Tungsten bulk concentrate acid leaching experiment method

Abstract

The invention discloses a tungsten bulk concentrate acid leaching experiment method, and relates to the technical field of acid leaching equipment. Raw materials are prepared, the raw materials comprise a first mineral aggregate, a second mineral aggregate and a mixture, and the mixture is prepared from the first mineral aggregate and the second mineral aggregate according to the mass ratio of 1: 1; the mineral aggregate I comprises the following components in percentage by mass: more than or equal to 31.0% of WO3, more than or equal to 15.2% of CaCO3 and more than or equal to 12.1% of total calcium; the mineral aggregate II comprises the following components in percentage by mass: greater than or equal to 24.0% of WO3, greater than or equal to 20.0% of CaCO3 and greater than or equal to 18.2% of total calcium; preparing ore pulp: respectively adding bottom water into the mineral aggregate I, the mineral aggregate II and the mixture, and stirring to prepare the ore pulp with the concentration of 50%; introducing the ore pulp into a reaction kettle, and recording the adding volume of the diluted hydrochloric acid solution; stopping adding when the diluted hydrochloric acid solution and the ore pulp do not generate bubbles; pumping out the mixed solution to obtain mineral aggregate filter residues, and adding 75ml of clear water to wash the mineral aggregate filter residues; stirring for 3-5 minutes, standing and filtering to obtain primary filtrate; adding 500ml of clear water into the mineral aggregate filter residues washed in the step 6, washing, stirring for 3-5 minutes, standing and filtering to obtain secondary filtrate and filter residues. The technical problem that the reaction in the existing reaction kettle is difficult to observe or continuously observe is solved.

Description

Technical Field

[0001] The invention relates to the technical field of acid leaching equipment, in particular to an acid leaching experimental method for tungsten mixed concentrate. Background Art

[0002] For acid leaching test of concentrate, it is necessary to remove calcium carbonate in the concentrate by hydrochloric acid solution to improve the tungsten grade of the concentrate. At present, enterprises have a variety of raw materials, which need to be tested and acid leaching tests with hydrochloric acid of different concentrations need to be carried out. During the test, it is necessary to test the loss of tungsten in the filtrate, the improvement of the quality of tungsten concentrate, and the consumption of hydrochloric acid and water. To achieve the industrial preparation of large quantities of mineral materials, corresponding experimental acid leaching equipment is needed for acid leaching testing.

[0003] Acid leaching equipment requires the addition of solid raw materials on the one hand, and the continuous addition of hydrochloric acid solution on the other hand. At present, most acid leaching equipment uses a single chamber and a single experiment to work, which has the problem of too long time for large-scale sampling experiments; secondly, the gas produced by the reaction of dilute hydrochloric acid solution and calcium carbonate material is carbon dioxide. When no gas is produced, it can be considered that the calcium carbonate is relatively reacted. Therefore, it is necessary to observe whether bubbles are generated to determine the continuous addition of dilute hydrochloric acid solution to detect the actual optimal ratio. The reaction in the reactor is difficult to observe first, and secondly, even if an observation port is set, it is difficult to observe continuously.

[0004] Therefore, we provide a new type of elastomer and detection mechanism for the high pressure roller grinding cylinder to solve the above problems. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0006] A tungsten mixed concentrate acid leaching experimental method comprises the following steps:

[0007] Step 1, assembling raw materials, the raw materials include mineral material 1, mineral material 2 and a mixture, and the mixture is a mass ratio of mineral material 1 to mineral material 2 of 1:1;

[0008] Step 2, the ore material 1 has a mass percentage of WO3 ≥ 31.0%, CaCO3 ≥ 15.2%, and total calcium ≥ 12.1%;

[0009] Mineral material 2 has a mass percentage of WO3 ≥ 24.0%, CaCO3 ≥ 20.0%, and total calcium ≥ 18.2%;

[0010] Step 3, preparing slurry: using a comparative test, ore material 1, ore material 2 and the mixed material are respectively added to bottom water and stirred to prepare a slurry with a concentration of 50%;

[0011] Step 4, diluting the raw hydrochloric acid to a hydrochloric acid solution, and grouping and preparing the concentrations to be 1 mol / L and 2 mol / L;

[0012] Step 5, passing the slurry into the reactor, and installing a liquid inlet pipe on the reactor, adding the dilute hydrochloric acid solution into the reactor, and the dilute hydrochloric acid solution is continuously added; recording the added volume of the dilute hydrochloric acid solution; when the dilute hydrochloric acid solution and the slurry do not generate bubbles, stop adding the dilute hydrochloric acid;

[0013] Step 6, pump out the mixed solution to obtain a mineral filter residue, add 75 ml of clean water to rinse the mineral filter residue; stir for 3-5 minutes, let stand and filter to obtain a primary filtrate;

[0014] Step 7, add 500 ml of clean water to the mineral residue after washing in step 6, stir for 3-5 minutes, and filter to obtain a secondary filtrate and residue.

[0015] In a further technical solution, in step 5, a reactor for acid leaching is required, wherein a plurality of reaction chambers are arranged in the reactor, and a drainage pipe is arranged at the bottom of the reactor; a fixed plate is installed in the reactor, and a filter rack is installed between the fixed plate and the drainage pipe; the filter rack and the fixed plate are both funnel-shaped and fixedly connected;

[0016] A leakage hole is provided on the fixed plate;

[0017] A gas detector and a rotor flowmeter are installed on the reactor, an exhaust hole is provided on each group of the reaction chambers, and the exhaust hole is connected to the gas pipeline connected to the gas detector, and the gas detector is connected to the air inlet of the rotor flowmeter, the air outlet of the rotor flowmeter is connected to the exhaust pipeline, and the exhaust pipeline is connected to an exhaust valve;

[0018] A displacement sensor is installed on the rotor flowmeter, a rotor is arranged in the rotor flowmeter, and a light shielding plate is arranged on the rotor.

[0019] In a further technical solution, valve 1 is provided on the liquid discharge pipe; valve 2 is installed on the liquid inlet pipe; a partition pipe is provided between adjacent reaction chambers, and a shut-off valve 1 is installed on the partition pipe; when a single group of reaction chambers is used independently, the shut-off valve 1 on the partition pipe is closed and the single group of reaction chambers is placed.

[0020] In a further technical solution, a discharge opening plate is installed on the reactor, and a closing ring is arranged in the reaction chamber; the closing ring is installed on the fixed plate;

[0021] A pressurized pipe port is installed on each group of reaction chambers, and a pressurized pipe is installed on the pressurized pipe port. Multiple groups of pressurized pipes are arranged and commonly connected to a total pressure pipe, and an electromagnetic control valve and a pressure regulating valve are installed in series outside the total pressure pipe, and a shut-off valve 2 is installed on the pressurized pipe; after the reaction of the dilute hydrochloric acid solution and the slurry is completed, a pressurized air flow needs to be introduced from the pressurized pipe port 9, and valve 1 is opened for drainage.

[0022] In a further technical solution, a position rack is detachably mounted on the top of the reactor, and the gas detector is mounted on the position rack;

[0023] The reactor is provided with a stirring shaft and a liquid inlet pipe, and a stirring blade is provided at the bottom of the stirring shaft.

[0024] In a further technical solution, the position frame is bent upward, and a position plate is installed on the position frame, and a main motor is installed on the position plate, the output end of the main motor is set downward, and a driving gear is installed on the output end;

[0025] The position frame is provided with a lateral opening on one side facing the stirring shaft, and the driving gear is adapted to extend out of the lateral opening and be installed with double-sided racks, both sides of the double-sided racks are provided with teeth, and one side is meshed with the driving gear;

[0026] A secondary gear is installed on the top of the stirring shaft extending out of the reactor, and the secondary gear is meshed with the tooth profile on the other side of the double-sided rack.

[0027] In a further technical solution, a guide plate is installed outside the position frame, the guide plate is bent and a slide bar is arranged inside; a slide groove is opened on the upper side of the racks on both sides, and the slide bar and the slide groove are matched.

[0028] In a further technical solution, a baffle is provided on one side of the double-sided rack relative to the position frame, and a travel switch is installed on the position frame; the travel switches are provided in two groups and are arranged opposite to each other, and a protective plate is installed on the opposite side of the two groups of travel switches, and the protective plate is fixedly connected to the position frame at the lateral opening;

[0029] The protection plate is provided with an open slot, and the contact rod of the travel switch extends out of the open slot;

[0030] In step 5, the main motor is turned on, driving the active gear to engage the double-sided racks and move, and the double-sided racks drive multiple sets of sub-gears to rotate; synchronously, when the baffle moves to the travel switch abutting the contact rod, the travel switch is turned on and off, and a signal is sent to the controller, which is installed on the inside of the reactor, to control the main motor to rotate in the opposite direction.

[0031] In a further technical solution, in step 5, two sets of signal graphs are obtained for the gas detector and the displacement sensor, the rotor flowmeter displacement range ∈ [a, b], and when it is at the value b, there is no airflow; the signal graph of the displacement sensor at the top of the rotor flowmeter is converted into a digital graph that conforms to the trend of a→b→a; when the value a appears again, valve 2 is closed by controlling the external circuit board.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] The present invention is provided with multiple reaction chambers for synchronous reaction, so that the synchronous reaction effect is easy to observe. The synchronous stirring effect is achieved by the gear rack set at the top, which can reduce the cost of equipment use and achieve a synchronous test effect. The present invention is provided with a pressurized pipeline to realize pressurized airflow to enable the ore liquid to be quickly discharged through the discharge pipe, and the pressurized airflow can quickly clean the inner wall of the reaction chamber, and achieve rapid extrusion onto the solid plate, so that the solid plate can achieve the effect of primary filtering of the filter residue, and the filter residue dropped on the filter mesh frame can be squeezed to achieve secondary filtering of the filter residue. The present invention is provided with double-sided racks to achieve the synchronous rotation of the driving gear and the auxiliary gear, and the travel switch set in the middle of the position frame can achieve the technical effect of extrusion-trigger-steering, and can achieve a reciprocating low-speed rotation effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is a front schematic diagram of the acid leaching equipment of the present invention;

[0035] Figure 2 It is a schematic top view of the acid leaching equipment of the present invention;

[0036] Figure 3 It is a top cross-sectional schematic diagram of the acid leaching equipment of the present invention;

[0037] Figure 4 for Figure 3 A magnified view of part A;

[0038] Figure 5 for Figure 3 A magnified view of part B;

[0039] Figure 6 It is a cross-sectional schematic diagram of the reaction kettle in the present invention;

[0040] Figure 7 This is a schematic diagram of the exterior of the reaction chamber of the present invention;

[0041] Figure 8 The rotor structure diagram of the present invention;

[0042] Fig. 9 A schematic diagram of a guide plate of the present invention;

[0043] Fig.10 It is a structural schematic diagram of the position frame of the present invention;

[0044] Fig.11 It is a curve diagram of rotor displacement and time in the acid leaching experimental method of the present invention.

[0045] In the figure:

[0046] 1. Reactor; 2. Reaction chamber; 3. Drain pipe; 4. Fixed plate; 5. Filter rack; 6. Gas detector; 7. Rotor flowmeter; 8. Exhaust hole; 10. Displacement sensor; 11. Rotor; 12. Valve 1; 13. Valve 2; 14. Separation pipeline; 15. Shut-off valve 1; 16. Discharge opening plate; 17. Pressurized pipeline; 18. Total pressure pipeline; 19. Solenoid control valve; 20. Pressure regulating valve; 21. Shut-off valve 2; 22. Position rack; 23. Stirring shaft; 24. Main motor; 25. Side port; 26. Driving gear; 27. Double-sided rack; 28. Sub-gear; 29. ​​Guide plate; 30. Slide; 31. Slide; 32. Baffle; 33. Travel switch; 34. Protective plate. DETAILED DESCRIPTION

[0047] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0048] See also Figure 1-11 The present invention provides a technical solution, a tungsten mixed concentrate acid leaching experimental method, comprising the following steps:

[0049] Step 1, assembling raw materials, the raw materials include mineral material 1, mineral material 2 and a mixture, and the mixture is a mass ratio of mineral material 1 to mineral material 2 of 1:1;

[0050] Step 2, the ore material 1 has a mass percentage of WO3 ≥ 31.0%, CaCO3 ≥ 15.2%, and total calcium ≥ 12.1%;

[0051] Mineral material 2 has a mass percentage of WO3 ≥ 24.0%, CaCO3 ≥ 20.0%, and total calcium ≥ 18.2%;

[0052] Step 3, preparing slurry: using a comparative test, ore material 1, ore material 2 and the mixed material are respectively added to bottom water and stirred to prepare a slurry with a concentration of 50%;

[0053] Step 4, diluting the raw hydrochloric acid to a hydrochloric acid solution, and grouping and preparing the concentrations to be 1 mol / L and 2 mol / L;

[0054] Step 5, the slurry is passed into the reactor 1, and a liquid inlet pipe is installed on the reactor 1, and the dilute hydrochloric acid solution is added into the reactor 1, and the dilute hydrochloric acid solution is added continuously; the added volume of the dilute hydrochloric acid solution is recorded; when the dilute hydrochloric acid solution and the slurry do not generate bubbles, the addition of the dilute hydrochloric acid is stopped;

[0055] Step 6, pump out the mixed solution to obtain a mineral filter residue, add 75 ml of clean water to rinse the mineral filter residue; stir for 3-5 minutes, let stand and filter to obtain a primary filtrate;

[0056] Step 7, add 500 ml of clean water to the mineral residue after washing in step 6, stir for 3-5 minutes, and filter to obtain a secondary filtrate and residue.

[0057] Table 1 below is a set of components of the raw material ore:

[0058] Table 1. Elemental analysis results of experimental raw materials

[0059]

[0060] After further acid leaching and concentration method, the following acid leaching indexes are obtained, as shown in Table 2-4:

[0061] Table 2. Mineral Acid Leaching Results

[0062]

[0063] Table 3. Acid leaching results of persimmon concentrate

[0064]

[0065]

[0066] Table 4. Acid leaching results of mixed concentrate

[0067]

[0068] The consumption of hydrochloric acid and water in the acid leaching process is shown in Table 5-7:

[0069] Table 5. Dongbo concentrate material consumption

[0070] Hydrochloric acid concentration (mol) Hydrochloric acid consumption (mol / kg concentrate) Industrial water consumption (L / kg concentrate) 2 3.12 26.11 1 3.36 61.63

[0071] Table 6. Consumption of concentrated mineral materials for persimmon selection

[0072] Hydrochloric acid concentration (mol) Hydrochloric acid consumption (mol / kg concentrate) Industrial water consumption (L / kg concentrate) 2 3.61 31.24 1 3.75 68.87

[0073] Table 7. Consumption of synthetic mineral materials

[0074] Hydrochloric acid concentration (mol) Hydrochloric acid consumption (mol / kg concentrate) Industrial water consumption (L / kg concentrate) 2 3.74 34.82 1 3.78 75.11

[0075] Experimental conclusion:

[0076] 1. From the acid leaching indicators, it can be seen that when the calcium carbonate content in tungsten concentrate fluctuates within the range of 15.54%-20.11%, the calcium carbonate content in the concentrate after acid leaching does not exceed 0.5%; at the same time, the grade of tungsten concentrate increases from 31%, 24%, and 27% to 37%, 31%, and 34%, respectively, with an increase of 6 to 7 percentage points.

[0077] 2. When the acid leaching test was carried out using 1mol / L (3.65%) and 2mol / L (7.30%) hydrochloric acid solutions as raw materials, the tungsten content in the filtrate after acid leaching fluctuated within the range of 0.5mg / L-1.5mg / L, and the loss rate of tungsten metal in the filtrate did not exceed 0.0025%.

[0078] 3. According to the test results, the hydrochloric acid consumption of Dongbo tungsten concentrate is 3.24mol / (kg concentrate), that is, 0.394 tons of industrial hydrochloric acid (concentration 30%) are consumed per ton of tungsten concentrate; the hydrochloric acid consumption of Persimmon tungsten concentrate is 3.68mol / (kg concentrate), that is, 0.448 tons of industrial hydrochloric acid (concentration 30%) are consumed per ton of tungsten concentrate; the hydrochloric acid consumption of mixed concentrate is 3.76mol / (kg concentrate), that is, 0.458 tons of industrial hydrochloric acid (concentration 30%) are consumed per ton of tungsten concentrate.

[0079] 4. The consumption of industrial water during acid leaching is as follows: Under the condition of high concentration hydrochloric acid solution (2mol / L), the water required for East Selected Concentrate is 26.11m 3 / ton of concentrate; persimmon concentrate requires 31.24m3 of water 3 / ton of concentrate; mixed concentrate requires 34.82m3 of water 3 / ton of concentrate. Under the condition of low concentration hydrochloric acid solution (1mol / L), the water required for East selection concentrate is 61.63m 3 / ton of concentrate; persimmon concentrate requires 68.87m3 of water 3 / ton of concentrate; mixed concentrate requires 75.11m3 of water 3 / ton of concentrate;

[0080] 5. Finally, high concentration hydrochloric acid solution (2mol / L) is used as the condition, and the mixed concentrate is used as the raw material. 0.458 tons of industrial hydrochloric acid is consumed per ton of concentrate. The pH of the acid leaching filtrate is basically maintained at about 2.5. According to pH=2, the residual hydrochloric acid in the filtrate is 0.01mol / L (concentration is 0.0365%), and the water consumption is 34.82m3 / ton of concentrate. The residual hydrochloric acid is 348.2mol, that is, 0.042 tons of industrial hydrochloric acid, and the residual amount is 9.17%.

[0081] Further, such as Figure 1-3As shown, in step 5, a reactor 1 is required to perform acid leaching, wherein a plurality of reaction chambers 2 are arranged in the reactor 1, and a drain pipe 3 is arranged at the bottom of the reactor 1; a fixed plate 4 is installed in the reactor 1, and a filter rack 5 is installed between the fixed plate 4 and the drain pipe 3; the filter rack 5 and the fixed plate 4 are both funnel-shaped and fixedly connected; a leakage hole is opened on the fixed plate 4;

[0082] A gas detector 6 and a rotor flowmeter 7 are installed on the reactor 1, and an exhaust hole 8 is provided on each group of the reaction chambers 2, and the exhaust hole 8 is connected to the gas pipeline connected to the gas detector 6, and the gas detector 6 is connected to the air inlet of the rotor flowmeter 7; a displacement sensor 10 is installed on the rotor flowmeter 7, and a rotor 11 is provided in the rotor flowmeter 7, and a light shielding plate is provided on the rotor 11, such as Figure 8 As shown,.

[0083] A valve 12 is provided on the liquid discharge pipe 3; a valve 2 13 is installed on the liquid inlet pipe; a partition pipe 14 is provided between adjacent reaction chambers 2, and a shut-off valve 15 is installed on the partition pipe 14; when a single group of reaction chambers 2 is used independently, the shut-off valve 15 on the partition pipe 14 is closed and the single group of reaction chambers is placed.

[0084] A discharge opening plate 16 is installed on the reactor 1, and a closing ring is provided in the reaction chamber 2; the closing ring is installed on the fixed plate 4; Figure 2 and 3 As shown, each group of the reaction chambers 2 is provided with a pressurized nozzle 9, a pressurized pipe 17 and a total pressure pipe 18 are provided with the pressurized nozzle 9, and an electromagnetic control valve 19 and a pressure regulating valve 20 are provided in series outside the total pressure pipe 18, and a shut-off valve 21 is provided on the pressurized pipe 17; after the reaction of the dilute hydrochloric acid solution and the ore pulp is completed, a pressurized air flow needs to be introduced from the pressurized nozzle 9, and a valve 12 needs to be opened for drainage.

[0085] A position frame 22 is detachably mounted on the top of the reactor 1 , and the gas detector 6 is mounted on the position frame 22 ; a stirring shaft 23 and a liquid inlet pipe are mounted on the reactor 1 , and a stirring blade is mounted on the bottom of the stirring shaft 23 .

[0086] like Figure 4 , 5As shown in 10, the position frame 22 is bent upward, and a position plate is installed on the position frame 22, and a main motor 24 is installed on the position plate, the output end of the main motor 24 is set downward, and a driving gear 26 is installed on the output end; the position frame 22 is provided with a lateral opening 25 on the side facing the stirring shaft 23, and the driving gear 26 is suitable for extending out of the lateral opening 25 and is installed with a double-sided rack 27, both sides of the double-sided rack 27 are provided with teeth, and one side is meshed with the driving gear 26; a sub-gear 28 is installed at the top of the stirring shaft 23 extending out of the reactor 1, and the sub-gear 28 is meshed with the teeth on the other side of the double-sided rack 27.

[0087] like Fig. 9 As shown, a guide plate 29 is installed outside the position frame 22, and the guide plate 29 is bent and a slide bar 31 is arranged inside; a slide groove 30 is opened on the upper side of the double-sided rack 27, and the slide bar 31 and the slide groove 30 are adapted.

[0088] like Figure 5 As shown, a baffle 32 is provided on one side of the double-sided rack 27 relative to the position frame 22, and a travel switch 33 is installed on the position frame 22; two groups of travel switches 33 are provided and installed oppositely, and a protective plate 34 is installed on the opposite side of the two groups of travel switches 33, and the protective plate 34 is fixedly connected to the position frame 22 at the lateral opening 25; the baffle 32 is located between the travel switches, and the baffle moves between the two groups of switches to achieve reciprocating movement control. An open slot is provided on the protective plate 34, and the touch rod of the travel switch 33 extends out of the open slot;

[0089] In step 5, the main motor 24 is turned on, driving the driving gear 26 to engage the double-sided racks 27 to move, and the double-sided racks 27 drive the multiple sets of sub-gears 28 to rotate; synchronously, when the baffle 32 moves to the limit switch 33 abuts the contact rod, the limit switch 33 is turned on and off, and a signal is sent to the controller, which is installed on the inner side of the reactor 1, and the transmission model controls the main motor 24 to rotate in the opposite direction.

[0090] like Fig.11 As shown, in step 5, two groups of signal graphs are obtained for the gas detector 6 and the displacement sensor 10. The displacement range of the rotor flowmeter 7 is ∈ [a, b], and when it is at the value b, there is no airflow passing through; the signal graph of the displacement sensor 10 at the top of the rotor flowmeter 7 is converted into a digital graph in accordance with the trend of a→b→a; when the value a appears again, the valve 2 13 is closed by controlling the external circuit board. The change between a and b is a continuous curve or straight line, referring to the continuity of the actual reaction.

[0091] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0092] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A tungsten mixed concentrate acid leaching experimental method, characterized in that: The following steps are involved: Step 1, assembling raw materials, the raw materials include mineral material 1, mineral material 2 and a mixture, and the mixture is a mass ratio of mineral material 1 to mineral material 2 of 1:1; Step 2, the ore material 1 has a mass percentage of WO3 ≥ 31.0%, CaCO3 ≥ 15.2%, and total calcium ≥ 12.1%; Mineral material 2 has a mass percentage of WO3 ≥ 24.0%, CaCO3 ≥ 20.0%, and total calcium ≥ 18.2%; Step 3, preparing slurry: using a comparative test, ore material 1, ore material 2 and the mixed material are respectively added to bottom water and stirred to prepare a slurry with a concentration of 50%; Step 4, diluting the raw hydrochloric acid to a hydrochloric acid solution, and grouping and preparing the concentrations to be 1 mol / L and 2 mol / L; Step 5, introducing the slurry into the reactor (1), and installing a liquid inlet pipe on the reactor (1), adding the dilute hydrochloric acid solution into the reactor (1), and the dilute hydrochloric acid solution is continuously added; recording the added volume of the dilute hydrochloric acid solution; and providing a detection component, when the dilute hydrochloric acid solution and the slurry do not generate bubbles, stopping the addition of the dilute hydrochloric acid; Step 6, pump out the mixed solution to obtain a mineral filter residue, add 75 ml of clean water to rinse the mineral filter residue; stir for 3-5 minutes, let stand and filter to obtain a primary filtrate; Step 7, add 500 ml of clean water to the mineral residue after washing in step 6, stir for 3-5 minutes, and filter to obtain a secondary filtrate and residue.

2. The tungsten mixed concentrate acid leaching experimental method according to claim 1 is characterized in that: In step 5, a reaction kettle (1) is required to perform acid leaching, wherein a plurality of reaction chambers (2) are arranged in the reaction kettle (1), and a drainage pipe (3) is arranged at the bottom of the reaction kettle (1); a fixed plate (4) is installed in the reaction kettle (1), and a filter rack (5) is installed between the fixed plate (4) and the drainage pipe (3); the filter rack (5) and the fixed plate (4) are both funnel-shaped and fixedly connected; A liquid leakage hole is provided on the fixed plate (4); The detection component is installed on the reaction kettle (1), and includes a gas detector (6) and a rotor flow meter (7). Each group of the reaction chambers (2) is provided with an exhaust hole (8), and the exhaust hole (8) is connected to a gas pipeline connected to the gas detector (6), and the gas detector (6) is connected to the air inlet of the rotor flow meter (7); A displacement sensor (10) is installed on the rotor flowmeter (7), a rotor (11) is arranged in the rotor flowmeter (7), and a light shielding plate is arranged on the rotor (11).

3. The acid leaching experimental method of tungsten mixed concentrate according to claim 1 is characterized in that: A valve (12) is provided on the liquid discharge pipe (3); a valve (13) is installed on the liquid inlet pipe; a partition pipe (14) is provided between adjacent reaction chambers (2), and a shutoff valve (15) is installed on the partition pipe (14); when a single group of reaction chambers (2) is used independently, the shutoff valve (15) on the partition pipe (14) is closed and the single group of reaction chambers is placed.

4. The acid leaching experimental method of tungsten mixed concentrate according to claim 3 is characterized in that: A discharge opening plate (16) is installed on the reaction kettle (1), and a closing ring is arranged in the reaction chamber (2); the closing ring is installed on the fixed plate (4); Each group of reaction chambers (2) is provided with a pressurized pipe port (9), a pressurized pipe (17) is provided on the pressurized pipe port (9), a total pressure pipe (18) is connected to the outside of the pressurized pipe (17), an electromagnetic control valve (19) and a pressure regulating valve (20) are installed in series outside the total pressure pipe (18), and a shut-off valve 2 (21) is installed on the pressurized pipe (17); after the reaction of the dilute hydrochloric acid solution and the ore slurry is completed, a pressurized air flow needs to be introduced from the pressurized pipe port (9), and the valve 1 (12) needs to be opened to discharge the liquid.

5. The acid leaching experimental method of tungsten mixed concentrate according to claim 3 is characterized in that: A position frame (22) is detachably mounted on the top of the reactor (1), and the gas detector (6) is mounted on the position frame (22); The reactor (1) is provided with a stirring shaft (23) and a liquid inlet pipe, and a stirring blade is provided at the bottom of the stirring shaft (23).

6. The tungsten mixed concentrate acid leaching experimental method according to claim 1, characterized in that: The position frame (22) is bent upward, a position plate is mounted on the position frame (22), a main motor (24) is mounted on the position plate, an output end of the main motor (24) is arranged downward, and a driving gear (26) is mounted on the output end; The position frame (22) is provided with a lateral opening (25) on one side facing the stirring shaft (23), and the driving gear (26) is adapted to extend out of the lateral opening (25) and be installed with double-sided racks (27), both sides of the double-sided racks (27) are provided with teeth, and one side is meshed with the driving gear (26); A pinion gear (28) is installed on the top of the stirring shaft (23) extending out of the reaction kettle (1), and the pinion gear (28) is meshed with the teeth on the other side of the double-sided rack (27).

7. The acid leaching experimental method of tungsten mixed concentrate according to claim 5 is characterized in that: A guide plate (29) is installed outside the position frame (22), and the guide plate (29) is bent and has a slide bar (31) inside; a slide groove (30) is opened on the upper side of the double-sided racks (27), and the slide bar (31) and the slide groove (30) are matched.

8. The tungsten mixed concentrate acid leaching experimental method according to claim 6 is characterized in that: A baffle (32) is provided on one side of the double-sided rack (27) relative to the position frame (22), and a travel switch (33) is installed on the position frame (22); two groups of travel switches (33) are provided and installed opposite to each other, and a protective plate (34) is installed on the opposite side of the two groups of travel switches (33), and the protective plate (34) is fixedly connected to the position frame (22) at the lateral opening (25); The protection plate (34) is provided with an open slot, and the contact rod of the travel switch (33) extends out of the open slot; In step 5, the main motor (24) is turned on, driving the driving gear (26) to engage with the double-sided racks (27) to move, and the double-sided racks (27) drive the multiple sets of sub-gears (28) to rotate; synchronously, when the baffle (32) moves to the limit switch (33) against the contact rod, the limit switch (33) is turned on and off, and a signal is sent to the controller installed on the inner side of the reactor (1), and the transmission model controls the main motor (24) to rotate in the opposite direction.

9. The tungsten mixed concentrate acid leaching experimental method according to claim 1, characterized in that: In step 5, two groups of signal graphs are obtained from the gas detector (6) and the displacement sensor (10). The displacement range of the rotor flowmeter (7) is ∈[a, b], and when it is at the value b, there is no airflow passing through. The signal graph of the displacement sensor (10) at the top of the rotor flowmeter (7) is converted into a digital graph in accordance with the trend of a→b→a. When the value a appears again, the valve 2 (13) is closed by controlling the external circuit board.

Images