Preparation process of fine tailing flocculant

Abstract

The preparation process comprises the following steps: S1, mixing polymeric alumina and polysilicic acid according to a mass ratio of 3: 1, adding a silane coupling agent, and stirring in a water bath at 50-80 DEG C; s2, preparing an aqueous solution with the concentration of 0.1-0.3% from anionic polyacrylamide powder with high molecular weight and anionic polyacrylamide powder with low molecular weight according to the mass ratio of 7: 3, and adding alcohol to accelerate dissolution; s3, adding glutaraldehyde into the organic solution obtained in S2, uniformly stirring, transferring into a reaction kettle, cooling to 5-10 DEG C, stirring for 10 minutes at a low speed, increasing the temperature of the reaction kettle from 5-10 DEG C to room temperature at a rate of 1 DEG C / minute, and finally adding 0.1 mol / L hydrochloric acid to adjust the pH value to 6-7; and S4, mixing and stirring the inorganic intermediate and the organic solution according to a mass ratio of (3-5): 1. The flocculating agent prepared from the anionic polyacrylamide powder with high molecular weight and the anionic polyacrylamide powder with low molecular weight by the process has the advantages that the fine particle capture rate, the settling speed, the anti-interference capability and the composite structure stability are improved, and the use cost is reduced to some extent.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of tailings treatment, and particularly relates to a preparation process of fine tailings flocculant. BACKGROUND

[0002] The flocculant plays a crucial role in the tailings treatment in the field of gold mining and mineral processing, especially for fine tailings which are difficult to settle. The efficient flocculant not only can accelerate the solid-liquid separation and improve the utilization rate of return water, but also can reduce the land occupation area of tailings pond and the risk of environmental pollution.

[0003] The existing single 800 million-1200 million molecular weight anionic or cationic PAM is configured as a flocculant, and a small number of scenarios (such as high-concentration sludge dewatering) use 1500 million-2000 million ultra-high molecular weight PAM. The selection basis is the traditional cognition that "the higher the molecular weight, the stronger the bridging ability" - long-chain molecules can connect suspended particles into large flocs through adsorption and bridging effect to improve the settling speed.

[0004] The single molecular weight PAM has the following problems when configuring the flocculant:

[0005] 1. High molecular weight PAM forms "hollow fluffy" flocs (porosity > 40%, density 1.1-1.2 g / cm³), and low molecular weight forms "small and loose" flocs, both of which have slow settling speed (< 15 m / h);

[0006] 2. Single high molecular weight PAM (such as 800 million-1200 million): its long-chain bridging ability is strong, but the molecular chain is easy to entangle and agglomerate, has poor dispersibility, cannot penetrate the gap between fine tailings (particle size < 20 μm), and the fine particle capture rate is < 70%;

[0007] Single low molecular weight PAM (such as 400 million-600 million): good dispersibility but weak bridging ability, small and loose flocs (particle size < 0.6 mm);

[0008] 3. Low exposure rate of active groups, sensitive to salt concentration and pH fluctuation;

[0009] Therefore, the present application provides a preparation process of fine tailings flocculant to meet the needs. SUMMARY

[0010] The present application aims to provide a preparation process of fine tailings flocculant to solve the technical problems raised in the above background.

[0011] To achieve the above-mentioned purpose, the present application provides the following technical solution: a preparation process of fine tailings flocculant, comprising the following steps:

[0012] S1: mixing polyalumina and polysilicic acid with a mass ratio of 3:1, adding silane coupling agent, stirring in a 50~80℃ water bath for 1~2 hours to promote the extension of inorganic polymer chain and surface modification, forming an inorganic intermediate with active groups; pH is controlled at 3~5;

[0013] S2: anionic polyacrylamide powder with a molecular weight of 1400~1600 and anionic polyacrylamide powder with a molecular weight of 400~600 are mixed according to a mass ratio of 7:3 to prepare a water solution with a concentration of 0.1%~0.3%, 5%~8% of the water solution is added to accelerate dissolution, and the concentration of the alcohol is greater than 95%; mechanical stirring is performed for 30 minutes until the solution is completely transparent to form an organic solution;

[0014] S3: 0.05%~0.1% glutaraldehyde is added to the organic solution obtained in S2, and after uniform stirring, it is transferred to a reaction kettle, cooled to 5~10℃, and stirred at low speed for 10 minutes; then the temperature of the reaction kettle is increased from 5~10℃ to room temperature at a rate of 1℃ / min, and the temperature is kept for 20 minutes; finally, 0.1 mol / L hydrochloric acid is added to adjust the pH to 6~7, neutralize the weak alkaline of glutaraldehyde, terminate the crosslinking reaction, and avoid the influence of residual crosslinking agent on the inorganic-organic composite in S4;

[0015] S4: the inorganic intermediate and the organic solution are mixed according to a mass ratio of 3~5:1, and stirred at room temperature with an anchor paddle at a speed of 40~50 rpm for 30~60 minutes to form an inorganic-organic composite structure through hydrogen bonding or electrostatic interaction;

[0016] S5: in S4, first add 0.1%~0.5% titanium acid ester coupling agent and stir for 30 minutes, then add 0.5%~2% calcium peroxide and continue to stir for 30 minutes, then warm up and mature, adjust the pH of the system to 6~7, and mature at 40℃ for 24 hours to improve the stability and storage period of the flocculant.

[0017] As a preferred embodiment in this embodiment, for S2, first add deionized water, then add powder, and stir while adding; after the formation of the stirring vortex, add polyacrylamide powder along the edge of the vortex, and use the shear force of the vortex to preliminarily disperse the powder to reduce agglomeration.

[0018] As a preferred embodiment in this embodiment, in step S2, the filtrate should have no residue by filtering through a 100-mesh sieve screen according to the standard of "completely transparent + no visible particles to the naked eye"; if there are small particles, the stirring time should be extended for 5-10 minutes or a small amount of alcohol should be added to promote dissolution, otherwise the residual particles will cause local over-crosslinking during the subsequent S3 crosslinking, forming rigid agglomerates and reducing the dispersibility of the flocculant.

[0019] As a preferred embodiment in the embodiment, the reactor comprises a heat preservation top cover provided with a stirring system, a heat preservation bottom cover provided with supporting feet and a discharge pipe, a hollow cylinder made of heat conductive material and provided with upper and lower openings, and a cooling part located at the periphery of the hollow cylinder and provided with a condensation cavity in the inner cavity; characterized in that the cooling part comprises a lower annular part and a plurality of upper arc-shaped parts arranged in a circle; the lower annular part and the plurality of upper arc-shaped parts each comprise a heat preservation shell and a heat conductive metal plate; the condensation cavity is located between the heat preservation shell and the heat conductive metal plate; and a heat conductive silica gel layer is mounted on the abutting end of the heat conductive metal plate and the outer wall of the hollow cylinder.

[0020] A first liquid inlet pipe and a first liquid outlet pipe are respectively mounted on each of the plurality of upper arc-shaped parts.

[0021] A second liquid inlet pipe is arranged on the lower annular part, and a second liquid outlet pipe is arranged at a position corresponding to the plurality of upper arc-shaped parts on the lower annular part.

[0022] An upper end of the hollow cylinder is provided with an installation ring made of heat preservation material, and the heat preservation top cover and the upper installation ring are connected by bolts.

[0023] A shielding removal unit is further arranged to drive the plurality of upper arc-shaped parts and the lower annular part to move and completely remove the shielding of the hollow cylinder, so that the hollow cylinder is directly exposed to the air for heating treatment.

[0024] As a preferred embodiment in the embodiment, the shielding removal unit comprises a plurality of driving rods arranged in a circle and a gear ring driven by a driving motor.

[0025] The number of groups of the driving rods is consistent with the number of groups of the upper arc-shaped parts, upper ends and lower ends of the plurality of driving rods are respectively rotationally arranged on corresponding upper installation plates and lower installation plates, the upper installation plates and the lower installation plates are respectively fixedly connected to the installation ring and the supporting feet, and a limiting column is arranged between the upper installation plate and the lower installation plate.

[0026] An upper driving sleeve and a lower driving sleeve are respectively sleeved on the upper end and the lower end of the driving rod, driving blocks are arranged in the inner cavities of the upper driving sleeve and the lower driving sleeve, and end portions of the driving blocks are slidingly arranged in helical grooves arranged on the driving rod.

[0027] The helical grooves of the driving rod from top to bottom are respectively a zone a, a zone b, a zone c, and a zone d, the helical groove of the zone a has a smaller groove spacing than the groove spacing of the zone c, the helical groove of the zone b has a groove spacing not less than the groove spacing of the zone c, and the helical groove of the zone d has a smaller groove spacing than the groove spacing of the zone c.

[0028] The upper driving sleeve and the lower driving sleeve are slidably connected with the limiting column through sliding sleeves, the lower driving sleeve is fixedly connected with the outer wall of the lower annular part through a connecting plate, a penetrating block is installed on the upper driving sleeve, and the penetrating block is penetrated by a penetrating rod, the right end of the penetrating rod is fixedly connected with the outer wall of the corresponding upper arc-shaped part, a roller is rotatably arranged on the left end of the penetrating rod, and the roller is located in a vertical recess arranged on the upper mounting plate, and the vertical recess is connected with an inclined recess arranged below.

[0029] The upper ends of the plurality of driving rods are installed with driving gears which are in engagement with the teeth of the tooth ring, and the tooth ring is rotatably arranged on the upper mounting plate.

[0030] As a preferred embodiment in the embodiment, a close-fitting unit is further arranged to ensure that the close-fitting surface of the upper arc-shaped part is close to the outer wall of the hollow cylinder.

[0031] As a preferred embodiment in the embodiment, the close-fitting unit comprises guide blocks which are circumferentially arranged on the upper and lower ends of the plurality of upper arc-shaped parts and the upper end of the lower annular part, and the guide blocks are arranged in a right-angled trapezoidal structure, and the upper end of the mounting ring and the upper end of the lower annular part are provided with guide insertion grooves which are matched with the guide blocks.

[0032] As a preferred embodiment in the embodiment, the penetrating block and the penetrating rod are both arranged in an inclined manner, and a blocking block is installed on the penetrating rod.

[0033] As a preferred embodiment in the embodiment, L-shaped limiting plates are installed on the plurality of upper mounting plates, and the lower end of the tooth ring is in contact with the bearing parts of the plurality of L-shaped limiting plates, and the bearing parts are provided with ball bearings which are matched with the tooth ring.

[0034] In summary, the technical effects and advantages of the present application are as follows:

[0035] 1. The structure of the present application is reasonable, and compared with the traditional process of single high molecular weight or single low molecular weight anionic polyacrylamide, the flocculant prepared by the process of the present application has improved fine particle capture rate, settling speed, anti-interference ability and composite structure stability, and the use cost is reduced.

[0036] 2. In the present application, the lower annular part, the plurality of upper arc-shaped parts and the shielding removal unit are arranged to drive the plurality of upper arc-shaped parts and the lower annular part to move and completely remove the shielding of the hollow cylinder, so that the hollow cylinder is directly exposed to the air for natural warming treatment. BRIEF DESCRIPTION OF DRAWINGS

[0037] 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 prior art description. Obviously, the drawings in the following description only constitute some embodiments of the present application, and for those skilled in the art, other drawings can also be obtained from these drawings without any creative effort.

[0038] Figure 1 The experimental data table of the present process.

[0039] Figure 2 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4.

[0040] Figure 3 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4. Figure 1 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4.

[0041] Figure 4 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4. Figure 2 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4.

[0042] Figure 5 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4.

[0043] Figure 6 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4. Figure 1 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4.

[0044] Figure 7 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4. Figure 1 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4.

[0045] Figure 8 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4. Figure 4 The schematic diagram of the three-dimensional structure of the reaction kettle of the present application is shown in Figure 4.

[0046] In the figure: 1, heat preservation top cover; 2, hollow cylinder; 3, mounting ring; 4, heat preservation bottom cover; 5, supporting foot; 6, upper arc-shaped part; 61, heat preservation shell; 62, heat-conducting metal plate; 63, heat-conducting silica gel layer; 64, condensation cavity; 7, lower annular part; 8, upper mounting plate; 9, lower mounting plate; 10, limiting column; 11, driving rod; 12, upper driving sleeve; 1201, driving block; 13, lower driving sleeve; 14, sliding sleeve; 15, L-shaped limiting plate; 16, gear ring; 17, driving gear; 18, driving motor; 19, first liquid inlet pipe; 20, first liquid outlet pipe; 21, second liquid inlet pipe; 22, second liquid outlet pipe; 23, through block; 24, through rod; 25, blocking block; 26, roller; 27, vertical groove; 28, inclined groove; 29, guide block; 30, guide plug-in slot. DETAILED DESCRIPTION

[0047] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0048] Example: A preparation process for a fine-grained tailings flocculant, comprising the following steps;

[0049] S1: Mix polyalumina and polysilicic acid at a mass ratio of 3:1, add silane coupling agent, and stir in a water bath at 50~80℃ for 1~2 hours to promote the extension of inorganic polymer chains and surface modification, forming an inorganic intermediate with active groups; control the pH at 3~5.

[0050] Polyalumina and polysilicic acid are mixed at a mass ratio of 3:1. Under acidic conditions of pH 3-5, Al... 3+ With [AlO4Al 12 (OH) 24 (H2O) 12 ] 7+ It exists in the form of high-charge oligomers and forms stable inorganic polymer chains with linear oligomers of polysilicic acid through -Al-O-Si- bonds. The chain length is uniform (the standard deviation of molecular weight distribution is ≤±5%), avoiding agglomeration caused by single Al or Si components (too much Al easily leads to rigid agglomeration, and too much Si easily leads to chain breakage).

[0051] After hydrolysis, silane coupling agents (such as KH550) condense with hydroxyl groups on the surface of inorganic chains, introducing -NH2 active groups (density up to 1.2 × 10⁻⁶). 18 (each g) provides sites for hydrogen bonding / electrostatic binding with the organic phase (PAM) in subsequent S4, ensuring precise matching of the "positively charged core" and "negatively charged network" during inorganic-organic composite formation.

[0052] S2: Prepare an aqueous solution with a concentration of 0.1% to 0.3% by mixing anionic polyacrylamide powder with a molecular weight of 1400 to 1600 and anionic polyacrylamide powder with a molecular weight of 400 to 600 at a mass ratio of 7:3. Add 5% to 8% of the aqueous solution and alcohol with a concentration greater than 95% to accelerate dissolution. Stir mechanically for 30 minutes until completely transparent to form an organic solution.

[0053] 1400~1600 million molecular weight PAM (high molecular weight) provides long chain skeleton (chain length > 1 μm), which can form a large floc skeleton through the "particle-chain-particle" effect; 400~600 million molecular weight PAM (low molecular weight) chain is short and flexible (chain length < 0.5 μm), which can penetrate into the gap between fine tailings (particle size < 20 μm), and the two are compounded in a mass ratio of 7:3, which solves the contradiction of "bridging and dispersion difficult to balance" of single molecular weight, and the fine particle capture rate is increased to more than 90% (single high molecular weight PAM is only 60%~70%);

[0054] 95% high concentration alcohol destroys the hydrogen bond between PAM molecules, accelerates dissolution; mechanical stirring makes PAM molecular chain fully stretch, and the exposure rate of active groups (-COO - , -CONH2) is > 90%, which provides uniform distribution of reaction sites for subsequent S3 crosslinking.

[0055] S3: 0.05%~0.1% glutaraldehyde is added to the organic solution obtained in S2, and after uniform stirring, it is transferred into a reaction kettle, cooled to 5~10℃, and stirred at low speed for 10 minutes, then the temperature of the reaction kettle is increased from 5~10℃ to room temperature at a rate of 1℃ / min, and the temperature is kept for 20 minutes, finally 0.1 mol / L hydrochloric acid is added to adjust the pH to 6~7, neutralize the weak alkaline of glutaraldehyde, and terminate the crosslinking reaction to avoid the influence of residual crosslinking agent on inorganic-organic complex in S4;

[0056] Low temperature (5~10℃) pre-crosslinking inhibits the rapid reaction of glutaraldehyde with PAM, avoiding local over-crosslinking; slowly increase the temperature to room temperature at a rate of 0.5~1℃ / min to form a "uniform and dense + moderate flexible" crosslinking network (crosslinking degree 25%~30%), avoiding the rigid agglomeration (rigid particle content <5%) caused by traditional high temperature crosslinking;

[0057] The uniformly distributed -C=N- bond (Schiff base structure) and the residual -NH2 group in the crosslinking network can form hydrogen bonds and electrostatic interactions with Al-OH and Si-OH of S1 inorganic intermediates, providing "molecular level anchoring sites" for subsequent S4 complex, and the binding energy of the complex structure is increased to 35~40 kJ / mol (single PAM is only 20~25 kJ / mol).

[0058] S4: Inorganic intermediates and organic solvents are mixed in a mass ratio of 3~5:1, stirred at room temperature with anchor paddle at a speed of 40~50 rpm for 30~60 minutes, and inorganic-organic complex structures are formed through hydrogen bonds or electrostatic interactions;

[0059] Inorganic intermediates (positively charged) and organic phases (negatively charged PAM crosslinked networks) are mixed at a mass ratio of 3-5:1 and gently stirred with an anchor paddle (40-50 rpm) to achieve microscopic uniform contact. The positively charged cores and negatively charged networks are connected by hydrogen bonds (-NH2 and Al-OH) and electrostatics (Al... 3+ With -COO - They synergistically combine to form a composite structure of "inorganic core (rigid framework) - organic arms (high and low molecular weight PAM synergy)";

[0060] High molecular weight PAM chains extend to form a large floc skeleton (particle size 1.0~1.3mm), while low molecular weight PAM chains fill the gaps in the skeleton, increasing the floc density (1.3~1.5g / cm³). Fine particles (<20μm) are efficiently captured (capture rate >95%), and the settling velocity reaches 20~25m / h (compared to only 10~15m / h for single PAM). The turbidity of the tailings slurry supernatant is reduced to <20NTU.

[0061] S5: Add 0.1%~0.5% titanate coupling agent to S4 and stir for 30 minutes. Then add 0.5%~2% calcium peroxide and continue stirring for 30 minutes. Heat the mixture to mature, adjust the pH of the system to 6~7, and mature at 40℃ for 24 hours to improve the stability and shelf life of the flocculant.

[0062] Titanate coupling agent (0.1%~0.5%) forms covalent bonds (-Si-O-Ti-OC-) with both the inorganic intermediate's -Si-OH and PAM's -COOH through the -Ti-O- group, improving interfacial compatibility by 40%; calcium peroxide (0.5%~2%) oxidizes PAM segments to generate more -COOH, increasing negative charge density by 25% and enhancing salt resistance (flocculation efficiency decline rate <8% at salinity of 1.0%, and >20% for single PAM);

[0063] Aging at 40℃ for 24 hours promotes the stability of covalent bonds and complete oxidative cross-linking, improves the shear resistance of the composite structure (inorganic particle shedding rate <5%), and extends the storage period to more than 60 days (single PAM <30 days); after the final flocculant is added to the tailings, the moisture content of the filter cake is reduced to 16%~18% (single PAM is 25%~30%), achieving efficient solid-liquid separation.

[0064] Experiments were conducted on this traditional single-molecular-weight flocculant and high- and low-molecular-weight composite flocculants prepared using this process, focusing on their fine particle capture rate, settling velocity, anti-interference ability, and composite structure stability. Data were recorded, and the resulting product was manufactured as follows: Figure 1 The table shown is from Figure 1 As shown in the table, the high and low molecular weight composite flocculants produced using this process all show improvements in fine particle capture rate, sedimentation velocity, anti-interference ability, and composite structure stability.

[0065] As a preferred embodiment in the present embodiment, for S2, the configuration is to add deionized water first and then add the powder, stirring while adding, and after the stirring vortex is formed, add the polyacrylamide powder along the edge of the vortex, use the shear force of the vortex to preliminarily disperse the powder and reduce agglomeration.

[0066] As a preferred embodiment in the present embodiment, in step S2, the filtrate should have no residue by filtering through a 100-mesh screen with the standard of "completely transparent + no visible particles to the naked eye"; if there are small particles, the stirring time needs to be extended for 5-10 minutes or a small amount of alcohol needs to be added to promote dissolution, otherwise the residual particles will cause local over-crosslinking during the subsequent S3 crosslinking, forming rigid agglomerates and reducing the dispersibility of the flocculant.

[0067] Compared with the flocculant configured by a single molecular weight, the flocculant configured by the two high and low molecular weight anionic polyacrylamide powders has the following advantages: 1. The bridging-dispersion synergistic effect is significant, and the fine particle capture rate is improved; 2. The flocculation morphology and settling performance are optimized, and the settling speed is improved; 3. The anti-interference ability is enhanced, and the stability of the composite structure is improved; 4. The use cost is reduced.

[0068] As a preferred embodiment in the present embodiment, as shown in Figures 2-4 and Figure 6 The reaction kettle includes a heat preservation top cover 1 provided with a stirring system, a heat preservation bottom cover 4 provided with supporting feet 5 and a discharge pipe, a hollow cylinder 2 made of heat conductive material and provided with upper and lower openings, and a cooling part located at the periphery of the hollow cylinder 2 and provided with a condensation cavity 64 in the inner cavity; characterized in that: the cooling part is a lower annular part 7 and a plurality of upper arc-shaped parts 6 arranged in a circle; the lower annular part 7 and the plurality of upper arc-shaped parts 6 each include a heat preservation shell 61 and a heat conductive metal plate 62; the condensation cavity 64 is located between the heat preservation shell 61 and the heat conductive metal plate 62; and a heat conductive silica gel layer 63 is installed on the abutting end of the heat conductive metal plate 62 and the outer wall of the hollow cylinder 2.

[0069] A first liquid inlet pipe 19 and a first liquid outlet pipe 20 are respectively installed on each of the plurality of upper arc-shaped parts 6.

[0070] A second liquid inlet pipe 21 and a second liquid outlet pipe 22 are respectively installed on the lower annular part 7.

[0071] The upper end of the hollow cylinder 2 is provided with an installation ring 3 made of heat preservation material, and the heat preservation top cover 1 is connected to the upper installation ring 3 through bolts.

[0072] A shielding removal unit is further provided for driving the plurality of upper arc-shaped parts 6 and the lower annular part 7 to move and completely remove the shielding of the hollow cylinder 2, so that the hollow cylinder 2 is directly exposed to the air for warming treatment.

[0073] In use, the outlet of the industrial water cooler is connected to the second inlet pipe 21, and the second outlet pipe 22 is connected to the first inlet pipe 19 through a connecting hose, and the first outlet pipe 20 is connected to the inlet of the water cooler;

[0074] When natural cooling of the solution in the reaction kettle is required, the shielding release unit can be controlled to work, driving the lower annular part 7 and the upper arc part 6 to move and release the blocking of the hollow cylinder 2, so that the hollow cylinder 2 is completely exposed to the air for rapid natural heat dissipation. After the heat dissipation is completed, the lower annular part 7 and the upper arc part 6 can be controlled to move reversely to restore to the original position.

[0075] It should be noted that: for process S3, direct heating of the solution in the reaction kettle by the electric heating pipe or heating of the condensate water and then heating the solution in the reaction kettle through heat conduction, all can easily form a temperature gradient of "high wall temperature (3~5℃ higher than the center) - low center temperature". The PAM molecular chains near the wall are high in temperature and strong in movement, and are quickly crosslinked with glutaraldehyde to form a local high crosslinking degree area (crosslinking degree >40%), the molecular chains are tightly wound to form rigid agglomerates (lack of flexibility); while the center area lags in temperature rise, the crosslinking degree is only 10%~15%, forming a loose network. Therefore, the disassembly cooling part is adopted to expose the heat conduction layer to the room temperature environment, relying on the natural heat exchange between the environment temperature and the solution in the kettle (5~10℃), the heat transfer rate is naturally controlled by the temperature difference (the actual temperature rise rate ≈0.5~0.8℃ / min, slightly lower than electric heating, but more uniform), the temperature difference of the whole kettle solution is ≤±0.5℃, the PAM molecular chain movement is synchronized in the whole kettle, avoiding local "overheating reaction" or "underheating reaction", and slowly rising temperature makes the PAM molecular chain have sufficient time to gradually stretch from "low temperature crimping state" to "linear stretching state", the active groups (amide groups) are uniformly exposed, the collision frequency with glutaraldehyde is consistent in the whole kettle, forming a uniform network with a crosslinking degree of 25%~30% and a distribution standard deviation of ±3%~5% (no rigid agglomerates, excellent flexibility).

[0076] As a preferred embodiment in the present embodiment, as shown in Figure 4 、 Figure 5 and Figure 8 , the shielding release unit includes a plurality of groups of driving rods 11 arranged circumferentially and a gear ring 16 driven by a driving motor 18;

[0077] The number of groups of driving rods 11 is consistent with the number of groups of upper arc parts 6, the upper and lower ends of the plurality of groups of driving rods 11 are respectively rotationally arranged on the corresponding upper mounting plate 8 and lower mounting plate 9, the upper mounting plate 8 and the lower mounting plate 9 are respectively fixedly connected to the mounting ring 3 and the support leg 5, and a limiting column 10 is installed between the corresponding upper mounting plate 8 and lower mounting plate 9;

[0078] The driving rod 11 is sleeved with an upper driving sleeve 12 and a lower driving sleeve 13 from top to bottom, respectively, and driving blocks 1201 are installed in the inner cavities of the upper driving sleeve 12 and the lower driving sleeve 13; the end portions of the driving blocks 1201 are slidingly arranged in the spiral grooves arranged on the driving rod 11;

[0079] The spiral grooves of the driving rod 11 are divided into a zone a, a zone b, a zone c and a zone d from top to bottom, the upper driving sleeve 12 initially starts in the zone a, the lower driving sleeve 13 initially starts in the zone c, the groove spacing of the spiral groove in the zone a is smaller than the groove spacing of the spiral groove in the zone c, the groove spacing of the spiral groove in the zone b is not smaller than the groove spacing of the spiral groove in the zone c, and the groove spacing of the spiral groove in the zone d is smaller than the groove spacing of the spiral groove in the zone c;

[0080] The upper driving sleeve 12 and the lower driving sleeve 13 are slidingly connected with the limiting column 10 through sliding sleeves 14, the lower driving sleeve 14 is fixedly connected with the outer wall of the lower annular portion 7 through a connecting plate, the upper driving sleeve 12 is installed with a penetrating block 23, the penetrating block 23 is penetrated by a penetrating rod 24, the right end of the penetrating rod 24 is fixedly connected with the outer wall of the corresponding upper arc-shaped portion 6, the left end of the penetrating rod 24 is rotationally arranged with a roller 26, the roller 26 is located in a vertical recess 27 arranged on the upper mounting plate 8, and the vertical recess 27 is connected with an inclined recess 28 located below;

[0081] The upper ends of the driving rods 11 are installed with driving gears 17 which are tooth-connected with the gear ring 16, and the gear ring 16 is rotationally arranged on the upper mounting plate 8.

[0082] When it is needed to naturally cool the solution in the reactor, the driving motor 18 can be controlled to work, and multiple groups of driving rods 11 are driven to rotate simultaneously through the cooperation of the gear ring 16 and the driving gear 17. At this time, the upper driving sleeve 12 and the lower driving sleeve 13 drive the upper arc-shaped part 6 and the lower annular part 7 to move downward, respectively. The upper driving sleeve 12 initially starts in the a area, and the lower driving sleeve 13 initially starts in the c area. Since the groove spacing of the spiral groove in the a area is smaller than the groove spacing in the c area, that is, the moving distance of the upper driving sleeve 12 per unit time is smaller than the distance of the lower driving sleeve 13 per unit time, the distance between the lower end of the upper arc-shaped part 6 and the upper end of the lower annular part 7 can be increased initially. When the roller 26 moves from the vertical groove 27 to the inclined groove 28, the upper arc-shaped part 6 will move transversely outward relative to the lower annular part 7, and finally a transverse gap between the upper arc-shaped part 6 and the lower annular part 7 is generated. When the roller 26 moves out of the inclined groove 28, the transverse gap distance remains unchanged. From the perspective of the top view, at this time, the upper arc-shaped part 6 is located outside the lower annular part 7. When the roller 26 moves out of the inclined groove 28, the upper driving sleeve 12 moves to the b area and moves downward at this time. At this time, the upper driving sleeve 12 will move downward quickly, and the lower driving sleeve 13 will subsequently move to the d area and move slowly, thereby shortening the height difference between the lower end of the upper arc-shaped part 6 and the lower end of the lower annular part 7. Finally, the lower annular part 7 moves below the hollow cylinder 2, and the upper arc-shaped part 6 moves to the periphery of the lower annular part 7, and the upper end of the upper arc-shaped part 6 is flush with the upper end of the lower annular part 7. At this time, the driving motor is controlled to stop working.

[0083] When it is needed to shield the outer wall of the hollow cylinder 2, the driving motor 18 can be controlled to drive the driving rods 11 to rotate reversely, thereby driving the upper arc-shaped part 6 and the lower annular part 7 to move upward, respectively. The roller 26 is in butt joint with the inclined groove 28, moves along the inclined path of the inclined groove 28, and enters the vertical groove 27, thereby finally restoring the original position of each part (i.e., the upper arc-shaped part 6 and the lower annular part 7 are tightly attached to the outer wall of the hollow cylinder 2).

[0084] It should be noted that: first, due to the limited length of the support foot, and the length of the hollow cylinder 2 is longer than the length of the support foot, the cooling part cannot be set as a whole ring structure, which is easy to block part of the hollow cylinder 2, so it is set as a plurality of upper arc-shaped parts 6 and a lower ring-shaped part 7, and after removing the shielding, the upper arc-shaped part 6 is located at the periphery of the lower ring-shaped part 7, which does not block the hollow cylinder 2 and reduces the occupied space; second, the connecting part of the through rod 24 and the upper arc-shaped part 6 is set upward, the connecting plate and the connecting part of the lower ring-shaped part 7 are set downward, the second liquid inlet pipe 21 and the second liquid outlet pipe 22 are set downward on the lower ring-shaped part 7, and the first liquid inlet pipe 19 and the first liquid outlet pipe 20 are set upward on the upper arc-shaped part 6. The position of each component is set so that the upper arc-shaped part 6 has enough falling space, further avoiding the blocking of the hollow cylinder 2 due to the excessive length of the cooling part 6; third, the outer surface of the hollow cylinder 2 is set as a smooth surface.

[0085] As a preferred embodiment in this embodiment, a close-fitting unit is also provided to ensure that the close-fitting surface of the upper arc-shaped part 6 is close to the outer wall of the hollow cylinder 2.

[0086] Due to the provision of the upper arc-shaped part 6, the edge of the upper arc-shaped part 6 cannot be closely fitted with the outer wall of the hollow cylinder 2 during actual fitting, which leads to poor and slow cooling of the internal solution during cooling. Therefore, the close-fitting unit is provided to make the edge of the upper arc-shaped part 6 close to the outer wall of the hollow cylinder 2.

[0087] As a preferred embodiment in this embodiment, as shown in Figure 7 The close-fitting unit includes guide blocks 29 arranged circumferentially on the upper and lower ends of the plurality of upper arc-shaped parts 6 and the upper end of the lower ring-shaped part 7, and the guide blocks 29 are arranged in a right trapezoidal structure. The mounting ring 3 and the upper end of the lower ring-shaped part 7 are provided with guide insertion grooves 30 adapted to the guide blocks 29.

[0088] Since the mounting ring 3 and the lower ring-shaped part 7 are arranged as a whole ring structure, the close-fitting surface of the structure can be closely fitted with the outer wall of the hollow cylinder 1, so the lower ring-shaped part 7 and the mounting ring 3 are used as force receiving members for correcting the edge of the upper arc-shaped part 6.

[0089] When it is needed to remove the blockage to the hollow cylinder 2, the driving rod 11 is driven to rotate by the driving motor 18, and due to the smaller slot interval of the spiral groove in the a area than that in the c area, at the beginning, the upper arc-shaped part 6 and the lower arc-shaped part 7 simultaneously move vertically downward (the roller 26 moves in the vertical groove), and the movement speed of the lower arc-shaped part 7 is greater than that of the upper arc-shaped part 6, the interval between the upper arc-shaped part 6 and the lower arc-shaped part 7 becomes larger, until the guide blocks 29 at the upper and lower ends of the upper arc-shaped part 6 are respectively removed from the corresponding guide insertion grooves 30, at which time the roller 26 enters the inclined groove 28, and the subsequent change of the horizontal displacement of the upper arc-shaped part 6 relative to the lower arc-shaped part 7 occurs.

[0090] When it is needed to remove the blockage to the hollow cylinder 2, the driving rod 11 is driven to rotate by the driving motor 18, and due to the smaller slot interval of the spiral groove in the a area than that in the c area, at the beginning, the upper arc-shaped part 6 and the lower arc-shaped part 7 simultaneously move vertically downward (the roller 26 moves in the vertical groove), and the movement speed of the lower arc-shaped part 7 is greater than that of the upper arc-shaped part 6, the interval between the upper arc-shaped part 6 and the lower arc-shaped part 7 becomes larger, until the guide blocks 29 at the upper and lower ends of the upper arc-shaped part 6 are respectively removed from the corresponding guide insertion grooves 30, at which time the roller 26 enters the inclined groove 28, and the subsequent change of the horizontal displacement of the upper arc-shaped part 6 relative to the lower arc-shaped part 7 occurs.

[0091] As a preferred embodiment in the present embodiment, as shown in Figure 5 The through block 23 and the through rod 24 are both inclined, and the blocking block 25 is installed on the through rod 24.

[0092] When the roller 26 is just removed from the inclined groove 28, the blocking block 25 will be in contact with the through block 23 to form a blockage, at which time the upper arc-shaped part 6 cannot continue to move horizontally outward, and due to the inclination of the through block 23 and the through rod 24, the component force of the gravity of the upper arc-shaped part 7 tends to make the through rod 24 move obliquely downward, so as to ensure that the through block 23 is in close contact with the blocking block 25 in the subsequent process, and prevent the displacement of the upper arc-shaped part 6 from being changed due to external reasons, thereby affecting the subsequent butt joint of the roller 26 and the inclined groove 28.

[0093] As a preferred embodiment in the present embodiment, as shown in Figure 4 A plurality of L-shaped limiting plates 15 are installed on the upper installation plate 8, and the lower end of the tooth ring 16 is in contact with the bearing part of the plurality of L-shaped limiting plates 15, and the bearing part is provided with a ball bearing adapted to the tooth ring 16.

[0094] The plurality of L-shaped limiting plates 15 are used to limit the tooth ring 16, and the ball bearings are used to ensure that the tooth ring 16 rotates well and reduces the friction between the tooth ring 16.

[0095] Finally, it should be noted that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art will appreciate that the technical solutions described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalent features, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A process for the preparation of a fine-grained tailings flocculant, characterized in that, It comprises the following steps: S1: mixing polyaluminum chloride with polysilicic acid at a mass ratio of 3:1, adding silane coupling agent, stirring in a 50-80℃ water bath for 1-2 hours to promote the extension of inorganic polymer chains and surface modification, forming an inorganic intermediate with active groups; pH is controlled at 3-5; S2: anionic polyacrylamide powder with a molecular weight of 1400-1600 and anionic polyacrylamide powder with a molecular weight of 400-600 are mixed at a mass ratio of 7:3 to prepare a 0.1%-0.3% aqueous solution, 5%-8% of the aqueous solution is added to accelerate dissolution, and the concentration is greater than 95%; mechanical stirring for 30 minutes to form a completely transparent organic solution; S3: 0.05%-0.1% glutaraldehyde is added to the organic solution obtained in S2, stirred uniformly, and then transferred to a reaction kettle, cooled to 5-10℃, low-speed stirring for 10 minutes, then the temperature of the reaction kettle is raised from 5-10℃ to room temperature at a rate of 0.5-1℃ / min, and aged for 20 minutes, finally 0.1 mol / L hydrochloric acid is added to adjust the pH to 6-7, neutralize the weak alkaline of glutaraldehyde, terminate the crosslinking reaction, and avoid the influence of residual crosslinking agent on inorganic-organic complex in S4; S4: mixing the inorganic intermediate with the organic solution at a mass ratio of 3-5:1, stirring at room temperature with an anchor paddle at a speed of 40-50 rpm for 30-60 minutes, and forming an inorganic-organic composite structure through hydrogen bonding or electrostatic interaction; S5: in S4, first add 0.1%-0.5% titanium coupling agent and stir for 30 minutes, then add 0.5%-2% calcium peroxide and continue to stir for 30 minutes, then warm up and age, adjust the pH of the system to 6-7, and age at 40℃ for 24 hours to improve the stability and storage period of the flocculant.

2. A process for the preparation of a fine tailings flocculant according to claim 1, characterized in that: In step S2, when configuring, first add deionized water, then add powder, stir while adding, after the formation of stirring vortex, add anionic polyacrylamide powder along the edge of the vortex, use the shear force of the vortex to preliminarily disperse the powder and reduce agglomeration.

3. The process for preparing a fine tailings flocculant according to claim 1, characterized in that: In step S2, the filtrate should be residue-free by filtering through a 100-mesh screen with the standard of "completely transparent + no visible particles"; if there are small particles, the stirring time should be extended for 5-10 minutes or a small amount of alcohol should be added to promote dissolution, otherwise the residual particles will cause local over-crosslinking during the subsequent S3 crosslinking, forming rigid agglomerates and reducing the dispersibility of the flocculant.

4. The preparation process of fine particle tailings flocculant according to claim 1, wherein the reactor comprises a heat preservation top cover (1) provided with a stirring system, a heat preservation bottom cover (4) provided with supporting feet (5) and a discharge pipe, a hollow cylinder (2) made of heat conductive material and provided with upper and lower openings, and a cooling part located at the periphery of the hollow cylinder (2) and provided with a condensation cavity (64) in the inner cavity; characterized in that: The cooling part is a lower annular part (7) and a plurality of upper arc-shaped parts (6) arranged in a circle, the lower annular part (7) and the plurality of upper arc-shaped parts (6) each include a heat preservation shell (61) and a heat conduction metal plate (62), the condensation cavity (64) is located between the heat preservation shell (61) and the heat conduction metal plate (62), and a heat conduction silica gel layer (63) is installed on the abutting end of the heat conduction metal plate (62) and the outer wall of the hollow cylinder (2); A plurality of first liquid inlet pipes (19) and first liquid outlet pipes (20) are installed on the plurality of upper arc-shaped parts (6) respectively; Second liquid outlet pipes (22) are arranged on the lower annular part (7) at positions corresponding to the groups of upper arc-shaped parts (6), and second liquid inlet pipes (21) are arranged on the lower annular part (7); The upper end of the hollow cylinder (2) is provided with an installation ring (3) made of heat-insulating material, and the heat-insulating top cover (1) is connected to the upper installation ring (3) by bolts; A shielding removal unit is further arranged to drive the groups of upper arc-shaped parts (6) and the lower annular part (7) to move and completely remove the shielding of the hollow cylinder (2), so that the hollow cylinder (2) is directly exposed to air for temperature rising treatment.

5. A process for the preparation of a fine tailings flocculant according to claim 4, characterized in that: The shielding removal unit comprises a plurality of groups of driving rods (11) arranged in a circle and a gear ring (16) driven by a driving motor (18); The number of groups of the driving rods (11) is consistent with the number of groups of the upper arc-shaped parts (6), and the upper and lower ends of the groups of driving rods (11) are rotatably arranged on corresponding upper and lower installation plates (8) and (9), respectively, which are fixedly connected to the installation ring (3) and the supporting leg (5), respectively, and a limiting column (10) is arranged between the upper and lower installation plates (8) and (9). An upper driving sleeve (12) and a lower driving sleeve (13) are arranged on the driving rod (11) in a sleeved manner from top to bottom, respectively, and a driving block (1201) is arranged in the inner cavity of each of the upper and lower driving sleeves (12) and (13). The spiral groove of the driving rod (11) comprises a zone a, a zone b, a zone c and a zone d from top to bottom, the upper driving sleeve (12) is initially arranged in the zone a, the lower driving sleeve (13) is initially arranged in the zone c, the slot interval of the spiral groove of the zone a is smaller than that of the zone c, the slot interval of the spiral groove of the zone b is not smaller than that of the zone c, and the slot interval of the spiral groove of the zone d is smaller than that of the zone c. The upper and lower driving sleeves (12) and (13) are slidably connected to the limiting column (10) through a sliding sleeve (14), the lower driving sleeve (14) is fixedly connected to the outer wall of the lower annular part (7) through a connecting plate, a penetrating block (23) is arranged on the upper driving sleeve (12), the penetrating block (23) is penetrated by a penetrating rod (24), the right end of the penetrating rod (24) is fixedly connected to the outer wall of the corresponding upper arc-shaped part (6), a roller (26) is rotatably arranged on the left end of the penetrating rod (24), the roller (26) is located in a vertical recess (27) arranged on the upper installation plate (8), and the vertical recess (27) is connected to an inclined recess (28) located below. The upper end of each of the groups of driving rods (11) is provided with a driving gear (17) engaged with the gear ring (16), and the gear ring (16) is rotatably arranged on the upper installation plate (8).

6. A process for the preparation of a fine tailings flocculant according to claim 5, characterized in that: A close-fitting unit is further arranged to ensure that the close-fitting surface of the upper arc-shaped part (6) is closely fitted to the outer wall of the hollow cylinder (2).

7. A process for the preparation of a fine tailings flocculant according to claim 6, characterized in that: The close-fitting unit comprises guide blocks (29) circumferentially arranged on the upper ends of the groups of upper arc-shaped parts (6) and the upper end of the lower annular part (7), and the guide blocks (29) are arranged in a right-angled trapezoidal structure, and the mounting ring (3) and the upper end of the lower annular part (7) are both provided with guide insertion grooves (30) matched with the guide blocks (29).

8. A process for the preparation of a fine tailings flocculant according to claim 5, characterized by: The through block (23) and the through rod (24) are both arranged obliquely, and the through rod (24) is provided with a blocking block (25).

9. The process for the preparation of a fine tailings flocculant according to claim 5, characterized in that: A plurality of groups of the upper mounting plates (8) are all provided with L-shaped limiting plates (15), and the lower end of the tooth ring (16) is in contact with the bearing portions of the plurality of groups of the L-shaped limiting plates (15), and the bearing portions are provided with balls matched with the tooth ring (16).

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