sample cup (1), a pre-sample tube (2) is arranged at the bottom of the pre-sample cup (1), and a pre-sample pump (3) is arranged on the pre-sample tube (2); a front sample sending pipe (8), a front liquid level sensor (4) and a reagent adding unit are arranged in the front sample cup (1);
the primary sampling module comprises a primary sample cup (14) and a filtering unit, and the filtering unit is positioned in the primary sample cup (14) and is used for dividing the primary sample cup (14) into an upper part and a lower part; a primary sampling tube (15) is arranged at the bottom of the primary sample cup (14), the other end of the primary sampling tube (15) is communicated with the front sample delivery tube (8), a primary sampling pump (16) is arranged on the primary sampling tube (15), a primary sample delivery tube (20) and a primary liquid level sensor (19) are arranged in the primary sample cup (14), one end of the primary sample delivery tube (20) is positioned at the upper part of the primary sample cup (14), a primary sample delivery pump (21) is arranged on the primary sample delivery tube (20), and the primary liquid level sensor (19) is positioned at the upper part of the primary sample cup (14);
the secondary sampling module includes secondary appearance cup (29), secondary sampling tube (38) and waste liquid pipe (34), the one end of secondary sampling tube (38) links to each other with the other end of once sending appearance pipe (20), and the other end of secondary sampling tube (38) is located secondary appearance cup (29), the one end of waste liquid pipe (34) links to each other with the bottom of secondary appearance cup (29).
2. The automatic hydrometallurgical solid-liquid separation device of claim 1, wherein the secondary sampling module further comprises a cleaning unit, the cleaning unit comprises a descaling pipe (35) and an acid washing pipe (36), and one end of each of the descaling pipe (35) and the acid washing pipe (36) is connected with the bottom of the secondary sample cup (29).
3. The automatic solid-liquid separation device for hydrometallurgy according to claim 1, wherein a secondary liquid level sensor (37) is arranged in the secondary sample cup (29).
4. The automatic hydrometallurgical solid-liquid separation device according to any one of claims 1 to 3, wherein the primary sampling module further comprises a cleaning assembly, the cleaning assembly comprises an upper water inlet pipe (26) and a lower water inlet pipe (22), and an upper water inlet valve (27) is arranged on the upper water inlet pipe (26); and a lower water inlet valve (23) and a pressure sensor (24) are arranged on the lower water inlet pipe (22), and a high-pressure spray flusher (25) is arranged at the lower part of the lower water inlet pipe (22) close to the filtering unit.
5. The automatic hydrometallurgical solid-liquid separation device according to any one of claims 1 to 3, wherein the filtration unit is a filter belt (17).
6. The separation method of the automatic hydrometallurgical solid-liquid separation device based on any one of claims 1 to 5, is characterized by comprising the following steps:
s01, pre-sampling: a front sampling pump (3) of the front pretreatment module rotates forwards, and a water sample enters a front sample cup (1) from a chute (13) through a front sample tube (2); when the prepositive liquid level sensor (4) detects a high-level signal, the prepositive sampling is finished;
s02, settling: a reagent adding unit adds a flocculating agent into the preposed sample cup (1) for sedimentation, and the next step is carried out after the sedimentation is finished;
s03, filter pressing and sampling: a primary sampling pump (16) of the primary sampling module rotates forwards, sample liquid of the front sample cup (1) enters the primary sample cup (14) through the front sample conveying pipe (8) and the primary sampling pipe (15) of the primary sampling module and then through the bottom of the primary sample cup (14), and the filtering unit filters the sample liquid; when the primary liquid level sensor (19) detects a high-level signal, the filter-pressing sampling is finished, and the next step is carried out;
s04, sample sending: a primary sample feeding pump (21) of the primary sampling module rotates positively, a primary sample cup (14) is subjected to filter pressing by a filter unit to obtain sample liquid at the upper part, and the sample liquid enters a secondary sample cup (29) of the secondary sampling module through a primary sample feeding pipe (20) and a secondary sampling pipe (38) to be sampled.
7. The separation method according to claim 6, further comprising a cleaning process after step S04, specifically:
injecting cleaning water into a front sample cup (1) of the front pretreatment module, reversely rotating a front sampling pump (3), and cleaning the front sample cup (1) and a front sampling pipe (2) by the cleaning water from top to bottom; injecting cleaning water into a primary sample cup (14) of the primary sampling module, reversely rotating a primary sampling pump (16), and cleaning the primary sample cup (14), a primary sampling pipe (15) and a preposed sample conveying pipe (8) from top to bottom by the cleaning water;
injecting cleaning water into a primary sample cup (14) of the primary sampling module, enabling a primary sample conveying pump (21) to rotate forwards, and cleaning the primary sample conveying pipe (20) and a secondary sampling pipe (38) by the cleaning water; the cleaning water of the secondary sample cup (29) is discharged through a waste liquid pipe (34);
a front sampling pump (3) of the front pretreatment module is reversed, and a front sampling cup (1) and a front sampling pipe (2) are emptied; and (3) injecting cleaning water into the lower part of the primary sample cup (14) of the primary sampling module, reversing the primary sampling pump (16), and cleaning the primary sample cup (14) and the primary sampling tube (15) by the cleaning water from bottom to top.
8. The separation method according to claim 7, further comprising an acid washing process after the washing process:
and adding pickling solution or descaling agent into the secondary sample cup (29), reversely rotating the primary sample feeding pump (21) of the primary sampling module, enabling the pickling solution or descaling agent of the secondary sample cup (29) to enter the primary sample cup (14) through the secondary sampling pipe (38) and the primary sample feeding pipe (20), beginning to soak the filtering unit and the pipeline, and entering a standby state after pickling is finished.
9. The separation method according to claims 6 to 8, further comprising a pretreatment process before step S01, specifically:
when the secondary sampling module starts triggering: discharging the residual liquid of the secondary sample cup (29) through a waste liquid pipe (34);
a primary sample feeding pump (21) of the primary sampling module rotates forwards, and residual liquid on the upper part of the filtering unit of the primary sample cup (14) is discharged to a secondary sample cup (29) of the secondary sampling module through a primary sample feeding pipe (20) and a secondary sampling pipe (38) of the secondary sampling module;
a primary sampling pump (16) of the primary sampling module is reversed, and residual liquid at the lower part of the filtering unit in the primary sample cup (14) is reversely discharged to a front sample cup (1) of the front pretreatment module through a primary sampling pipe (15) and a front sample delivery pipe (8) of the front pretreatment module;
and (3) reversely rotating a front sampling pump (3) of the front pretreatment module, reversely discharging the residual liquid of the front sampling cup (1) to a sampling chute (13) through a front sampling pipe (2), and ending the reverse discharge process.
10. The separation method according to claim 9, characterized in that after the reverse drainage process is finished, rinsing is started when the front liquid level sensor (4) detects a low signal, specifically: a front sampling pump (3) of the front pretreatment module rotates forwards, a water sample enters a front sample cup (1) from a chute (13) through a front sampling pipe (2), and after rinsing is finished, rinsing is started to discharge reversely; the specific process of rinsing and back discharging is as follows: the preposed sampling pump (3) of the preposed preprocessing module is reversed, the moistened water sample is reversely discharged to the chute (13) from the preposed sampling cup (1) through the preposed sampling pipe (2), and the preposed sampling is started after the moistening and reverse discharging are finished.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102010086A (en) * | 2010-12-01 | 2011-04-13 | 新疆天业（集团）有限公司 | Method for treating mercury-containing wastewater with three-section continuous process |
| CN105688481A (en) * | 2016-03-09 | 2016-06-22 | 李亚娟 | Solid-liquid separation device with intelligent cleaning function |
| CN211170226U (en) * | 2019-12-10 | 2020-08-04 | 苏州业华环境科技有限公司 | Nickel-containing wastewater treatment system |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010086A (en) * | 2010-12-01 | 2011-04-13 | 新疆天业（集团）有限公司 | Method for treating mercury-containing wastewater with three-section continuous process |
| CN105688481A (en) * | 2016-03-09 | 2016-06-22 | 李亚娟 | Solid-liquid separation device with intelligent cleaning function |
| CN211170226U (en) * | 2019-12-10 | 2020-08-04 | 苏州业华环境科技有限公司 | Nickel-containing wastewater treatment system |
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