Separation device for boron removal and purification of lithium-containing brine

Abstract

The utility model is applicable to the technical field of product fluid separation, and provides a separation device for boron removal and purification of lithium-containing brine, which comprises a continuous fluid separation component, 30 separation units are arranged in the continuous fluid separation component, are sequentially arranged at intervals according to sequence numbers and are connected in series through a pipeline, and the continuous fluid separation component is connected with the continuous fluid separation component through a pipeline. The separation units are elution pipes, each separation unit is filled with ion exchange resin, and the continuous fluid separation assembly is sequentially divided into a material washing area, an air pressure material area, a feeding area, a thinner feeding area, a reverse top water area, a water washing alkali area, an alkali regeneration area, an alkali pre-regeneration area, a water washing acid area, an acid regeneration area and an acid pre-regeneration area from the initial end to the tail end. According to the scheme, procedures are integrated, meanwhile, the production efficiency is improved, and the production period is shortened; errors caused by manual operation are reduced; and continuous operation and continuous discharging can be realized, so that the efficiency is greatly improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of product fluid separation, and particularly relates to a separation device for removing boron and purifying lithium-containing brine. Background Technique

[0002] Lithium, as an important raw material for lithium batteries, is being developed by various countries. Lithium mainly comes from salt lake brine, which generally contains elements such as calcium, magnesium, boron, and lithium. Therefore, in the process of lithium extraction, boron removal is particularly important.

[0003] In the existing lithium extraction and boron removal process for lithium-containing brine, there are still many manual operation steps, and the obtained product has low purity, low yield, and high cost. Summary of the Utility Model

[0004] The purpose of the utility model is to provide a separation device for removing boron and purifying lithium-containing brine to solve the problems in the above background technique.

[0005] To achieve the above purpose, the utility model provides the following technical solution: A separation device for removing boron and purifying lithium-containing brine includes a continuous fluid separation component. The continuous fluid separation component is internally provided with 30 separation units. The 30 separation units are arranged at intervals in sequence according to the serial numbers and are connected in series through pipelines. The separation unit is an elution tube, and each separation unit is filled with ion exchange resin. The continuous fluid separation component is sequentially divided into a washing material area, a pneumatic feeding area, a feeding area, a dilute material feeding area, a backwashing water area, a water washing with alkali area, an alkali regeneration area, an alkali pre-regeneration area, a water washing with acid area, an acid regeneration area, and an acid pre-regeneration area from the initial end to the end.

[0006] Preferably, the washing material area includes 4 separation units and feeds in series in the forward direction; the pneumatic feeding area includes 1 separation unit and feeds in the forward direction.

[0007] Preferably, the feeding area contains 4 separation units and feeds in parallel in the forward direction; the dilute material feeding area contains 6 separation units and is divided into 3 groups, and the 3 groups feed in series in the forward direction at the same time; the backwashing water area contains 2 separation units and feeds in series in the reverse direction.

[0008] Preferably, the water washing with alkali area contains 4 separation units and feeds in series in the forward direction; the alkali regeneration area contains 1 separation unit and feeds in the forward direction; the alkali pre-regeneration area contains 2 separation units and feeds in series in the positive-reverse direction.

[0009] Preferably, the water washing with acid area contains 3 separation units and feeds in series in the forward direction; the acid regeneration area contains 1 separation unit and feeds in the forward direction; the acid pre-regeneration area contains 2 separation units and feeds in series in the positive-reverse direction.

[0010] Preferably, the material washing area, air pressure material area, feeding area, thinner feeding area, reverse top water area, water washing alkali area, alkali regeneration area, alkali pre-regeneration area, water washing acid area, acid regeneration area and acid pre-regeneration area are arranged in sequence along the circumferential direction.

[0011] The utility model has at least the following beneficial effects:

[0012] (1) The utility model provides a separation device for removing boron and purifying lithium-containing brine, integrating processes, improving production efficiency, shortening the production cycle, and reducing errors caused by manual operation;

[0013] (2) The utility model provides a separation device for removing boron and purifying lithium-containing brine, which can operate continuously and discharge materials continuously, greatly improving the efficiency;

[0014] (3) The utility model provides a separation device for removing boron and purifying lithium-containing brine, adopting a continuous fluid separation and purification technology, and having the following advantages:

[0015] ①. Due to continuous operation, the product composition and concentration remain stable, facilitating the matching of downstream processes;

[0016] ②. Due to the improvement of production efficiency, the resin columns, storage tanks and supporting scales are very small, the equipment is compact, easy to install in any position, easy to match with the old production process and equipment, and the floor area is only about one-fourth of the same scale;

[0017] ③. According to the needs of the production process, the rotation speed can be automatically adjusted with the change of the mass and flow rate of the incoming fluid, so it can ensure operation in the best economic state;

[0018] ④. According to the convenience of the production process, the flow direction of the fluid can be connected in a countercurrent or cocurrent manner;

[0019] ⑤. Due to the adoption of multiple separation units, the production method process can be flexibly changed. Description of the Drawings

[0020] Figure 1 It is a schematic diagram of the overall structure of the utility model. Detailed Embodiments

[0021] Next, the technical solutions in the embodiments of the utility model will be clearly and completely described in conjunction with the drawings in the embodiments of the utility model. Obviously, the described embodiments are only a part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the protection scope of the utility model.

[0022] Embodiment

[0023] Please refer to Figure 1 , the present utility model provides a technical solution: a separation device for removing boron and purifying lithium-containing brine, including a continuous fluid separation component. There are 30 separation units built in the continuous fluid separation component, and the 30 separation units are arranged at intervals in sequence according to the serial numbers (as Figure 1 shown), and are connected in series through pipelines. The separation unit is an elution tube, and each separation unit is filled with ion exchange resin. The continuous fluid separation component is sequentially divided into a washing material area, a pneumatic pressure material area, a feeding area, a dilute material feeding area, a reverse water flushing area, a water washing with alkali area, an alkali regeneration area, an alkali pre-regeneration area, a water washing with acid area, an acid regeneration area, and an acid pre-regeneration area from the initial end to the terminal end; the washing material area, the pneumatic pressure material area, the feeding area, the dilute material feeding area, the reverse water flushing area, the water washing with alkali area, the alkali regeneration area, the alkali pre-regeneration area, the water washing with acid area, the acid regeneration area, and the acid pre-regeneration area are arranged in sequence along the circumferential direction.

[0024] Washing material area: It contains 4 separation units, adopts a forward feeding method, uses pure water to wash the resin clean, the washing liquid enters the 5th and 6th separation units in the dilute material feeding area, and the lithium-containing brine between the resins is deboronated again by the resin to obtain the main product deboronated liquid.

[0025] Pneumatic pressure material area: It contains 1 separation unit, adopts a forward feeding method, uses compressed air to press out the material liquid between the resins, the material liquid enters the 5th and 6th separation units in the dilute material feeding area, and the lithium-containing brine between the resins is deboronated again by the resin to obtain the main product deboronated liquid.

[0026] Feeding area: It contains 4 separation units, adopts a 4-group simultaneous forward parallel feeding method, the raw material liquid sequentially passes through the 4 separation units in the feeding area, the borate radical is exchanged and adsorbed onto the resin, the tail liquid enters the 5th and 6th separation units in the dilute material feeding area, and the lithium-containing brine is deboronated again by the resin to obtain the main product deboronated liquid.

[0027] Dilute material feeding area: It contains 6 separation units, is evenly divided into 3 groups, adopts a 3-group simultaneous forward series feeding method, the feeding tail liquid, the pneumatic pressure material liquid, and the water washing material liquid are mixed and pumped into the dilute material area together, and the dilute material is deboronated again by the resin to obtain the main product deboronated liquid.

[0028] Reverse water flushing area: It contains 2 separation units, adopts a reverse series feeding method, the deboronated liquid is pumped into the resin column from the lower part in the reverse direction to eject the pure water between the resins, which is reused as recycled water in other processes.

[0029] Water washing with alkali area: It contains 4 separation units, adopts a forward series feeding method, uses pure water to wash the regeneration reagent alkali liquid on the resin clean, and the outflow liquid enters the recycled alkali tank.

[0030] Alkali regeneration area: It contains 1 separation unit, adopts the forward feeding method, uses sodium hydroxide with a concentration of 1 - 2 mol / L to regenerate the resin with alkali, converts the resin into the hydroxide form, restores the resin performance, and the effluent enters the recycled alkali tank.

[0031] Alkali pre - regeneration area: It contains 2 separation units, adopts the positive - reverse series feeding method, pumps the recycled alkali into the pre - regeneration area, and uses this part of dilute alkali to pre - regenerate the resin to reduce the consumption of alkali solution. The effluent is discharged as wastewater from the system.

[0032] Water washing and acid area: It contains 3 separation units, adopts the forward series feeding method, uses pure water to wash the regeneration reagent hydrochloric acid on the resin clean, and the effluent enters the recycled acid tank.

[0033] Acid regeneration area: It contains 1 separation unit, adopts the forward feeding method, uses hydrochloric acid with a concentration of 1 - 2 mol / L to regenerate the resin with acid, and the effluent enters the recycled acid tank.

[0034] Acid pre - regeneration area: It contains 2 separation units, adopts the positive - reverse series feeding method, pumps the recycled acid into the pre - regeneration area, and uses this part of dilute acid to pre - regenerate the resin to reduce the consumption of hydrochloric acid. The effluent is the by - product boric acid.

[0035] The filling amount of each separation unit in the continuous fluid separation system is 300 - 600 ml. The feeding speed in the washing area is 30 - 50 mL / min, the compressed air pressure in the pneumatic feeding area is 0.3 - 2 bar, the feeding speed in the dilute material feeding area is 100 - 300 mL / min, the feeding speed in the reverse water flushing area is 10 - 30 mL / min, the feeding speed in the water washing and alkali area is 40 - 100 mL / min, the feeding speed in the alkali regeneration area is 20 - 50 mL / min, the feeding speed in the alkali pre - regeneration area is 60 - 150 mL / min, the feeding speed in the water washing and acid area is 20 - 60 mL / min, the feeding speed in the acid regeneration area is 20 - 60 mL / min, and the feeding speed in the acid pre - regeneration area is 40 - 120 mL / min.

[0036] The present utility model adopts the advanced separation method of the continuous fluid separation device, replacing the fixed - bed separation column in the traditional method. The improved production method process is as follows:

[0037] Lithium - containing brine - - raw material tank - - continuous fluid separation device - - boron - removed liquid / boric acid - - enter the downstream process section.

[0038] The specific method is that the lithium-containing brine passes through a continuous fluid separation device filled with ion exchange resin. In the continuous fluid separation unit, the hydroxide ions on the resin are exchanged with the borate ions in the brine, and boron is adsorbed onto the resin, thereby achieving the effect of boron removal from the brine. The resin that has been in use will enter the regeneration zone as the system rotates. After regeneration and rinsing in the regeneration zone, the separation column can continue to operate.

[0039] The continuous fluid separation device technology used in the present utility model realizes each step such as material washing, pneumatic feeding, feeding, dilute material feeding, water washing with alkali, alkali regeneration, alkali pre-regeneration, water washing with acid, acid regeneration, and acid pre-regeneration in the traditional production in a continuous production method, with continuous feeding and continuous product output, completely revolutionizing the traditional fixed bed technology. In the present utility model, during the continuous operation of the continuous fluid separation device and the sequential switching of each fluid distribution valve, each separation unit will pump liquids of different media such as brine, pure water, acid-base reagents, etc. in sequence according to the method design.

[0040] Based on the above technical solutions, the present application provides the following partial implementation cases:

[0041] This implementation case uses ion exchange resin, with a designed processing capacity of 12 L / h. According to the characteristics of the lithium-containing brine itself, the filling amount of each resin is 400 ml. It is divided into the following segmented areas:

[0042] (1) Material washing area (1 - 4#): Water inlet area, with pure water entering in the forward direction, a feeding speed of 40 mL / min. It is necessary to detect the conductivity of the outlet of the 1# resin column before rotation to ensure that the residual brine between the resins is rinsed clean.

[0043] (2) Pneumatic feeding area (5#): Air inlet area, with compressed air entering in the forward direction, a pressure of 0.5 bar.

[0044] (3) Feeding area (6 - 9#): Adopts a parallel forward feeding method with 4 groups, and the total feeding speed is 200 mL / min.

[0045] (4) Dilute material feeding area (10 - 15#): Dilute material feeding area, evenly divided into 2 groups, adopts a series forward feeding method, with a total feeding speed of 240 mL / min. It is necessary to detect the boron content at the outlets of the 14# and 15# before rotation to ensure that the boron content in the boron removal liquid is qualified.

[0046] (5) Reverse water flushing area (16 - 17#): Adopts a reverse feeding method, with a feeding speed of 15 mL / min. The outflow liquid is recycled water. It is necessary to monitor the lithium content of the outflow liquid at the outlet of the 17# to avoid yield loss.

[0047] (6) Water washing and caustic soda area (18 - 21#): Inlet area, pure water is fed in series in the forward direction, the feeding speed is 60 mL / min. It is necessary to detect the conductivity at the outlet of the 18# resin column before transfer to ensure that the sodium hydroxide is thoroughly rinsed.

[0048] (7) Caustic soda regeneration area (22#): The inlet of 22# is 1 mol / L sodium hydroxide, fed in the forward direction, the feeding speed is 40 mL / min. It is necessary to detect the pH at the outlet of the 22# resin column before transfer to ensure that the resin is completely regenerated.

[0049] (8) Caustic soda pre - regeneration area (23 - 24#): Fed in series in the forward - reverse direction, 23# is fed in the forward direction and 24# is fed in the reverse direction, the feeding speed is 100 mL / min. The recycled caustic soda is used to pre - regenerate the resin to save the consumption of caustic soda solution.

[0050] (9) Water washing and hydrochloric acid area (25 - 27#): Inlet area, pure water is fed in the forward direction, the feeding speed is 40 mL / min. It is necessary to detect the conductivity at the outlet of the 25# resin column before transfer to ensure that the hydrochloric acid is thoroughly rinsed.

[0051] (10) Hydrochloric acid regeneration area (28#): The inlet of 28# is 2 mol / L hydrochloric acid, fed in the forward direction, the feeding speed is 40 mL / min. It is necessary to detect the pH at the outlet of the 28# resin column before transfer to ensure that the resin is completely regenerated.

[0052] (11) Hydrochloric acid pre - regeneration area (29 - 30#): Fed in series in the forward - reverse direction, 29# is fed in the forward direction and 30# is fed in the reverse direction, the feeding speed is 80 mL / min. The recycled hydrochloric acid is used to pre - regenerate the resin to save the consumption of caustic soda solution, and the effluent is the by - product boric acid.

[0053] The above implementation cases are tested, and the result analysis is as follows:

[0054] Experimental data record table 1 (treatment capacity 12 L / h)

[0055]

[0056]

[0057] Experimental data record table 2 (treatment capacity 12 L / h)

[0058] 1 Li yield 99.9％ 2 Boron removal rate 96.8％

[0059] The basic principle, main features and advantages of the utility model are shown and described above. For those skilled in the art, it is obvious that the utility model is not limited to the details of the above exemplary embodiments, and the utility model can be implemented in other specific forms without departing from the spirit or basic features of the utility model. Therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the utility model is limited by the attached claims rather than the above description. Therefore, it is intended to include all changes within the meaning and scope of the equivalent elements of the claims in the utility model, and any figure marks in the claims should not be regarded as limiting the claims involved.

[0060] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A separation device for removing boron and purifying lithium-containing brine, characterized in that, It includes a continuous fluid separation component, and there are 30 separation units built in the continuous fluid separation component. The 30 separation units are arranged at intervals in sequence according to the serial numbers and are connected in series through pipelines. The separation unit is an elution tube, and each separation unit is filled with ion exchange resin. The continuous fluid separation component is sequentially divided into a material washing area, a pneumatic feeding area, a feeding area, a dilute material feeding area, a backwashing water area, a water washing and caustic area, a caustic regeneration area, a caustic pre-regeneration area, a water washing and acid area, an acid regeneration area, and an acid pre-regeneration area from the initial end to the terminal end.

2. The separation device for removing boron and purifying lithium-containing brine according to claim 1, characterized in that: The material washing area includes 4 separation units and feeds in series in the forward direction in sequence; the pneumatic feeding area includes 1 separation unit and feeds in the forward direction.

3. The separation device for removing boron and purifying lithium-containing brine according to claim 2, wherein: The feeding area contains 4 separation units and feeds in parallel in the forward direction; the dilute material feeding area contains 6 separation units and is divided into 3 groups, and the 3 groups feed in series in the forward direction at the same time; the backwashing water area contains 2 separation units and feeds in series in the reverse direction.

4. A separation device for boron removal and purification of lithium-containing brine according to claim 3, characterized in that: The water washing and caustic area contains 4 separation units and feeds in series in the forward direction; the caustic regeneration area contains 1 separation unit and feeds in the forward direction; the caustic pre-regeneration area contains 2 separation units and feeds in series in the positive-reverse direction.

5. The separation device for removing boron and purifying lithium-containing brine according to claim 4, wherein: The water washing and acid area contains 3 separation units and feeds in series in the forward direction; the acid regeneration area contains 1 separation unit and feeds in the forward direction; the acid pre-regeneration area contains 2 separation units and feeds in series in the positive-reverse direction.

6. The separation device for removing boron and purifying lithium-containing brine according to claim 5, wherein: The material washing area, the pneumatic feeding area, the feeding area, the dilute material feeding area, the backwashing water area, the water washing and caustic area, the caustic regeneration area, the caustic pre-regeneration area, the water washing and acid area, the acid regeneration area, and the acid pre-regeneration area are arranged in sequence along the circumferential direction.

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