Wastewater detection sampling device for lithium ore flotation, sulfonamide-containing collector and preparation method

Abstract

The application provides a wastewater detection sampling device for lithium ore flotation, a sulfonamide-containing collector and a preparation method, relates to the technical field of wastewater sampling, and comprises a sampling box, a suction mechanism, a layered sampling mechanism and a mixed sampling mechanism. The suction mechanism comprises a mounting seat arranged at the bottom of the sampling box, two threaded support legs which are threadedly connected to the inner side of the mounting seat, a suction pump arranged at the top of the mounting seat, and a water inlet pipe fixed to the inner side of the sampling box. The cooperation between the driving motor and the electric push rod can sequentially pour the sampling water in the four sampling bottles into the mixing cylinder, so that the mixed sample of the flotation wastewater can be obtained. After the mixed sample is obtained, the cooperation between the driving motor and the suction mechanism can again perform layered sampling on the lithium ore flotation wastewater at different depths. The lithium ore flotation wastewater can be layered sampled and mixed sampled at one time, and the sampling efficiency of the lithium ore flotation wastewater is effectively improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of wastewater sampling, in particular to a wastewater detection sampling device for lithium ore flotation, a sulfonamide-containing collector and a preparation method. BACKGROUND

[0002] Wastewater detection sampling after lithium ore flotation is a crucial link in industrial production. The flotation wastewater usually contains heavy metals, flotation reagent residues, suspended solids and fluorides, etc. Direct discharge will pollute water bodies, soil and threaten the ecological system. Moreover, by detecting the residual concentration of flotation reagents in wastewater, the dosage of flotation reagents can be optimized, the utilization rate of reagents can be improved, and the production cost can be reduced.

[0003] Publication No. CN221485409U discloses a filtering sampling and detection device for industrial wastewater treatment. The device is provided with a movable frame outside the filter cartridge, a plurality of brushes are installed on the movable frame, a plurality of gears are engaged to drive the plurality of brushes to rotate to clean the filter cartridge, prevent the filter cartridge from being blocked, and ensure the sampling efficiency. A plurality of storage bottles are arranged on the movable turntable in the treatment box to store wastewater at different positions. The device can be used for on-site detection with a wastewater detector. The device can also pour the sample into the collection chamber without leaving a protective sample, which greatly improves the detection efficiency.

[0004] In the related art, after the lithium ore is floated, a detection sampling device is used to sample the wastewater generated during the flotation. However, after the lithium ore wastewater is discharged, the upper clear liquid and the bottom slurry will be stratified. The existing sampling device is not convenient for stratified sampling and mixed sampling of the lithium ore flotation wastewater at one time.

[0005] Therefore, it is necessary to provide a wastewater detection sampling device for lithium ore flotation, a sulfonamide-containing collector and a preparation method to solve the above technical problems. SUMMARY

[0006] The present application provides a wastewater detection sampling device for lithium ore flotation, a sulfonamide-containing collector and a preparation method, which solves the technical problem that the existing sampling device in the related art is not convenient for stratified sampling and mixed sampling of the lithium ore flotation wastewater at one time.

[0007] To solve the above technical problems, the wastewater detection sampling device for lithium ore flotation provided by the present application comprises a sampling box, a suction mechanism, a stratified sampling mechanism and a mixed sampling mechanism.

[0008] The suction mechanism comprises a mounting seat arranged at the bottom of the sampling box, two threaded support legs threadedly connected to the inner side of the mounting seat, a suction pump arranged at the top of the mounting seat, a water inlet pipe fixed to the inner side of the sampling box, and a drain pipe communicated with the right side of the water inlet pipe.

[0009] The layered sampling mechanism comprises a rotating shaft which is vertically connected to the inner side of the sampling box, the bottom end of the rotating shaft is fixedly provided with a rotating disc, the top of the rotating disc is fixedly provided with two rotating seats, the inner side of the two rotating seats is rotatably connected with rotating rods, the surface of the two rotating rods is fixedly provided with overturning seats, the top of the overturning seats is fixedly provided with two clamping frames, the opposite side of the two clamping frames is provided with sampling bottles, and the top of the sampling box is provided with a driving motor for driving the rotating shaft to rotate;

[0010] The mixed sampling mechanism comprises an electric push rod which is fixedly arranged in the inner side of the sampling box, the output end of the electric push rod is fixedly provided with a gear plate, the right end of the rotating rod is fixedly provided with a gear, the bottom of the inner wall of the sampling box is fixedly provided with an annular disc, and the bottom of the sampling box is fixedly provided with a mixing cylinder.

[0011] Preferably, the surface of the water inlet pipe and the surface of the drain pipe are provided with valves, and the suction pump is communicated with the water inlet pipe through a hose when the suction pump works.

[0012] Preferably, the sampling bottles arranged on the top of the rotating disc are arranged in four groups along the center of the rotating disc, when the electric push rod drives the gear plate to extend, the gear plate is engaged with the gear, and the rotating rod and the overturning seat are driven to rotate clockwise through the gear.

[0013] Preferably, the bottom of the rotating disc is fixedly provided with a driving mechanism, the driving mechanism comprises a gear disc which is fixedly arranged at the bottom of the rotating disc, the inner side of the left side of the annular disc is fixedly provided with a supporting seat, the top of the supporting seat is rotatably connected with a driven gear, the driven gear is engaged with the gear disc, the top of the driven gear is fixedly provided with a half gear, the inner wall of the sampling box is fixedly provided with a guide rod, the surface of the guide rod is slidably connected with a rack seat, the half gear is engaged with the rack seat, and the surface of the guide rod and the front side of the rack seat are sleeved with a spring;

[0014] The top of the supporting seat is fixedly provided with a detection mechanism, the detection mechanism comprises a sliding rail which is fixedly arranged at the top of the supporting seat, the surface of the sliding rail is slidably connected with a sliding frame, the inner side of the sliding frame is provided with a PH detector, the right side of the sliding frame is rotatably connected with a guide wheel, the top of the rack seat is fixedly provided with a moving plate, and the inner side of the moving plate is slidably connected with the guide wheel.

[0015] Preferably, the back of the inner wall of the sampling box is fixedly provided with a dropping mechanism, the dropping mechanism comprises a fixed disc which is fixedly arranged on the back of the inner wall of the sampling box, the bottom of the fixed disc is fixedly provided with a funnel, the surface of the rotating shaft is fixedly provided with a storage disc, the bottom of the storage disc is rotatably connected with the top of the fixed disc, and the top of the sampling box is communicated with a dropping pipe.

[0016] Preferably, the bottom end of the rotating shaft is fixedly provided with a mixing mechanism, the mixing mechanism comprises a mixing shaft fixedly provided at the bottom end of the rotating shaft, the surface of the mixing shaft is fixedly provided with two groups of connecting frames, the surface of the two groups of connecting frames is fixedly provided with a mixing frame, and the bottom end of the mixing shaft is fixedly provided with a mixing paddle.

[0017] Preferably, the bottom of the mixing cylinder is communicated with a discharge pipe, the right side of the sampling box is fixedly provided with a controller, the front side of the sampling box is rotationally connected with a box door, the bottom of the sampling box is fixedly provided with four supporting legs, and the mounting seat is fixedly connected with two supporting legs on the front side.

[0018] The sulfonamide-containing collector comprises a compound having the following general chemical structure or a chemical isomer or a salt thereof:

[0019] The core structure is a sulfonamide group (-SO2NH-), and carbon chains of different lengths are connected on both sides to form a structure of "carbon chain-sulfonamide group-carbon chain";

[0020] The compound is one of the following compounds:

[0021] JL-173: The sulfonamide group is connected to a straight-chain alkyl group containing 4 carbons on one side and to a straight-chain alkyl group containing 4 carbons on the other side;

[0022] JL-174: The sulfonamide group is connected to a straight-chain alkyl group containing 4 carbons on one side and to a straight-chain alkyl group containing 6 carbons on the other side;

[0023] JL-175: The sulfonamide group is connected to a straight-chain alkyl group containing 6 carbons on one side and to a straight-chain alkyl group containing 4 carbons on the other side;

[0024] JL-176: The sulfonamide group is connected to a straight-chain alkyl group containing 8 carbons on both sides;

[0025] JL-177: The sulfonamide group is connected to a straight-chain alkyl group containing 8 carbons on one side and to a straight-chain alkyl group containing 6 carbons on the other side;

[0026] JL-178: The sulfonamide group is connected to a straight-chain alkyl group containing 10 carbons on both sides;

[0027] JL-179: The sulfonamide group is connected to a straight-chain alkyl group containing 12 carbons on both sides.

[0028] The sulfonamide-containing collector preparation method comprises the following steps:

[0029] S1: Dissolve a sulfuryl chloride derivative A (1.0 equivalent) in dichloromethane (DCM) (0.4 M) in a round-bottom flask, and cool the reaction mixture to 0 degrees Celsius in an ice bath;

[0030] S2: The amine derivative B (1.1 eq) and Et3N (1.2 eq) were added to the solution under stirring and the reaction mixture was slowly heated to room temperature and stirring was continued until TLC showed complete consumption of the starting material;

[0031] S3: The reaction mixture was quenched with 1.0 M HC1 and the reaction mixture was extracted with methyl chloroform three times and the combined organic phase was washed with brine and the residue was dried over anhydrous Na2S04;

[0032] S4: The solution was concentrated under vacuum and finally purified on a silica gel column using petroleum ether and ethyl acetate to obtain the product C.

[0033] Preferably, the vacuum system needs to be strictly sealed during the process of vacuum concentration of the solution to avoid air leakage affecting the vacuum degree, and the equipment needs to be cleaned immediately after concentration to prevent the residue from solidifying.

[0034] Compared with the related art, the lithium ore flotation wastewater detection sampling device, the sulfonamide-containing collector and the preparation method have the following beneficial effects:

[0035] The driving motor is used for rotating clockwise to sequentially adjust the positions of the four sampling bottles, and then the suction mechanism is used for sucking the lithium ore flotation wastewater at different depths into the four sampling bottles, so as to perform stratified sampling on the lithium ore flotation wastewater. The electric push rod is used for driving the gear plate to extend to the left, so that the gear drives the turnover seat and the sampling bottle to rotate, and the sampling water in the sampling bottle flows into the mixing cylinder through the annular disc. The driving motor and the electric push rod are matched, so that the sampling water in the four sampling bottles can be sequentially poured into the mixing cylinder, so as to perform mixed sampling on the flotation wastewater. After the mixed sampling, the driving motor and the suction mechanism are matched, so that the stratified sampling on the lithium ore flotation wastewater at different depths can be performed again. The lithium ore flotation wastewater can be stratified sampled and mixed sampled at one time, and the sampling efficiency of the lithium ore flotation wastewater is effectively improved. BRIEF DESCRIPTION OF DRAWINGS

[0036] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor based on the drawings shown.

[0037] Figure 1 The best structure schematic diagram provided by the present application is provided.

[0038] Figure 2 The structure schematic diagram of the rear view provided by the present application is provided.

[0039] Figure 3 isFigure 1 Structure schematic view of the sampling box cross section view shown in the figure;

[0040] Figure 4 Structure schematic view of the suction mechanism provided by the present application;

[0041] Figure 5 Structure schematic view of the layered sampling mechanism provided by the present application;

[0042] Figure 6 Structure schematic view of the mixed sampling mechanism provided by the present application;

[0043] Figure 7 Structure schematic view of the Figure 6 and Figure 5 Structure schematic view of the state that the electric push rod and the gear plate extend, and the gear drives the rotary rod and the turnover seat to rotate;

[0044] Figure 8 Structure schematic view of the driving mechanism and the detection mechanism provided by the present application;

[0045] Figure 9 Structure schematic view of the Figure 8 Structure schematic view of the bottom view of the rotary disc shown in the figure;

[0046] Figure 10 Structure schematic view of the state that the gear disc drives the passive gear and the half gear to rotate, and the rack seat slides forward on the surface of the guide rod;

[0047] Figure 11 Structure schematic view of the dropping mechanism provided by the present application;

[0048] Figure 12 Structure schematic view of the mixing mechanism provided by the present application;

[0049] Figure 13 General chemical structure of the sulfonamide-containing collector provided by the present application;

[0050] Figure 14 General chemical structure of the compound provided by the present application.

[0051] Explanation of the reference numerals:

[0052] 1. Sampling box;

[0053] 2. Suction mechanism; 21. Mounting seat; 22. Threaded support leg; 23. Suction pump; 24. Water inlet pipe; 25. Drain pipe;

[0054] 3. Layered sampling mechanism; 31. Rotary shaft; 32. Rotary disc; 33. Rotary seat; 34. Rotary rod; 35. Turnover seat; 36. Clamping frame; 37. Sampling bottle; 38. Driving motor;

[0055] 4, mixed sampling mechanism; 41, electric push rod; 42, gear plate; 43, gear;

[0056] 5, annular disc; 6, mixing cylinder;

[0057] 7, drive mechanism; 71, gear disc; 72, support seat; 73, passive gear; 74, half gear; 75, guide rod; 76, rack seat; 77, spring;

[0058] 8, detection mechanism; 81, slide rail; 82, sliding frame; 83, PH detector; 84, guide wheel; 85, moving plate;

[0059] 9, delivery mechanism; 91, fixed disc; 92, funnel; 93, storage disc; 94, delivery pipe;

[0060] 10, mixing mechanism; 101, mixing shaft; 102, connecting frame; 103, mixing frame; 104, mixing paddle;

[0061] 11, discharge pipe; 12, controller; 13, box door; 14, support leg.

[0062] The implementation, functional features and advantages of the present application will be further described with reference to the embodiments in combination with the accompanying drawings. DETAILED DESCRIPTION

[0063] The technical solutions in the embodiments of the present application will be described clearly and completely below in combination with the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0064] The present application provides a wastewater detection sampling device for lithium ore flotation, a sulfonamide collector and a preparation method.

[0065] First embodiment:

[0066] Please refer to Figures 1 to 7 , the wastewater detection sampling device for lithium ore flotation comprises a sampling box 1, a suction mechanism 2, a layered sampling mechanism 3 and a mixed sampling mechanism 4.

[0067] The suction mechanism 2 comprises a mounting seat 21 arranged at the bottom of the sampling box 1, two threaded support legs 22 threadedly connected to the inner side of the mounting seat 21, and a suction pump 23 arranged at the top of the mounting seat 21.

[0068] Please combine Figure 4The suction pipe is connected to the surface of the suction pump 23, and then the suction pump 23 is started. The suction pump 23 pumps the flotation wastewater into the water inlet pipe 24 through the hose. By controlling the height of the suction pipe in the flotation wastewater, the wastewater at different heights can be pumped layer by layer.

[0069] Preferably, when the upper layer of wastewater is pumped out, and the lower layer of wastewater needs to be pumped out, by controlling the valve on the surface of the water inlet pipe 24 and the water outlet pipe 25, the residual wastewater in the pipe can be discharged through the water outlet pipe 25, and then the lower layer of wastewater can be discharged into the sampling box 1 through the water inlet pipe 24, avoiding the mixing of the sampling water during layer sampling.

[0070] The layer sampling mechanism 3 comprises a rotating shaft 31 vertically connected to the inner side of the sampling box 1. The bottom end of the rotating shaft 31 is fixedly provided with a rotating disc 32. The top of the rotating disc 32 is fixedly provided with two rotating seats 33. The inner sides of the two rotating seats 33 are rotatably connected with rotating rods 34. The surfaces of the two rotating rods 34 are fixedly provided with overturning seats 35. The top of the overturning seat 35 is fixedly provided with two clamping frames 36. The opposite sides of the two clamping frames 36 are provided with sampling bottles 37. The top of the sampling box 1 is provided with a driving motor 38 for driving the rotating shaft 31 to rotate.

[0071] Please refer to Figure 3 and Figure 5 : The driving motor 38 is started. The driving motor 38 drives the rotating shaft 31 to rotate. The rotating shaft 31 rotates and drives the rotating disc 32 to rotate. The rotating disc 32 rotates to adjust the positions of the four sampling bottles 37 in turn, and then the sampled wastewater is classified and stored.

[0072] Preferably, the driving motor 38 rotates 90 degrees clockwise each time.

[0073] The mixing sampling mechanism 4 comprises an electric push rod 41 fixedly arranged on the inner side of the sampling box 1. The output end of the electric push rod 41 is fixedly provided with a gear plate 42. The right end of the rotating rod 34 is fixedly provided with a gear 43. The bottom of the inner wall of the sampling box 1 is fixedly provided with an annular disc 5. The bottom of the sampling box 1 is fixedly provided with a mixing cylinder 6.

[0074] Please refer to Figure 6 and Figure 7 : The electric push rod 41 is started. The electric push rod 41 extends and drives the gear plate 42 to extend to the left. When the gear plate 42 contacts the gear 43, the gear 43 drives the rotating rod 34, the overturning seat 35, the clamping frame 36 and the sampling bottle 37 to rotate, so that the sampling bottle 37 is inclined, the sampling water in the sampling bottle 37 is overturned, and the sampling water flows into the mixing cylinder 6 through the annular disc 5.

[0075] Further, when the sampling water in the sampling bottle 37 flows into the mixing cylinder 6, the electric push rod 41 is started to drive the gear plate 42 to reset to the right, the gear plate 42 moves to the right to drive the gear 43 to rotate in the reverse direction, thereby resetting the turnover seat 35 and the sampling bottle 37;

[0076] Further, the positions of the four sampling bottles 37 are adjusted by intermittent rotation of the driving motor 38, and under the reciprocating working state of the electric push rod 41, the sampling water in the four sampling bottles 37 can be poured into the mixing cylinder 6 in sequence, thereby mixing the sampling of the flotation wastewater.

[0077] The surfaces of the water inlet pipe 24 and the drain pipe 25 are provided with valves, and the suction pump 23 is in communication with the water inlet pipe 24 through a hose when it is working.

[0078] The sampling bottles 37 arranged on the top of the rotating disc 32 are arranged in four groups along the center of the rotating disc 32, and when the electric push rod 41 drives the gear plate 42 to extend, the gear plate 42 is engaged with the gear 43, and the rotating rod 34 and the turnover seat 35 are driven to rotate clockwise by the gear 43.

[0079] In the embodiment, unlike the existing wastewater sampling device, the driving motor 38 is rotated clockwise to adjust the positions of the four sampling bottles 37 in sequence, and then the suction mechanism 2 is used to draw the lithium ore flotation wastewater at different depths into the four sampling bottles 37, thereby stratified sampling the lithium ore flotation wastewater. The electric push rod 41 drives the gear plate 42 to extend to the left, so that the gear 43 drives the turnover seat 35 and the sampling bottle 37 to rotate, and the sampling water in the sampling bottle 37 flows into the mixing cylinder 6 through the annular disc 5. Through the cooperation between the driving motor 38 and the electric push rod 41, the sampling water in the four sampling bottles 37 can be poured into the mixing cylinder 6 in sequence, thereby mixing the sampling of the flotation wastewater. After mixing the sampling, the driving motor 38 and the suction mechanism 2 can be used to stratify sample the lithium ore flotation wastewater at different depths again, which facilitates stratified sampling and mixing sampling of the lithium ore flotation wastewater at one time, effectively improves the sampling efficiency of the lithium ore flotation wastewater, and facilitates rapid detection of the collector residual amount in the lithium ore flotation wastewater.

[0080] Second embodiment:

[0081] Please refer to Figure 3 , Figures 8 to 11The bottom of the rotating disc 32 is fixedly provided with a driving mechanism 7, the driving mechanism 7 comprises a gear disc 71 fixedly provided on the bottom of the rotating disc 32, the inner side of the left side of the annular disc 5 is fixedly provided with a supporting seat 72, the top of the supporting seat 72 is rotationally connected with a driven gear 73, the driven gear 73 is engaged with the gear disc 71, the top of the driven gear 73 is fixedly provided with a half gear 74, the inner wall of the sampling box 1 is fixedly provided with a guide rod 75, the surface of the guide rod 75 is slidingly connected with a rack seat 76, the half gear 74 is engaged with the rack seat 76, the surface of the guide rod 75 and located in front of the rack seat 76 is sleeved with a spring 77;

[0082] Please combine Figure 8 and Figure 9 : when the rotating disc 32 rotates, the bottom gear disc 71 is driven to rotate, the gear disc 71 rotates to drive the driven gear 73 and the half gear 74 to rotate counterclockwise, the half gear 74 rotates to drive the rack seat 76 to slide forward on the surface of the guide rod 75, so that the spring 77 is contracted, when the half gear 74 is disengaged from the rack seat 76, the rack seat 76 is driven to slide backward on the surface of the guide rod 75 under the expansion of the spring 77, so that the position of the rack seat 76 is reset;

[0083] The top of the supporting seat 72 is fixedly provided with a detection mechanism 8, the detection mechanism 8 comprises a sliding rail 81 fixedly provided on the top of the supporting seat 72, the surface of the sliding rail 81 is slidingly connected with a sliding frame 82, the inner side of the sliding frame 82 is provided with a PH detector 83, the right side of the sliding frame 82 is rotationally connected with a guide wheel 84, the top of the rack seat 76 is fixedly provided with a moving plate 85, the inner side of the moving plate 85 is slidingly connected with the guide wheel 84;

[0084] Please combine Figure 8 and Figure 10 : when the rack seat 76 moves forward, the moving plate 85 is driven to move forward, the moving plate 85 moves forward to drive the guide wheel 84 to slide upward on the inner side of the moving plate 85, the guide wheel 84 slides upward to drive the sliding frame 82 to slide upward on the surface of the sliding rail 81, the sliding frame 82 slides upward to drive the PH detector 83 to move upward, so that the bottom end of the PH detector 83 is disengaged from the sampling bottle 37;

[0085] Further, when the rack seat 76 is reset backward, the moving plate 85 is driven to move backward, so that the guide wheel 84 slides downward on the inner side of the moving plate 85, the guide wheel 84 slides downward to drive the sliding frame 82 to slide downward on the surface of the sliding rail 81, the sliding frame 82 slides downward to drive the PH detector 83 to move downward, so that the position of the PH detector 83 is reset, and the bottom end of the PH detector 83 is reinserted into the sampling bottle 37.

[0086] The back of the inner wall of the sampling box 1 is fixed with a feeding mechanism 9, the feeding mechanism 9 includes a fixed disc 91 fixed to the back of the inner wall of the sampling box 1, the bottom of the fixed disc 91 is fixed with a funnel 92, the surface of the rotating shaft 31 is fixed with a storage disc 93, the bottom of the storage disc 93 is rotatably connected with the top of the fixed disc 91, and the top of the sampling box 1 is communicated with a feeding pipe 94;

[0087] Please refer to Figure 3 and Figure 11 : The stabilizer is fed into the storage disc 93 through the feeding pipe 94, when the driving motor 38 drives the rotating shaft 31 to rotate clockwise by 90 degrees, the rotating shaft 31 will simultaneously drive the storage disc 93 to rotate by 90 degrees, so that the through hole in the storage disc 93 coincides with the funnel 92, and the stabilizer in the storage disc 93 falls into the sampling bottle 37 through the funnel 92;

[0088] Preferably, four through holes are arranged in the storage disc 93 for storing stabilizers, when the driving motor 38 drives the rotating disc 32 to rotate clockwise by 90 degrees intermittently, the positions of the four sampling bottles 37 are adjusted in sequence, and the stabilizer is fed into the storage disc 93 in sequence, the stabilizer can be fed into the four sampling bottles 37 in sequence under the rotation of the storage disc 93, so that the oxidation or degradation of the flotation collector is avoided, and the accuracy of sampling and detection of lithium ore flotation wastewater is improved.

[0089] In the embodiment, when the driving motor 38 drives the rotating disc 32 to rotate clockwise by 90 degrees intermittently through the rotating shaft 31, the positions of the four sampling bottles 37 are adjusted in sequence, under the action of the driving mechanism 7, the sliding frame 82 drives the PH detector 83 to complete an up-down movement, so that the PH value of the flotation wastewater in each sampling bottle 37 is measured in sequence, and the rotating shaft 31 intermittently rotates to simultaneously drive the storage disc 93 to intermittently rotate, the stabilizer is fed into the storage disc 93 in sequence, and the stabilizer can be fed into the four sampling bottles 37 in sequence under the rotation of the storage disc 93, so that the oxidation or degradation of the flotation collector is avoided.

[0090] Third embodiment:

[0091] Please refer to Figures 1 to 3 and Figure 12 , the bottom end of the rotating shaft 31 is fixed with a mixing mechanism 10, the mixing mechanism 10 includes a mixing shaft 101 fixed to the bottom end of the rotating shaft 31, the surface of the mixing shaft 101 is fixed with two groups of connecting frames 102, the surfaces of the two groups of connecting frames 102 are fixed with mixing frames 103, and the bottom end of the mixing shaft 101 is fixed with mixing paddles 104;

[0092] Please refer to Figure 3 and Figure 12When the rotating shaft 31 rotates, the mixing shaft 101 is driven to rotate, and the mixing shaft 101 drives the mixing frame 103 and the mixing paddle 104 to rotate, so that the sampling water is mixed.

[0093] The bottom of the mixing cylinder 6 is communicated with a discharge pipe 11, the right side of the sampling box 1 is fixedly provided with a controller 12, the front side of the sampling box 1 is rotatably connected with a box door 13, the bottom of the sampling box 1 is fixedly provided with four supporting legs 14, and the mounting seat 21 is fixedly connected with two supporting legs 14 on the front side;

[0094] Preferably, after the layered sampling and mixed sampling of the lithium ore flotation wastewater are completed, the four sampling bottles 37 can be taken out in sequence by opening the box door 13, and the mixed sample can be taken out by opening the discharge pipe 11.

[0095] In the embodiment, when the rotating shaft 31 rotates, the mixing shaft 101 is driven to rotate, and the mixing shaft 101 drives the mixing frame 103 and the mixing paddle 104 to rotate, so that the sampling water is mixed, and the mixed water sample can be stirred during the layered sampling and mixed sampling of the lithium ore flotation wastewater, so that the high-concentration mineral particles in the lithium ore flotation wastewater are prevented from precipitating.

[0096] Please refer to Figures 1 to 12 The working principle of the wastewater detection sampling device for lithium ore flotation provided by the application is as follows:

[0097] Step S1, the device is moved to a lithium ore flotation wastewater pool or a tailing pool, a suction pipe is connected to the surface of the suction pump 23, the height of the suction pipe in the wastewater pool is adjusted, and then the suction pump 23 is started, the suction pump 23 pumps the flotation wastewater into the water inlet pipe 24 through the hose, and the wastewater is pumped into the sampling bottle 37 through the water inlet pipe 24;

[0098] When the sampling bottle 37 contains a certain amount of sampling water, the valve on the surface of the water inlet pipe 24 and the drain pipe 25 is adjusted, the wastewater in the pipeline is discharged through the drain pipe 25, and the suction pipe is adjusted to another height, and the wastewater in other layers is pumped by the suction pump 23.

[0099] Step S2, during the drainage time of the drain pipe 25, the driving motor 38 is started, the driving motor 38 drives the rotating disc 32 to rotate clockwise by 90 degrees through the rotating shaft 31, so as to adjust another sampling bottle 37 to the bottom of the water inlet pipe 24, then the valve on the surface of the water inlet pipe 24 and the drain pipe 25 is adjusted, the flotation wastewater at other heights is pumped into another sampling bottle 37, and the lithium ore flotation wastewater in different layers is pumped into different sampling bottles 37 through the intermittent rotation of the driving motor 38.

[0100] Step S3, when the first sampling bottle 37 completes sampling and rotates 270 degrees clockwise, the electric push rod 41 is started, the electric push rod 41 extends to drive the gear plate 42 to extend to the left, when the gear plate 42 contacts the gear 43, the rotating rod 34, the turnover seat 35, the clamping frame 36 and the sampling bottle 37 are driven to rotate through the gear 43, so that the sampling bottle 37 is tilted, the sampling water in the sampling bottle 37 is overturned, and the sampling water flows into the mixing cylinder 6 through the annular disc 5;

[0101] Through intermittent rotation of the driving motor 38, the four sampling bottles 37 are sequentially sampled and the positions of the four sampling bottles 37 are adjusted. Under the reciprocating working state of the electric push rod 41, the sampling water in the four sampling bottles 37 can be sequentially poured into the mixing cylinder 6, so that the mixed sample of the flotation wastewater is obtained. After the mixed sample is obtained, through cooperation of the driving motor 38 and the suction mechanism 2, the layered sampling of the lithium ore flotation wastewater at different depths can be performed again;

[0102] Step S4, when the rotating disc 32 rotates, the bottom gear disc 71 is simultaneously driven to rotate, the gear disc 71 rotates to drive the passive gear 73 and the half gear 74 to rotate counterclockwise, the half gear 74 rotates to drive the rack seat 76 to slide forward on the surface of the guide rod 75, so that the spring 77 is contracted, and when the half gear 74 is disengaged from the rack seat 76, the rack seat 76 is slid backward on the surface of the guide rod 75 under expansion of the spring 77, so that the position of the rack seat 76 is reset;

[0103] In the reciprocating movement process of the rack seat 76, the moving plate 85 is simultaneously driven to reciprocate, when the rack seat 76 moves forward, the moving plate 85 is simultaneously driven to move forward, the moving plate 85 moves forward to drive the guide wheel 84 to slide upward on the inner side of the moving plate 85, the guide wheel 84 slides upward to drive the sliding frame 82 to slide upward on the surface of the slide rail 81, the sliding frame 82 slides upward to drive the PH detector 83 to move upward, so that the bottom end of the PH detector 83 is disengaged from the sampling bottle 37, when the rack seat 76 is reset backward, the moving plate 85 is simultaneously driven to move backward, and then the guide wheel 84 slides downward on the inner side of the moving plate 85, the guide wheel 84 slides downward to drive the sliding frame 82 to slide downward on the surface of the slide rail 81, the sliding frame 82 slides downward to drive the PH detector 83 to move downward, so that the position of the PH detector 83 is reset, and the bottom end of the PH detector 83 is reinserted into the sampling bottle 37;

[0104] When the driving motor 38 drives the rotating disc 32 to rotate 90 degrees clockwise intermittently through the rotating shaft 31 to adjust the positions of the four sample bottles 37 in turn, the sliding frame 82 drives the PH detector 83 to complete an up-down movement under the action of the driving mechanism 7, so as to measure the PH value of the floatation waste water in each sample bottle 37 in turn;

[0105] When the driving motor 38 drives the rotating disc 32 to rotate 90 degrees clockwise intermittently to adjust the positions of the four sample bottles 37 in turn, the stabilizer is put into the storage disc 93 in turn, and the stabilizer can be put into the four sample bottles 37 in turn under the rotation of the storage disc 93, so as to avoid the oxidation or degradation of the floatation collector;

[0106] When the rotating shaft 31 rotates, the mixing shaft 101 rotates to drive the mixing frame 103 and the mixing paddle 104 to rotate, so as to mix the sample water.

[0107] When the layering sampling and mixed sampling of the lithium ore floatation waste water are completed, the four sample bottles 37 can be taken out in turn by opening the box door 13, and the mixed sample can be taken out by opening the discharge pipe 11. When the mixed sample is taken out, part of the waste water needs to be discharged, and then the mixed sample is taken by the sample bottle 37.

[0108] Please refer to Figure 13 and Figure 14 , the sulfonamide collector includes a compound having the following general chemical structure or a chemical isomer or a salt thereof:

[0109] The core structure is a sulfonamide group (-SO2NH-), and two sides are connected with carbon chains of different lengths to form a structure of "carbon chain-sulfonamide-carbon chain";

[0110] Please refer to Figure 13 : wherein: n, m are any one of 1-10;

[0111] The compound is one of the following compounds:

[0112] JL-173: one side of the sulfonamide group is connected with a straight-chain alkyl group containing 4 carbons, and the other side is connected with a straight-chain alkyl group containing 4 carbons;

[0113] JL-174: one side of the sulfonamide group is connected with a straight-chain alkyl group containing 4 carbons, and the other side is connected with a straight-chain alkyl group containing 6 carbons;

[0114] JL-175: one side of the sulfonamide group is connected with a straight-chain alkyl group containing 6 carbons, and the other side is connected with a straight-chain alkyl group containing 4 carbons;

[0115] JL-176: both sides of the sulfonamide group are connected with straight-chain alkyl groups containing 8 carbons;

[0116] JL-177: sulfonamide group is connected to a straight-chain alkyl group containing 8 carbons on one side and to a straight-chain alkyl group containing 6 carbons on the other side;

[0117] JL-178: sulfonamide group is connected to a straight-chain alkyl group containing 10 carbons on both sides;

[0118] JL-179: sulfonamide group is connected to a straight-chain alkyl group containing 12 carbons on both sides;

[0119] Preferably, different ore samples need to be configured with different collectors, and a lithium mica mixed collector is configured for lithium mica, and the flotation agent includes 50-70% of sulfonamide compound JL-178, 10-45% of amine, 3-18% of fatty acid / salt, 2-9% of alcohol, 0.5-5% of kerosene and 30-70% of deionized water;

[0120] Sulfonamide has good selectivity for spodumene, and can effectively separate spodumene from other gangue minerals to a certain extent. It can preferentially adsorb on the surface of spodumene, and has weak adsorption on other impurity minerals. This is the reason why it can effectively improve the grade of spodumene concentrate. Sulfonamide can also chemically react with active sites on the surface of spodumene to form stable chemical bonds or surface complexes, thereby firmly adsorbing on the surface of spodumene particles and effectively collecting them. Even in the case of low spodumene content, the collecting effect can be well played to improve the recovery rate of spodumene;

[0121] In addition, compared with some traditional collectors, sulfonamide can still maintain good flotation performance at low temperature. When flotation operation is carried out in cold areas or winter, the flotation effect of sulfonamide is less affected by temperature, which can ensure the stability of the flotation process and the relative stability of the index. In the flotation process, the chemical properties of sulfonamide are relatively stable and not easy to decompose to produce harmful substances, which has less pollution to the environment. Moreover, in the wastewater treatment process, it is relatively easy to remove and degrade by some conventional treatment methods, which meets the environmental protection requirements of modern mining;

[0122] Further, the amine includes one or more of dodecylamine, tetradecylamine, hexadecylamine, coconut amine, and dodecyltrimethylammonium chloride;

[0123] Further, the fatty acid / salt includes one or more of oleic acid and its salts, linoleic acid and its salts, and linolenic acid and its salts;

[0124] Further, the alcohol includes one or more of ethanol, propanol, tert-butyl alcohol, and pentanol;

[0125] Further, the kerosene includes one or more of ethanol, propanol, tert-butyl alcohol, and pentanol;

[0126] The present application is described below through specific examples:

[0127] Fourth embodiment:

[0128] The lithium mica ore sample of the present embodiment is detected, and the raw ore Li2O grade is 1.57% (i.e. the content of Li2O in the raw ore is 1.57%). According to the flotation process of lithium mica, the following steps are included:

[0129] According to the same proportion, when the lithium mica flotation reagent is configured, the sulfonamide of the present application is replaced by dodecyl sulfonic acid. The prepared lithium mica collector is subjected to flotation according to the above flotation steps, and finally we obtain lithium mica concentrate;

[0130] The lithium mica concentrate obtained by using the sulfonamide of the present application is dried in an oven overnight, collected and mixed uniformly, and sent for detection. The detection results show that the Li2O grade of the lithium mica concentrate is 5.84%, and the recovery rate reaches 88.0%;

[0131] The lithium mica concentrate obtained by using dodecyl sulfonic acid is dried in an oven overnight, collected and mixed uniformly, and sent for detection. The detection results show that the Li2O grade of the lithium mica concentrate is 4.63%, and the recovery rate reaches 63.7%;

[0132] The concentrate grade obtained by using the sulfonamide lithium mica flotation reagent developed by the present application is improved by 4.27 percentage points compared with the raw ore grade, and the enrichment ratio reaches 3.7;

[0133] The sulfonamide lithium mica flotation reagent of the present application has higher concentrate grade and recovery rate than the lithium mica flotation reagent containing dodecyl sulfonic acid;

[0134] For easy viewing, the following table is made:

[0135]

[0136] Lithium mica ore sample flotation results under different collectors

[0137] Fifth embodiment:

[0138] The water quality is adjusted by bicarbonate, sulfate, chloride, etc.

[0139] The above lithium mica flotation operation is still adopted. Soft water is added to one flotation tank, and hard water is added to the other. Finally, the sulfonamide lithium mica flotation reagent and the lithium mica flotation reagent containing dodecyl sulfonic acid are added respectively, and finally four groups of lithium mica concentrates are obtained;

[0140] In hard water, calcium ions can combine with some groups in sulfonamides to form precipitates, thereby reducing the effective concentration of collectors in water and affecting their collecting performance on minerals. Metal ions in high-hardness water can also be adsorbed on the surface of minerals, changing the properties of the mineral surface. For example, in the flotation of spodumene, calcium and magnesium ions can be adsorbed on the surface of spodumene, changing the surface potential and affecting the interaction between sulfonamide collectors and the surface of spodumene, thereby reducing the adsorption amount and stability of the collector, and thus reducing the concentrate grade and recovery rate, affecting the collecting effect on lithium ore;

[0141] The concentrate grade and recovery rate of the concentrate floated by the sulfonamide flotation reagent of the present application are better than those of dodecyl sulfonic acid collector in soft water and hard water. The main reason is that both the sulfonic acid group and the amino group have lithium ion collecting ability. However, in hard water, calcium and magnesium ions mainly react with negatively charged groups, thereby affecting the performance of the sulfonamide collector. In soft water, there are no impurity ions, which can effectively maintain the stability of the effective components of the collector in water.

[0142] For easy viewing, the following table is prepared:

[0143]

[0144] Flotation results of different collectors and soft and hard water on lepidolite samples

[0145] Sixth embodiment:

[0146] Several large beakers are taken, and in order to eliminate the influence of water quality, the large beakers are filled with pure water by a pure water machine. The above-mentioned lepidolite flotation operation is still adopted, the temperature of the water in different beakers is adjusted by heating or freezing, and then added into the flotation tank. The temperature is 5, 10, 15, 20, 25, 30, and 35 o C. Finally, the sulfonamide collector in the present application is added, and the Li2O recovery rate and grade change under different temperatures are compared;

[0147] For easy viewing, the following table is prepared:

[0148]

[0149] Flotation results of lepidolite samples under different temperatures

[0150] In the low temperature range of 5-10 o C, the sulfonamide collector still exhibits good activity in the lepidolite flotation system. This characteristic makes the flotation effect less affected by temperature fluctuations when carrying out flotation operations in winter, thereby effectively ensuring the stability of the flotation process and the relative stability of various flotation indicators. In the range of 15-25 oThe collecting ability of the collector shows an upward trend in the temperature range of C, which is one of the more suitable flotation temperature ranges. Under this temperature condition, most lithium mica collectors containing sulfonic acid groups can exhibit good collecting performance, and relatively high lithium mica recovery rate and concentrate grade can be obtained, thereby providing favorable temperature condition support for efficient flotation of lithium mica;

[0151] In the temperature range of 25-35 o In the temperature range of C, the collecting ability of the collector shows a downward trend. This is because the increase in temperature will intensify the movement of various ions in the ore pulp, and the competitive adsorption of impurity ions in other ores and the collector on the surface of lithium mica will be enhanced, thereby consuming the sulfonamide collector, reducing the adsorption amount of the collector on the surface of lithium mica, and further reducing the collecting effect;

[0152] In summary, the sulfonamide mixed collector of the present application has higher selectivity, is more resistant to low temperature, and has stronger collecting ability than dodecyl sulfonic acid.

[0153] The preparation method of the sulfonamide-containing collector comprises the following steps:

[0154] S1: Dissolve the sulfuryl chloride derivative A (1.0 equivalent) in dichloromethane (DCM) (0.4 M) in a round-bottom flask, and cool the reaction mixture to 0°C in an ice bath;

[0155] S2: Add the amine derivative B (1.1 equivalent) and Et3N (1.2 equivalent) to the solution under stirring, slowly heat the reaction mixture to room temperature, and continue stirring until the original material is completely consumed by TLC;

[0156] S3: Quench the reaction mixture with 1.0 M HCl, extract the reaction mixture with methyl chloroform three times, wash the combined organic phase with brine, and dry the residue with anhydrous Na2SO4;

[0157] S4: Vacuum concentrate the solution, and finally purify it on a silica gel column with petroleum ether and ethyl acetate to obtain the product C.

[0158] During the vacuum concentration process, the vacuum system needs to be strictly sealed to avoid air leakage affecting the vacuum degree. The equipment should be cleaned immediately after concentration to prevent the residue from solidifying;

[0159] Specifically, the synthesis route of the sulfonamide compound C is as follows:

[0160]

[0161] Further, when the compound A is as shown below:

[0162] ;

[0163] Compound B is as shown below:

[0164] ;

[0165] The sulfonamide compound C produced by the above synthetic route is as shown below:

[0166] ;

[0167] Further, when Compound A is as shown below:

[0168] ;

[0169] Compound B is as shown below:

[0170] ;

[0171] The sulfonamide compound C produced by the above synthetic route is as shown below:

[0172] ;

[0173] Further, when Compound A is as shown below:

[0174] ;

[0175] Compound B is as shown below:

[0176] ;

[0177] The sulfonamide compound C produced by the above synthetic route is as shown below:

[0178] ;

[0179] Further, when Compound A is as shown below:

[0180] ;

[0181] Compound B is as shown below:

[0182] ;

[0183] The sulfonamide compound C produced by the above synthetic route is as shown below:

[0184] ;

[0185] Further, when Compound A is as shown below:

[0186] ;

[0187] Compound B is as shown below:

[0188] ;

[0189] The sulfonamide compound C generated by the above synthetic route is as shown below:

[0190] ;

[0191] Further, when compound A is as shown below:

[0192] ;

[0193] Compound B is as shown below:

[0194] ;

[0195] The sulfonamide compound C generated by the above synthetic route is as shown below:

[0196] ;

[0197] Further, when compound A is as shown below:

[0198] ;

[0199] Compound B is as shown below:

[0200] ;

[0201] The sulfonamide compound C generated by the above synthetic route is as shown below:

[0202] .

[0203] The above merely describes the preferred embodiments of the present application, and is not intended to limit the patent scope of the present application. Any equivalent structural transformation, direct / indirect application in other related technical fields, or the like, made under the concept of the present application, using the content of the present application specification and drawings, are included in the patent protection scope of the present application.

Claims

1. A wastewater sampling device for lithium ore flotation, characterized in that: It includes a sampling box, a suction mechanism, a stratified sampling mechanism and a mixed sampling mechanism; The suction mechanism includes a mounting base provided at the bottom of the sampling box, the inner side of the mounting base is threadedly connected to two threaded support legs, a suction pump is provided on the top of the mounting base, a water inlet pipe is fixed on the inner side of the sampling box, and a drain pipe is connected to the right side of the water inlet pipe; The stratified sampling mechanism includes a rotating shaft vertically connected to the inner side of the sampling box, a rotating disk is fixedly provided at the bottom end of the rotating shaft, two rotating seats are fixedly provided on the top of the rotating disk, the inner sides of the two rotating seats are rotatably connected to rotating rods, the surfaces of the two rotating rods are fixedly provided with flip seats, two clamping frames are fixedly provided on the top of the flip seats, and sampling bottles are provided on opposite sides of the two clamping frames, and a driving motor for driving the rotating shaft to rotate is provided on the top of the sampling box; The mixing sampling mechanism includes an electric push rod fixedly mounted on the inner side of the sampling box, a gear plate fixedly mounted on the output end of the electric push rod, a gear fixedly mounted on the right end of the rotating rod, an annular disk fixedly mounted on the bottom of the inner wall of the sampling box, and a mixing cylinder fixedly mounted on the bottom of the sampling box; The sampling bottles arranged on the top of the rotating disk are arranged in four groups in a circular array along the center of the rotating disk. When the electric push rod drives the gear plate to extend, the gear plate engages with the gear and drives the rotating rod and the flip seat to rotate clockwise through the gear. The bottom of the rotating disk is fixedly provided with a driving mechanism, and the driving mechanism includes a gear disk fixedly provided at the bottom of the rotating disk, a support seat is fixedly provided on the inner side of the left side of the annular disk, the top of the support seat is rotatably connected to a driven gear, the driven gear is meshed with the gear disk, a half gear is fixedly provided on the top of the driven gear, a guide rod is fixedly provided on the inner wall of the sampling box, a rack seat is slidably connected to the surface of the guide rod, the half gear is meshed with the rack seat, and a spring is sleeved on the surface of the guide rod and located on the front side of the rack seat; A detection mechanism is fixedly provided on the top of the support seat, and the detection mechanism includes a slide rail fixedly provided on the top of the support seat, the surface of the slide rail is slidably connected to a sliding frame, a pH detector is provided on the inner side of the sliding frame, the right side of the sliding frame is rotatably connected to a guide wheel, a movable plate is fixedly provided on the top of the rack seat, and the guide wheel is slidably connected to the inner side of the movable plate.

2. The wastewater sampling device for lithium ore flotation according to claim 1, characterized in that: Valves are provided on the surfaces of the water inlet pipe and the drain pipe, and the suction pump is connected to the water inlet pipe through a hose when working.

3. The wastewater sampling device for lithium ore flotation according to claim 1, characterized in that: A delivery mechanism is fixedly provided on the back of the inner wall of the sampling box, and the delivery mechanism includes a fixed plate fixedly provided on the back of the inner wall of the sampling box, a funnel is fixedly provided on the bottom of the fixed plate, a storage plate is fixedly provided on the surface of the rotating shaft, the bottom of the storage plate is rotatably connected to the top of the fixed plate, and the top of the sampling box is connected to a delivery tube.

4. The wastewater sampling device for lithium ore flotation according to claim 1, characterized in that: A mixing mechanism is fixedly provided at the bottom end of the rotating shaft, and the mixing mechanism includes a mixing shaft fixedly provided at the bottom end of the rotating shaft, two sets of connecting frames are fixedly provided on the surface of the mixing shaft, and mixing frames are fixedly provided on the surfaces of the two sets of connecting frames, and a mixing paddle is fixedly provided at the bottom end of the mixing shaft.

5. The wastewater sampling device for lithium ore flotation according to claim 1, characterized in that: The bottom of the mixing cylinder is connected to a discharge pipe, a controller is fixedly provided on the right side of the sampling box, the front side of the sampling box is rotatably connected to a box door, the bottom of the sampling box is fixedly provided with four supporting legs, and the mounting seat is fixedly connected to the two supporting legs on the front side.

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