Device for preparing lithium bicarbonate through continuous carbonization

Abstract

The utility model relates to a device for preparing lithium bicarbonate through continuous carbonization. According to the technical scheme, the lower end of a pulping tank is connected to a side line inlet of a first carbonizer through a pipeline and a first liquid transfer pump, a middle side outlet of the first carbonizer is connected with a side line inlet of a second carbonizer through a pipeline, and a middle side outlet of the second carbonizer is connected with a side line inlet of a third carbonizer through a pipeline; a middle side outlet of the third carbonizer is connected with a side line inlet of a fourth carbonizer through a pipeline, a middle side outlet of the fourth carbonizer is connected to a storage tank through a pipeline and a second liquid transfer pump, and the tops of the four carbonizers are respectively connected to a carbon dioxide recoverer through pipelines. The device has the beneficial effects that liquid sequentially flows through the four carbonizers, carbon dioxide is gasified by the carbon dioxide gasifier and then enters all the carbonizers at the same time, low-pressure safe reaction is achieved, and the reaction rate is high; in addition, excessive carbon dioxide at the top of each carbonizer is effectively compressed and recycled through the carbon dioxide recoverer, so that the loss is reduced.

Description

Technical Field

[0001] The utility model relates to a continuous carbonization device in lithium carbonate purification technology, and particularly relates to a device for continuously carbonizing to prepare lithium bicarbonate. Background Art

[0002] As an important raw material for lithium fluoride, relatively high requirements are placed on its metal ions. High-purity lithium carbonate is required to synthesize battery-grade lithium fluoride that meets the requirements. Currently, the production cost of directly purchasing high-purity lithium carbonate is relatively high. Most enterprises use industrial-grade lithium carbonate to purify to high-purity lithium carbonate. Mainly, a suspension of lithium carbonate and water in a reaction kettle is hydrogenated by introducing carbon dioxide to generate an aqueous solution of lithium bicarbonate. The reaction equation is Li2CO3 + H2O + CO2 == 2LiHCO3. Subsequently, high-purity lithium carbonate is produced through operations such as thermal decomposition and filtration.

[0003] Usually, the kettle reaction increases the conversion rate of lithium bicarbonate by increasing the amount of carbon dioxide introduced or raising the pressure value. Through practical applications, it is known that the kettle batch reaction has the characteristics of low efficiency, high pressure, and high unit consumption. Among them, excessive carbon dioxide is discharged intermittently and cannot form an effective recovery, resulting in waste of resources. At the same time, high pressure also poses uncertain safety risks to production. Based on the above background, a device for continuously carbonizing to prepare lithium bicarbonate needs to be designed. Summary of the Utility Model

[0004] The purpose of the utility model is to provide a device for continuously carbonizing to prepare lithium bicarbonate in view of the above-mentioned defects existing in the prior art. The utility model uses four groups of carbonizers in series, which is a low-pressure safe reaction with a fast reaction rate. At the same time, the surplus carbon dioxide gas is effectively recovered and reused, reducing the loss of carbon dioxide.

[0005] A device for continuously carbonizing to prepare lithium bicarbonate mentioned in the utility model has the following technical solution: It includes a pulping tank, a first transfer pump, a first carbonizer, a second carbonizer, a third carbonizer, a fourth carbonizer, a second transfer pump, a carbon dioxide recovery device, and a storage tank. The lower end of the pulping tank is connected to the side inlet of the first carbonizer through a pipeline and the first transfer pump. The middle side outlet of the first carbonizer is connected to the side inlet of the second carbonizer through a pipeline. The middle side outlet of the second carbonizer is connected to the side inlet of the third carbonizer through a pipeline. The middle side outlet of the third carbonizer is connected to the side inlet of the fourth carbonizer through a pipeline. The middle side outlet of the fourth carbonizer is connected to the storage tank through a pipeline and the second transfer pump. The tops of the first carbonizer, the second carbonizer, the third carbonizer, and the fourth carbonizer are respectively connected to the carbon dioxide recovery device through pipelines.

[0006] Preferably, the outer walls of the above-mentioned first carbonizer, second carbonizer, third carbonizer, and fourth carbonizer are respectively provided with jacket cavities. The bottom of the jacket cavity of the first carbonizer is connected to the first heat exchanger through a pipeline and a first circulation pump. The bottom of the jacket cavity of the second carbonizer is connected to the second heat exchanger through a pipeline and a second circulation pump. The bottom of the jacket cavity of the third carbonizer is connected to the third heat exchanger through a pipeline and a third circulation pump. The bottom of the wall cavity of the fourth carbonizer is connected to the fourth heat exchanger through a pipeline and a fourth circulation pump.

[0007] Preferably, the bottom of the jacket cavity of the above-mentioned first carbonizer is connected to the inlet and outlet of the tube side of the first heat exchanger through a pipeline and a first circulation pump, and the inlet and outlet of the shell side of the first heat exchanger are connected to cooling water.

[0008] Preferably, carbon dioxide distributors are respectively arranged on the lower sides of the above-mentioned first carbonizer, second carbonizer, third carbonizer, and fourth carbonizer.

[0009] Preferably, the output end of the above-mentioned carbon dioxide recovery device is connected to a carbon dioxide storage tank through a compressor.

[0010] Preferably, the above-mentioned first carbonizer includes a carbonizer main body, a jacket cavity, a lower outlet, a feed inlet, an air outlet, a lithium carbonate distributor, and a carbon dioxide inlet. The jacket cavity is arranged on the outer side of the carbonizer main body. The lower end of the carbonizer main body is provided with a lower outlet. The top of the carbonizer main body is provided with an air outlet. The feed inlet is installed on the side line of the carbonizer main body. The lithium carbonate distributor is installed in the upper middle part of the inner cavity of the carbonizer main body and is connected to the feed inlet at one end. A carbon dioxide inlet is arranged on the lower side of the carbonizer main body. The carbon dioxide distributor is located in the lower part of the inner cavity of the carbonizer main body and is connected to the carbon dioxide inlet.

[0011] Preferably, the above-mentioned carbon dioxide distributor includes a lower distribution ring, a middle distribution ring, an upper distribution ring, a connecting pipe, lower spray holes, middle spray holes, and upper spray holes. The lower distribution ring, middle distribution ring, and upper distribution ring are sequentially connected through the connecting pipe. The outer diameter of the lower distribution ring is larger than the outer diameter of the middle distribution ring, and the outer diameter of the middle distribution ring is larger than the outer diameter of the upper distribution ring. A circle of lower spray holes is evenly distributed on the upper surface of the lower distribution ring. A circle of middle spray holes is evenly distributed on the upper surface of the middle distribution ring. A circle of upper spray holes is evenly distributed on the upper surface of the lower distribution ring.

[0012] Preferably, the aperture of the above-mentioned upper spray holes is larger than the aperture of the middle spray holes, and the aperture of the middle spray holes is larger than the aperture of the lower spray holes.

[0013] The beneficial effects of the present utility model are as follows: The present utility model uses centrifugal mother liquor or external condensed water for water replenishment, and slurries and weighs industrial lithium carbonate. After the slurrying is completed, it is sent to four series-connected carbonators through a first transfer pump. The liquid flows through the first carbonator, the second carbonator, the third carbonator, and the fourth carbonator in sequence. Carbon dioxide is gasified through a carbon dioxide gasifier and simultaneously enters each carbonator, where a carbonization reaction occurs to generate lithium bicarbonate. It is a low-pressure safe reaction with a fast reaction rate. Since a carbon dioxide distribution device is provided in the carbonator, it ensures that carbon dioxide is evenly distributed in the tower. The heat released by the carbonization reaction is carried away by the circulating cooling water in the carbonation tower, so that the reaction temperature is controlled at room temperature. In addition, the excess carbon dioxide at the top of each carbonator is effectively compressed and recycled through a carbon dioxide recovery device, reducing losses. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 is a schematic structural diagram of the present utility model;

[0015] Figure 2 is a schematic structural diagram of the first carbonator;

[0016] Figure 3 is a schematic diagram of the carbon dioxide distributor in the top view direction;

[0017] In the above figures: slurrying tank 1, first transfer pump 2, first heat exchanger 3, first carbonator 4, second carbonator 5, third carbonator 6, fourth carbonator 7, second heat exchanger 8, third heat exchanger 9, fourth heat exchanger 10, first circulation pump 11, second circulation pump 12, third circulation pump 13, fourth circulation pump 14, second transfer pump 15, carbon dioxide recovery device 16, storage tank 17, carbon dioxide storage tank 18, compressor 19, carbon dioxide distributor a, carbonator main body 4.1, jacket cavity 4.2, lower outlet 4.3, feed inlet 4.4, gas outlet 4.5, lithium carbonate distributor 4.6, carbon dioxide inlet 4.7, lower distribution ring a1, middle distribution ring a2, upper distribution ring a3, connecting pipe a4, lower spray hole a5, middle spray hole a6, upper spray hole a7. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0018] The following is a description of the preferred embodiments of the present utility model with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only for the purpose of illustrating and explaining the present utility model, and are not used to limit the present utility model.

[0019] Example 1, referring to Figure 1, a lithium bicarbonate continuous carbonization preparation device mentioned in the present utility model includes a pulping tank 1, a first liquid transfer pump 2, a first carbonizer 4, a second carbonizer 5, a third carbonizer 6, a fourth carbonizer 7, a second liquid transfer pump 15, a carbon dioxide recovery device 16, and a storage tank 17. The lower end of the pulping tank 1 is connected to the side inlet of the first carbonizer 4 through a pipeline and the first liquid transfer pump 2. The middle side outlet of the first carbonizer 4 is connected to the side inlet of the second carbonizer 5 through a pipeline. The middle side outlet of the second carbonizer 5 is connected to the side inlet of the third carbonizer 6 through a pipeline. The middle side outlet of the third carbonizer 6 is connected to the side inlet of the fourth carbonizer 7 through a pipeline. The middle side outlet of the fourth carbonizer 7 is connected to the storage tank 17 through a pipeline and the second liquid transfer pump 15. The tops of the first carbonizer 4, the second carbonizer 5, the third carbonizer 6, and the fourth carbonizer 7 are respectively connected to the carbon dioxide recovery device 16 through pipelines.

[0020] Among them, the outer walls of the above-mentioned first carbonizer 4, second carbonizer 5, third carbonizer 6, and fourth carbonizer 7 are respectively provided with jacket cavities 4.2. The bottom of the jacket cavity of the first carbonizer 4 is connected to the first heat exchanger 3 through a pipeline and the first circulation pump 11. The bottom of the jacket cavity of the second carbonizer 5 is connected to the second heat exchanger 8 through a pipeline and the second circulation pump 12. The bottom of the jacket cavity of the third carbonizer 6 is connected to the third heat exchanger 9 through a pipeline and the third circulation pump 13. The bottom of the wall cavity of the fourth carbonizer 7 is connected to the fourth heat exchanger 10 through a pipeline and the fourth circulation pump 14.

[0021] In addition, the bottom of the jacket cavity of the first carbonizer 4 is connected to the inlet and outlet of the tube side of the first heat exchanger 3 through a pipeline and the first circulation pump 11. The inlet and outlet of the shell side of the first heat exchanger 3 are connected to cooling water.

[0022] Furthermore, carbon dioxide distributors a are respectively provided on the lower sides of the above-mentioned first carbonizer 4, second carbonizer 5, third carbonizer 6, and fourth carbonizer 7.

[0023] The output end of the above-mentioned carbon dioxide recovery device 16 is connected to a carbon dioxide storage tank 18 through a compressor 19.

[0024] When the utility model is in use, centrifugal mother liquor or external condensed water is used for water replenishment, and industrial lithium carbonate is slurried and weighed, and then enters the first carbonator 4 through the first transfer pump 2. The slurry concentration is about 4%, the temperature of the first carbonator 4 is greater than 40 °C, the pressure of the first carbonator 4 is normal pressure, the liquid level of the first carbonator 4 is maintained stable, and then it enters the second carbonator 5, the third carbonator 6, and the fourth carbonator 7 in sequence to achieve continuous carbonization. Carbon dioxide is gasified by a carbon dioxide gasifier and then enters each carbonator at the same time, and carbonization reactions occur in each carbonator to generate lithium bicarbonate; a heat exchanger is provided outside each carbonator, and general circulating water is used for cooling to control the reaction temperature to proceed at normal temperature; the lithium bicarbonate solution generated in the carbonator enters the subsequent production steps, and the excessive carbon dioxide at the top is effectively compressed and recovered through the carbon dioxide recovery device 16 and the compressor 19, and then stored in the carbon dioxide storage tank 18 for reuse, reducing the loss of carbon dioxide.

[0025] Embodiment 2, a device for continuously carbonizing to prepare lithium bicarbonate mentioned in the utility model, includes a pulping tank 1, a first transfer pump 2, a first carbonator 4, a second carbonator 5, a third carbonator 6, a fourth carbonator 7, a second transfer pump 15, a carbon dioxide recovery device 16, and a storage tank 17. The lower end of the pulping tank 1 is connected to the side inlet of the first carbonator 4 through a pipeline and the first transfer pump 2. The middle side outlet of the first carbonator 4 is connected to the side inlet of the second carbonator 5 through a pipeline. The middle side outlet of the second carbonator 5 is connected to the side inlet of the third carbonator 6 through a pipeline. The middle side outlet of the third carbonator 6 is connected to the side inlet of the fourth carbonator 7 through a pipeline. The middle side outlet of the fourth carbonator 7 is connected to the storage tank 17 through a pipeline and the second transfer pump 15. The tops of the first carbonator 4, the second carbonator 5, the third carbonator 6, and the fourth carbonator 7 are respectively connected to the carbon dioxide recovery device 16 through pipelines.

[0026] The difference from Embodiment 1 is:

[0027] Refer to Figure 2 , the first carbonator 4 mentioned in this embodiment includes a carbonator main body 4.1, a jacket cavity 4.2, a lower outlet 4.3, a feed inlet 4.4, an air outlet 4.5, a lithium carbonate distributor 4.6, and a carbon dioxide inlet 4.7. A jacket cavity 4.2 is provided outside the carbonator main body 4.1. A lower outlet 4.3 is provided at the lower end of the carbonator main body 4.1. An air outlet 4.5 is provided at the top of the carbonator main body 4.1. A feed inlet 4.4 is installed on the side line of the carbonator main body 4.1. The lithium carbonate distributor 4.6 is installed in the upper middle part of the inner cavity of the carbonator main body 4.1 and is connected to the feed inlet 4.4 at one end. A carbon dioxide inlet 4.7 is provided on the lower side of the carbonator main body 4.1. The carbon dioxide distributor a is located in the lower part of the inner cavity of the carbonator main body 4.1 and is connected to the carbon dioxide inlet 4.7.

[0028] Refer toFigure 3 , the carbon dioxide distributor a mentioned in this embodiment includes a lower distribution ring a1, a middle distribution ring a2, an upper distribution ring a3, a connecting pipe a4, a lower spray hole a5, a middle spray hole a6, and an upper spray hole a7. The lower distribution ring a1, the middle distribution ring a2, and the upper distribution ring a3 are sequentially connected through the connecting pipe a4, and the outer diameter of the lower distribution ring a1 is greater than the outer diameter of the middle distribution ring a2, and the outer diameter of the middle distribution ring a2 is greater than the outer diameter of the upper distribution ring a3. A circle of lower spray holes a5 is evenly distributed on the upper surface of the lower distribution ring a1, a circle of middle spray holes a6 is evenly distributed on the upper surface of the middle distribution ring a2, and a circle of upper spray holes a7 is evenly distributed on the upper surface of the lower distribution ring a1. Among them, the lower distribution ring a1 is connected to the carbon dioxide inlet 4.7 through a connecting pipe, and the carbon dioxide gas is ejected from the spray holes on the lower distribution ring a1, the middle distribution ring a2, and the upper distribution ring a3 in sequence, forming a gradient spray, so that the carbonization reaction is more sufficient.

[0029] Embodiment 3, a continuous carbonization device for preparing lithium bicarbonate mentioned in the present invention includes a pulping tank 1, a first transfer pump 2, a first carbonizer 4, a second carbonizer 5, a third carbonizer 6, a fourth carbonizer 7, a second transfer pump 15, a carbon dioxide recovery device 16, and a storage tank 17. The lower end of the pulping tank 1 is connected to the side inlet of the first carbonizer 4 through a pipeline and the first transfer pump 2. The middle side outlet of the first carbonizer 4 is connected to the side inlet of the second carbonizer 5 through a pipeline. The middle side outlet of the second carbonizer 5 is connected to the side inlet of the third carbonizer 6 through a pipeline. The middle side outlet of the third carbonizer 6 is connected to the side inlet of the fourth carbonizer 7 through a pipeline. The middle side outlet of the fourth carbonizer 7 is connected to the storage tank 17 through a pipeline and the second transfer pump 15. The tops of the first carbonizer 4, the second carbonizer 5, the third carbonizer 6, and the fourth carbonizer 7 are respectively connected to the carbon dioxide recovery device 16 through pipelines.

[0030] The difference from Embodiment 2 is:

[0031] Referring to Figure 3 , the aperture of the upper spray hole a7 mentioned in this embodiment is greater than the aperture of the middle spray hole a6, and the aperture of the middle spray hole a6 is greater than the aperture of the lower spray hole a5. Since the carbon dioxide gas is ejected upward along the lower distribution ring a1, the middle distribution ring a2, and the upper distribution ring a3 in sequence, by setting different apertures, the carbon dioxide gas can react more fully with the lithium carbonate liquid, and the effect is better.

[0032] The above are only the preferred embodiments of the present invention. Any person skilled in the art may modify the present invention by using the technical solutions described above or modify it into an equivalent technical solution. Therefore, any simple modification or equivalent transformation made according to the technical solutions of the present invention falls within the scope of protection required by the present invention.

Claims

1. A continuous carbonization device for preparing lithium bicarbonate, characterized in that: The invention comprises a pulping tank (1), a first liquid transfer pump (2), a first carbonizer (4), a second carbonizer (5), a third carbonizer (6), a fourth carbonizer (7), a second liquid transfer pump (15), a carbon dioxide recovery device (16), and a storage tank (17). The lower end of the pulping tank (1) is connected to the side line inlet of the first carbonizer (4) through a pipeline and the first liquid transfer pump (2). The middle side outlet of the first carbonizer (4) is connected to the side line inlet of the second carbonizer (5) through a pipeline. The middle side outlet of the carbonizer (5) is connected to the side line inlet of the third carbonizer (6) through a pipeline, the middle side outlet of the third carbonizer (6) is connected to the side line inlet of the fourth carbonizer (7) through a pipeline, the middle side outlet of the fourth carbonizer (7) is connected to the storage tank (17) through a pipeline and a second liquid transfer pump (15), and the tops of the first carbonizer (4), the second carbonizer (5), the third carbonizer (6), and the fourth carbonizer (7) are respectively connected to the carbon dioxide recovery device (16) through pipelines.

2. The continuous carbonization device for preparing lithium bicarbonate according to claim 1, characterized in that: The outer walls of the first carbonizer (4), the second carbonizer (5), the third carbonizer (6), and the fourth carbonizer (7) are respectively provided with a sandwich wall cavity; the bottom of the sandwich wall cavity of the first carbonizer (4) is connected to the first heat exchanger (3) via a pipeline and a first circulation pump (11); the bottom of the sandwich wall cavity of the second carbonizer (5) is connected to the second heat exchanger (8) via a pipeline and a second circulation pump (12); the bottom of the sandwich wall cavity of the third carbonizer (6) is connected to the third heat exchanger (9) via a pipeline and a third circulation pump (13); and the bottom of the wall cavity of the fourth carbonizer (7) is connected to the fourth heat exchanger (10) via a pipeline and a fourth circulation pump (14).

3. The continuous carbonization device for preparing lithium bicarbonate according to claim 2, characterized in that: The bottom of the sandwich cavity of the first carbonizer (4) is connected to the tube-side inlet and outlet of the first heat exchanger (3) via a pipeline and a first circulation pump (11), and the shell-side inlet and outlet of the first heat exchanger (3) are connected to cooling water.

4. The continuous carbonization device for preparing lithium bicarbonate according to claim 3, characterized in that: A carbon dioxide distributor (a) is provided on the lower side of each of the first carbonizer (4), the second carbonizer (5), the third carbonizer (6), and the fourth carbonizer (7).

5. The continuous carbonization device for preparing lithium bicarbonate according to claim 4, characterized in that: The output end of the carbon dioxide recovery device (16) is connected to the carbon dioxide storage tank (18) via a compressor (19).

6. The continuous carbonization device for preparing lithium bicarbonate according to claim 1, characterized in that: The first carbonizer (4) comprises a carbonizer body (4.1), a wall cavity (4.2), a lower outlet (4.3), a feed port (4.4), an air outlet (4.5), a lithium carbonate distributor (4.6), and a carbon dioxide inlet (4.7). The wall cavity (4.2) is provided on the outside of the carbonizer body (4.1), the lower end of the carbonizer body (4.1) is provided with a lower outlet (4.3), the top of the carbonizer body (4.1) is provided with an air outlet (4.5), the feed port (4.4) is installed on the side line of the carbonizer body (4.1), the lithium carbonate distributor (4.6) is installed in the middle and upper part of the inner cavity of the carbonizer body (4.1), and one end is connected to the feed port (4.4), the carbon dioxide inlet (4.7) is provided on the lower side of the carbonizer body (4.1), and the carbon dioxide distributor (a) is located in the lower part of the inner cavity of the carbonizer body (4.1) and is connected to the carbon dioxide inlet (4.7).

7. The continuous carbonization device for preparing lithium bicarbonate according to claim 6, characterized in that: The carbon dioxide distributor (a) comprises a lower distribution ring (a1), a middle distribution ring (a2), an upper distribution ring (a3), a connecting pipe (a4), a lower jet hole (a5), a middle jet hole (a6), and an upper jet hole (a7). The lower distribution ring (a1), the middle distribution ring (a2), and the upper distribution ring (a3) ​​are connected in sequence through the connecting pipe (a4), and the outer diameter of the lower distribution ring (a1) is greater than the outer diameter of the middle distribution ring (a2), and the outer diameter of the middle distribution ring (a2) is greater than the outer diameter of the upper distribution ring (a3). A circle of lower jet holes (a5) is evenly distributed on the upper surface of the lower distribution ring (a1), a circle of middle jet holes (a6) is evenly distributed on the upper surface of the middle distribution ring (a2), and a circle of upper jet holes (a7) is evenly distributed on the upper surface of the lower distribution ring (a1).

8. The device for preparing lithium bicarbonate by continuous carbonization according to claim 7, characterized in that: The aperture of the upper jet hole (a7) is larger than the aperture of the middle jet hole (a6), and the aperture of the middle jet hole (a6) is larger than the aperture of the lower jet hole (a5).

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