CN114538475B - Potassium chloride production system and production method - Google Patents
Potassium chloride production system and production method Download PDFInfo
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- CN114538475B CN114538475B CN202210270629.2A CN202210270629A CN114538475B CN 114538475 B CN114538475 B CN 114538475B CN 202210270629 A CN202210270629 A CN 202210270629A CN 114538475 B CN114538475 B CN 114538475B
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
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Abstract
The application discloses a potassium chloride production method, which comprises the following steps: feeding carnallite ore pulp serving as a raw material into a reverse flotation device, a cold crystallization device and a first screening device in sequence, and obtaining coarse potassium undersize and coarse potassium oversize after reverse flotation, cold crystallization and screening in sequence; concentrating the coarse potassium undersize in a second concentrating device to obtain a first underflow and a first overflow; washing the first bottom flow for multiple times in a repulping and washing device to obtain potassium chloride; the first overflow is subjected to brine mixing with old brine in a brine mixing device to obtain brine mixing ore pulp, the brine mixing ore pulp is subjected to solid-liquid separation by a first separation device, and the obtained solid phase is sent to a hot melting device to be dissolved and crystallized to obtain potassium chloride. The application takes carnallite ore pulp as raw material, carries out halogen mixing on the first overflow of the byproduct generated by the reverse flotation cold crystallization process, and then provides the first overflow to a hot melting device for continuously producing potassium chloride, thereby realizing cascade production of a plurality of processes in series, improving the yield of the potassium chloride and greatly improving the disposable recovery rate of the carnallite ore.
Description
Technical Field
The application relates to a potassium chloride production system and a production method, in particular to a comprehensive utilization technology of resources.
Background
The Chinese potassium resource widely exists in remote areas such as Qinghai, wherein the Qinghai reserve accounts for more than 50% of the national reserve, the representative resource is a salt lake resource, the salt lake resource mainly comprises a sediment resource and a brine resource, the salt lake brine belongs to a liquid chloride mineral resource and is rich in various components, the salt lake brine is processed by carnallite mineral with rich content to prepare potassium chloride to produce potassium fertilizer, the potassium fertilizer is one of three chemical fertilizers of nitrogen and phosphorus, the potassium element has remarkable effect on the life process in a regulating plant body, the absorption condition of water in the plant body, the synthesis and the transfer of sugar are improved, and the yield and the quality of crops can be effectively improved by using the potassium fertilizer.
There are many processes for producing potash fertilizer by using carnallite raw ore in salt lake brine, and the reverse flotation-cold crystallization process is an advanced process in large-scale production. Raw materials are carnallite raw ores, generally comprise pure carnallite and a certain amount of sodium chloride, and the reverse flotation process during production is as follows: adding a flotation reagent into a saturated flotation medium, selectively increasing the hydrophobicity of the surface of sodium chloride in carnallite raw ore, separating sodium chloride along with foam, leaving the carnallite in ore pulp, dehalogenating to obtain low-sodium carnallite with lower sodium content, then entering the crystallizer to perform a cold crystallization process, adding water to perform decomposition crystallization, controlling the decomposition condition to supersaturate potassium chloride in the solution, using the supersaturation degree of a carnallite decomposition system to enable the crystal particles of the potassium chloride to grow at normal temperature to obtain coarse potassium slurry, and performing the processes of filtering, repulping, washing and the like to obtain finished potassium chloride.
In the process, the recovery rate of potassium chloride is low, usually only 30% -40%, and discharged crude potassium waste liquid contains a large amount of potassium chloride, sodium chloride and other materials, so that the utilization rate of carnallite is reduced. The potassium chloride in the crude potassium waste liquid is recycled through tedding in a salt pan so as to improve the utilization rate of carnallite. However, the salt pan tedding method is long in period, the product obtained after tedding contains more sodium chloride besides potassium chloride, and the flotation process is needed to separate sodium chloride from potassium chloride again, so that only part of potassium chloride is recovered, a large amount of potassium chloride is discharged along with the crude potassium waste liquid, and the utilization rate of carnallite is still low.
Disclosure of Invention
The application aims to provide a potassium chloride production system and a production method, which are used for solving the problem of low utilization rate of carnallite in the existing potassium fertilizer production process.
In order to achieve the above object, the present application provides the following technical solutions: a method for producing potassium chloride, wherein the method for producing potassium chloride comprises the following steps:
the method comprises the steps of firstly (S1) taking carnallite ore pulp as a raw material, sequentially conveying the carnallite ore pulp into a reverse flotation device, a cold crystallization device and a first screening device, and sequentially carrying out reverse flotation, cold crystallization and screening to obtain coarse potassium undersize and coarse potassium oversize;
a second step (S2) of concentrating the coarse potassium undersize product in a second concentrating device to obtain a first underflow and a first overflow;
a third step (S3) of washing the first bottom flow for a plurality of times in a repulping and washing device to obtain potassium chloride;
a fourth step (S4) of adding the old brine into the first overflow in a brine adding device to obtain brine adding ore pulp containing solid-phase potassium chloride and solid-phase sodium chloride;
fifthly, carrying out solid-liquid separation on the halogen-added ore pulp through a first separation device (S5);
a sixth step (S6) of delivering the solid phase obtained after the solid-liquid separation into a hot melting device for dissolution and crystallization to obtain potassium chloride;
the sixth step (S6) includes:
s61, heating the solid phase obtained after solid-liquid separation and a sodium chloride saturated solution to dissolve part of potassium chloride in the solid phase into the potassium chloride saturated solution, and leaving part of sodium chloride in the solid phase;
s62, reducing the temperature of the saturated potassium chloride solution to crystallize and separate out potassium chloride;
s63, separating the crystallized chlorinating agent saturated solution to obtain potassium chloride.
According to one embodiment of the application, in the first step (S1), the coarse potassium oversize is fed to the thermosol device after being crushed by the crushing device.
According to an embodiment of the present application, in the first step (S1), the cold crystallization includes:
the low-sodium carnallite obtained by reverse flotation of carnallite pulp is subjected to solid-liquid separation by a first centrifugal machine, a solid phase is obtained and sent to a first crystallizer for decomposition, and a liquid phase is obtained and sent to a first belt machine for solid-liquid separation;
the solid phase obtained after the solid-liquid separation of the first belt conveyor is sent to a second crystallizer for decomposition;
and delivering the decomposed bottom flows in the first crystallizer and the second crystallizer into a third crystallizer for crystallization to obtain a crystallized bottom flow, and delivering the crystallized bottom flow into the first screening device for screening.
According to one embodiment of the present application, the third step (S3) includes: and performing primary solid-liquid separation on the first bottom through a second centrifugal machine, performing primary repulping washing on the obtained solid phase, performing secondary solid-liquid separation on the washed solid phase through a third centrifugal machine, wherein the obtained solid phase is potassium chloride with the mass fraction of more than 95%, and performing secondary repulping washing on a part of the solid phase to obtain potassium chloride with the mass fraction of more than 98%.
According to one embodiment of the application, the liquid phase obtained by the primary solid-liquid separation and the liquid phase obtained by the secondary solid-liquid separation are concentrated, the obtained bottom flow enters a second belt machine to carry out solid-liquid separation, and the obtained solid phase is potassium chloride with the mass fraction of more than 95%.
The application also provides a potassium chloride production system, wherein the potassium chloride production system comprises:
the reverse flotation device is used for carrying out reverse flotation on carnallite pulp to obtain low-sodium carnallite;
the cold crystallization device is connected with the reverse flotation device and is used for crystallizing the low-sodium carnallite to obtain crystallization underflow;
the first screening device is connected to the back of the cold crystallization device and is used for screening the crystallization underflow to obtain coarse potassium undersize and coarse potassium oversize;
the second concentration device is connected to the rear of the first screening device and is used for concentrating the coarse potassium undersize to obtain a first underflow and a first overflow;
the repulping and washing device is connected with the second concentration device and is used for washing the first underflow for a plurality of times to obtain potassium chloride;
the brine mixing device is connected with the second concentrating device and is used for mixing the first overflow and the old brine to obtain brine mixing ore pulp containing solid-phase potassium chloride and solid-phase sodium chloride;
the first separation device is connected with the brine mixing device and is used for carrying out solid-liquid separation on the brine mixing pulp;
and the hot melting device is connected with the first separation device and is used for dissolving and crystallizing the solid phase obtained after the solid-liquid separation of the brine-blended ore pulp to obtain potassium chloride.
According to one embodiment of the present application, the cold crystallization apparatus includes:
a first centrifuge, connected to the reverse flotation device, for solid-liquid separation of the low sodium carnallite;
a first crystallizer connected to the first centrifuge and used for decomposing the solid phase obtained by the first centrifuge;
the first belt conveyor is connected to the rear of the first centrifugal machine and is used for solid-liquid separation of a liquid phase obtained by the first centrifugal machine;
a second crystallizer connected after the first belt machine and used for decomposing the solid phase obtained by the first belt machine,
and the third crystallizer is respectively connected with the first crystallizer and the second crystallizer and is used for receiving and crystallizing the decomposed underflow in the first crystallizer and the decomposed underflow in the second crystallizer.
According to one embodiment of the application, the potassium chloride production system further comprises a crushing device arranged between the first screening device and the thermosol device for crushing the coarse potassium oversize.
According to one embodiment of the application, the repulping washing apparatus comprises:
the second centrifugal machine is connected with the second concentration device and is used for carrying out primary solid-liquid separation on the first bottom flow;
the first scrubber is connected with the second centrifugal machine and is used for performing first repulping and washing on the solid phase obtained by the first-stage solid-liquid separation;
the third centrifugal machine is connected with the first scrubber and is used for carrying out secondary solid-liquid separation on the liquid phase obtained by the first scrubber;
the second scrubber is connected to the third centrifugal machine and is used for performing second repulping washing on the solid phase obtained by the second-stage solid-liquid separation;
and a fourth centrifugal machine connected with the second scrubber and used for carrying out three-stage solid-liquid separation on the liquid phase obtained by the second scrubber to obtain potassium chloride with the mass fraction of more than 98%.
According to one embodiment of the application, the repulping washing apparatus further comprises:
the first concentrator is respectively connected with the second centrifugal machine, the third centrifugal machine and the fourth centrifugal machine and is used for concentrating a liquid phase obtained by the primary solid-liquid separation, a liquid phase obtained by the secondary solid-liquid separation and a liquid phase obtained by the tertiary solid-liquid separation;
and the second belt machine is connected with the first thickener and then is used for carrying out solid-liquid separation on the bottom flow obtained by the first thickener to obtain potassium chloride with the mass fraction of more than 95%.
Compared with the prior art, the potassium chloride production system and the production method provided by the application have the following advantages:
the application takes carnallite ore pulp as raw material, utilizes reverse flotation cold crystallization process to produce potassium chloride, simultaneously mixes byproduct first overflow (i.e. crude potassium waste liquid) produced by the reverse flotation cold crystallization process with old brine to produce brine pulp containing solid-phase potassium chloride and solid-phase sodium chloride, and then provides the brine pulp to a hot-melting device to dissolve and crystallize to continue producing potassium chloride.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for the purpose of illustrating preferred embodiments and are not to be construed as limiting the application. In the drawings:
FIG. 1 is a flow chart showing the steps of a method for producing potassium chloride according to a preferred embodiment of the present application;
FIG. 2 is a process flow diagram of a preferred embodiment of a method for producing potassium chloride provided by the present application;
FIG. 3 is a process flow diagram of the evaporation of raw halogen in the potassium chloride production process of FIG. 2;
FIG. 4 is a process flow diagram of the preparation of carnallite slurry in the potassium chloride production process of FIG. 2;
FIG. 5 is a process flow diagram of foam concentration in the potassium chloride production process of FIG. 2;
FIG. 6 is a flow chart of a process for cold crystallization in the potassium chloride production process of FIG. 2;
FIG. 7 is a flow chart of a process for concentrating and washing in the potassium chloride production process of FIG. 2;
FIG. 8 is a flow chart of a process for adding halogen and hot-melting in the potassium chloride production method shown in FIG. 2;
FIG. 9 is a flow chart of the process of crushing and thermosol in the process of producing potassium chloride shown in FIG. 2.
Reference numerals:
a reverse flotation device, a 2 cold crystallization device, a 21 first centrifuge, a 22 first crystallizer, a 23 first belt machine, a 24 second crystallizer, a 25 third crystallizer, a 3 first screening device, a 4 second concentration device, a 5 repulping washing device, a 51 second centrifuge, a 52 first washer, a 53 third centrifuge, a 54 second washer, a 55 fourth centrifuge, a 56 first concentration device, a 57 second belt machine, a 6 brine mixing device, a 7 first separation device, an 8 hot melting device, a 81 hot melting device, a 82 vacuum crystallizer, a 83 second separation device, a 9 crushing device, a 10 evaporation device, a 101 sodium salt pond, a 102 first conditioning pond, a 103 first carnallite pond, a 20 first processing device, a 201 raw ore vibrating screen, a 202 second concentration device, a 203 first crusher, a 30 foam concentration device, a 301 third concentration device, a 302 first slurry mixer, a third belt machine, a 304 second conditioning pond, a 305 second carnallite pond, a 306 third carnallite pond, and a 40 first concentration device.
Detailed Description
The application provides many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific examples described in the following embodiments of the present application are merely illustrative of the specific embodiments of the present application and do not constitute a limitation on the scope of the application.
The application is further described below with reference to the drawings and detailed description.
As shown in fig. 1, fig. 1 is a flow chart of steps of a potassium chloride production method according to a preferred embodiment of the present application.
The application provides a potassium chloride production method, which comprises the following steps:
the method comprises the following steps of firstly, S1, sequentially feeding carnallite ore pulp serving as a raw material into a reverse flotation device 1, a cold crystallization device 2 and a first screening device 3, and sequentially carrying out reverse flotation, cold crystallization and screening to obtain coarse potassium undersize and coarse potassium oversize;
a second step S2, concentrating the coarse potassium undersize in a second concentrating device 4 to obtain a first underflow and a first overflow;
step 3, washing the first bottom flow for multiple times in a repulping and washing device 5 to obtain potassium chloride;
step S4, the first overflow is subjected to brine mixing with old brine in a brine mixing device 6 to obtain brine mixing ore pulp containing solid-phase potassium chloride and solid-phase sodium chloride;
s5, carrying out solid-liquid separation on the halogen-added ore pulp through a first separation device 7;
s6, sending the solid phase obtained after solid-liquid separation into a hot melting device 8 for dissolution and crystallization to obtain potassium chloride;
the sixth step S6 includes:
s61, heating the solid phase obtained after solid-liquid separation and a sodium chloride saturated solution to dissolve part of potassium chloride in the solid phase into the potassium chloride saturated solution, and leaving part of sodium chloride in the solid phase;
s62, reducing the temperature of the saturated potassium chloride solution to crystallize and separate out potassium chloride;
s63, separating the crystallized chlorinating agent saturated solution to obtain potassium chloride.
As shown in fig. 1, 2 and 3, fig. 2 is a process flow chart of a potassium chloride production method according to a preferred embodiment of the present application; FIG. 3 is a process flow diagram of the evaporation of raw halogen in the potassium chloride production process of FIG. 2.
In the first step S1, when the carnallite pulp is prepared, raw brine collected in a salt pan collecting area can be selected as a starting raw material, the raw brine enters an evaporation device 10 to be subjected to multistage raw brine evaporation, the evaporation device 10 comprises a sodium salt pond 101, a first regulating pond 102 and a first carnallite pond 103 which are sequentially connected, the raw brine firstly enters the sodium salt pond 101 to be subjected to first tedding evaporation to generate solid-phase potassium salt, brine in the sodium salt pond 101 is discharged to the first regulating pond 102 after being tedded to reach a certain index, the solid-phase potassium salt and the carnallite are subjected to second tedding evaporation to generate the solid-phase potassium salt and the carnallite, brine in the first regulating pond 102 is discharged to the first carnallite pond 103 after being tedded to reach an ore-forming brine point E, the generated solid-phase is carnallite ore, and the ore-forming brine reaches the index of old brine after being tedded in the first carnallite pond 103 and can be discharged as old brine into the next production process. If the old brine is a solution containing more magnesium chloride, namely F point mother solution (magnesium chloride, sodium chloride and carnallite co-saturated solution), the F point mother solution is taken as raw material F brine, and is mixed with the first overflow in the brine mixing device 6, and the potassium chloride in the first overflow can be recovered without adding other substances by utilizing substances in the process, so that the utilization rate of carnallite ore is further improved.
According to one embodiment of the present application, the kalium salt generated in the sodium salt tank 101 and the first adjusting tank 102 are both sent to the first separating device 7 for solid-liquid separation, the obtained liquid phase can be returned to each tank for reuse, the obtained solid phase is sent to the thermosol device 8 for dissolution and crystallization, so as to obtain potassium chloride, and the kalium salt obtained by evaporating the raw halogen is fused with the thermosol process, so that sodium chloride and potassium chloride in the kalium salt can be effectively recovered.
As shown in fig. 2 and 4, fig. 4 is a process flow diagram of the preparation of carnallite pulp in the potassium chloride production process of fig. 2.
According to one embodiment of the present application, when the carnallite pulp is prepared, raw bittern collected in the salt pan collecting area is used as a starting material and enters the evaporation device 10 for multistage evaporation, so as to obtain carnallite ore, and the carnallite ore can be sent to the first treatment device 20 for further preparing the carnallite pulp.
Specifically, the first treatment device 20 includes a raw ore vibrating screen 201, a second thickener 202 connected to the raw ore vibrating screen 201, and a first crusher 203 respectively connected to the raw ore vibrating screen 201 and the second thickener 202, wherein carnallite ore enters the raw ore vibrating screen 201 to perform multistage screening, an upper screen is salt pan sundries, a middle screen is large-particle carnallite, a middle screen oversize enters the first crusher 203, after reaching a flotation requirement, enters the second thickener 202 to perform concentration, a undersize is raw ore, enters the second thickener 202 to perform concentration, and carnallite ore pulp and overflow are obtained, and the overflow can be used for flushing the first crusher 203.
The carnallite pulp is subjected to reverse flotation in the reverse flotation device 1 through a reagent to obtain foam and underflow, wherein the underflow is low-sodium carnallite and is sent to the cold crystallization device 2, and the reverse flotation device 1 is in the prior art and is not described in detail herein.
As shown in fig. 2 and 5, fig. 5 is a process flow diagram of foam concentration in the potassium chloride production process of fig. 2.
The froth obtained by reverse flotation enters a froth concentrating device 30 for froth concentration, the froth concentrating device 30 comprises a third concentrating machine 301, a first pulp mixing machine 302, a third belt machine 303, a second regulating tank 304, a second carnallite tank 305 and a third carnallite tank 306, the third concentrating machine 301, the first pulp mixing machine 302, the third belt machine 303, the second regulating tank 304 and the second carnallite tank 305 are sequentially connected, and the third carnallite tank 306 is connected with the third concentrating machine 301.
Foam enters the third thickener 301 to be concentrated, the concentrated bottom flow returns to the third carnallite pond 306, foam overflowed in the third thickener 301 enters the first pulp mixer 302, fresh water and old brine are added to be stirred, KCl in the foam is diluted to dissolve the KCl into solution as much as possible, slurry enters the third belt conveyor 303 to be subjected to solid-liquid separation, the obtained liquid phase enters the second regulating tank 304 and the second carnallite pond 305 to be continuously evaporated, the obtained solid phase is NaCl waste slag, the NaCl waste slag can enter a drying process, the produced NaCl grade can reach 80% -99%, and the obtained NaCl waste slag is directly packaged and sold.
The first carnallite pond 103, the second carnallite pond 305 and the third carnallite pond 306 may be the same pond or different ponds; the first adjusting tank 102 and the second adjusting tank 304 may be the same tank, may be different tanks, may be the sodium salt tank 101, and are determined according to the composition of the materials in the tanks.
As shown in fig. 5, further, the low sodium carnallite may be concentrated in the first concentrating device 40 to form a concentrated underflow that enters the cold crystallization device 2 to reduce the throughput, and the concentrated overflow may be returned to the reverse flotation device 1 for flushing.
Specifically, the first concentrating device 40 is a thickener, which is a solid-liquid separation device based on gravity sedimentation, and is generally a cylindrical shallow groove with a conical bottom formed by using concrete, wood or metal welding plates as structural materials. The ore pulp with the solid weight of 10-30% can be concentrated into the underflow ore pulp with the solid weight of 30-56% by gravity sedimentation, and the thickened underflow ore pulp is discharged from a bottom flow port at the bottom of the thickener under the action of a rake which is arranged in the thickener and runs slowly, so that cleaner clarified liquid (overflow) is generated at the upper part of the thickener and is discharged from an annular chute at the top. Compared with solid-liquid separation devices such as a clarification tank, the thickener has the advantages of simple structure, low electric energy consumption and good technical indexes, and the separated solid-liquid two phases are naturally discharged from different outlets, so that the operation is convenient.
As shown in fig. 2 and 6, fig. 6 is a process flow chart of cold crystallization in the potassium chloride production method shown in fig. 2.
The cold crystallization apparatus 2 includes: a first centrifuge 21, connected to the reverse flotation device 1, for solid-liquid separation of the low sodium carnallite; a first crystallizer 22 connected to the first centrifuge 21 and configured to decompose a solid phase obtained by the first centrifuge 21; a first belt conveyor 23 connected to the first centrifuge 21 and configured to perform solid-liquid separation of a liquid phase obtained by the first centrifuge 21; a second crystallizer 24 connected to the first belt conveyor 23 and configured to decompose a solid phase obtained by the first belt conveyor 23; and a third crystallizer 25 connected to the first crystallizer 22 and the second crystallizer 24, respectively, for receiving and crystallizing the decomposed underflow in the first crystallizer 22 and the second crystallizer 24.
In the first step S1, the cold crystallization includes: the low-sodium carnallite obtained by reverse flotation of the carnallite ore pulp is subjected to solid-liquid separation by the first centrifugal machine 21, so that a solid phase is obtained and sent to the first crystallizer 22 for decomposition, and a liquid phase is obtained and sent to the first belt machine 23 for solid-liquid separation; the solid phase obtained after the solid-liquid separation of the first belt conveyor 23 is sent to the second crystallizer 24 for decomposition, and the obtained liquid phase is returned to the third carnallite pool 306 for recycling; the bottom flows after decomposition in the first crystallizer 22 and the second crystallizer 24 are sent to a third crystallizer 25 for crystallization, so as to obtain a crystallization bottom flow, the crystallization bottom flow is sent to the first sieving device 3 for sieving, and the crystallization overflows generated in the processes of the first crystallizer 22, the second crystallizer 24 and the third crystallizer 25 can be sent to the first sieving device 3 for flushing.
In the prior art, a set of crystallizer is often used, since the particle size of the low-sodium carnallite is about 0.01-10mm, the low-sodium carnallite contains large particles and small particles, if all the low-sodium carnallite enters one crystallizer for crystallization, a large amount of fresh water needs to be added for dissolution crystallization, a large amount of fresh water and raw materials can be lost, the underflow output of the crystallizer is low, the level difference is high, in the embodiment, the low-sodium carnallite is subjected to solid-liquid separation by the first centrifugal machine 21, the low-sodium carnallite with different particle sizes is subjected to first separation, the low-sodium carnallite with different particle sizes is firstly separated into large particles and small particles, the large-particle low-sodium carnallite enters the first crystallizer 22 for decomposition, the small-particle low-sodium carnallite enters the first belt conveyor 23 for solid-liquid separation again, and the obtained solid phase enters the second crystallizer 24 for decomposition, and the first crystallizer 22 and the second crystallizer 24 are subjected to solid-liquid separation and then jointly conveying the decomposed low-sodium carnallite to the third crystallizer 25 for crystallization. In this embodiment, a conventional set of crystallizers is divided into a first crystallizer 22 and a second crystallizer 24 for decomposing and a third crystallizer 25 for crystallizing, and the low-sodium photo-halogen is decomposed sufficientlyStone, KCl and MgCl dissolved therein 2 The problem of different particle sizes is avoided, and the recovery rate is improved.
The crystallization underflow is sent to the first screening device 3 for screening to obtain coarse potassium undersize and coarse potassium oversize; the first screening device 3 is in particular a vibrating screen. The particles with different particle diameters are separated through the vibrating screen, so that the damage of large particle materials to the screen mesh during centrifugal separation through the centrifugal machine is avoided. The screen mesh size of the first screening device 3 is set according to actual production.
As shown in fig. 2 and 7, fig. 7 is a process flow chart of concentration and washing in the potassium chloride production method shown in fig. 2.
And in the second step S2, the coarse potassium undersize is concentrated in a second concentrating device 4, and a first underflow and a first overflow are obtained after a certain concentration is achieved.
Specifically, the second concentrating device 4 is a thickener, which is a solid-liquid separation device based on gravity sedimentation, and is generally a cylindrical shallow groove with a conical bottom formed by using concrete, wood or metal welding plates as structural materials. The ore pulp with the solid weight of 10-30% can be concentrated into the underflow ore pulp with the solid weight of 30-56% by gravity sedimentation, and the thickened underflow ore pulp is discharged from a bottom flow port at the bottom of the thickener under the action of a rake which is arranged in the thickener and runs slowly, so that cleaner clarified liquid (overflow) is generated at the upper part of the thickener and is discharged from an annular chute at the top. Compared with solid-liquid separation devices such as a clarification tank, the thickener has the advantages of simple structure, low electric energy consumption and good technical indexes, and the separated solid-liquid two phases are naturally discharged from different outlets, so that the operation is convenient.
In the third step S3, the first underflow is washed several times in a repulping and washing device 5 to obtain potassium chloride.
As shown in fig. 7, according to an embodiment of the present application, the repulping washing apparatus 5 includes: a second centrifuge 51 connected to the second concentrating device 4 for performing a first-stage solid-liquid separation on the first underflow; a first scrubber 52 connected to the second centrifuge 51 for performing a first reslurry of the solid phase obtained by the first-stage solid-liquid separation; a third centrifuge 53 connected to the first scrubber 52 for performing a second-stage solid-liquid separation of the liquid phase obtained by the first scrubber 52; a second scrubber 54 connected to the third centrifuge 53 for performing a second repulping and washing of the solid phase obtained by the second solid-liquid separation; and a fourth centrifuge 55 connected to the second scrubber 54, and configured to perform three-stage solid-liquid separation on the liquid phase obtained by the second scrubber 54, thereby obtaining potassium chloride with a mass fraction of 98% or more.
The first bottom flows through the first-stage solid-liquid separation of the second centrifugal machine 51, the obtained solid phase is subjected to first repulping washing in the first washer 52 through a washing solution, the washing solution can be proportioned in advance through fresh water and mother liquor, the first repulping washing is followed by the second-stage solid-liquid separation of the third centrifugal machine 53, the obtained solid phase is potassium chloride with the mass fraction of more than 95%, according to production requirements, the potassium chloride with the mass fraction of more than 95% can be divided into two parts, one part is a potassium chloride finished product with the mass fraction of more than 95%, if the requirement of higher mass fraction exists, the other part of the solid phase is subjected to second repulping washing in the second washer 54, a small amount of washing solution is added, and the washing solution is subjected to third-stage solid-liquid separation of the fourth centrifugal machine 55, so that the potassium chloride with the mass fraction of more than 98% is obtained, and the potassium chloride with different grades is prepared.
The application adjusts the existing primary repulping washing to double repulping washing, on one hand, solves the loss of small-particle-size potassium in the existing primary repulping washing, can also improve the recovery rate of potassium resources, and can also adjust fresh water according to the demands of customers to produce two products with different grades.
According to one embodiment of the application, the repulping washing apparatus 5 further comprises: a first concentrator 56 connected to the second centrifuge 51, the third centrifuge 53, and the fourth centrifuge 55, respectively, for concentrating a liquid phase obtained by the first-stage solid-liquid separation, a liquid phase obtained by the second-stage solid-liquid separation, and a liquid phase obtained by the third-stage solid-liquid separation; and a second belt conveyor 57 connected to the first thickener 56, and configured to perform solid-liquid separation on the underflow obtained by the first thickener 56, thereby obtaining potassium chloride with a mass fraction of 95% or more.
The liquid phase obtained by the first-stage solid-liquid separation, the liquid phase obtained by the second-stage solid-liquid separation, and the liquid phase obtained by the third-stage solid-liquid separation are concentrated by potassium in the first concentrator 56, the obtained concentrated overflow of potassium can be used as mother liquor to return to the first scrubber 52 and the second scrubber 54 for reslurry scrubbing, the obtained underflow enters the second belt conveyor 57 for solid-liquid separation, the obtained solid phase is potassium chloride with a mass fraction of more than 95%, and the obtained liquid phase can be returned to the third crystallizer 25 for use as high-potassium mother liquor for recrystallization.
As shown in fig. 2 and 8, fig. 8 is a process flow chart of adding halogen and hot-melting in the potassium chloride production method shown in fig. 2.
In the fourth step S4, the first overflow is subjected to brine mixing with old brine in the brine mixing device 6 to obtain brine mixing ore pulp containing solid-phase potassium chloride and solid-phase sodium chloride.
The first overflow is used as raw material E halogen, the old halogen is used as raw material F halogen, and the first overflow and the old halogen are mixed in the halogen mixing device 6 and then mixed to obtain halogen mixing pulp containing solid-phase potassium chloride and solid-phase sodium chloride.
Further, the old brine contains 0.28 percent of potassium chloride, 0.26 percent of sodium chloride and more than or equal to 32.4 percent of magnesium chloride, can be prepared from salt lake brine by sun drying, and can also be prepared into saturated solution of sodium chloride, magnesium chloride and carnallite.
The halogen adding principle is as follows: the first overflow is used as raw material E halogen, namely E point mother solution (potassium chloride, sodium chloride and carnallite co-saturated solution), the old halogen is used as raw material F halogen, and is more magnesium chloride-containing solution, namely F point mother solution (magnesium chloride, sodium chloride and carnallite co-saturated solution), the first overflow and the old halogen are mixed, the mixed solution is in a supersaturated state, the magnesium chloride has salting-out effect on the potassium chloride, potassium chloride is separated out firstly, and after the sodium chloride is saturated, the potassium chloride and the sodium chloride are separated out together, so that the formed brine-mixed ore pulp contains solid-phase potassium chloride and solid-phase sodium chloride.
And a fifth step S5, carrying out solid-liquid separation on the brine-blended ore pulp through the first separation device 7.
The solid phase obtained by solid-liquid separation comprises solid-phase potassium chloride and solid-phase sodium chloride, and the obtained liquid phase can be returned to each pool for reuse.
And step S6, sending the solid phase obtained after the solid-liquid separation into the thermosol device 8 for dissolution and crystallization to obtain potassium chloride.
The sixth step S6 includes:
s61, heating the solid phase obtained after solid-liquid separation and a sodium chloride saturated solution to dissolve part of potassium chloride in the solid phase into the potassium chloride saturated solution, and leaving part of sodium chloride in the solid phase;
s62, reducing the temperature of the saturated potassium chloride solution to crystallize and separate out potassium chloride;
s63, separating the crystallized chlorinating agent saturated solution to obtain potassium chloride.
The thermosol device 8 comprises a thermosol device 81, a vacuum crystallizer 82 and a second separation device 83 which are connected in sequence.
The principle of hot melting is as follows: because of the difference in solubility between potassium chloride and sodium chloride at different temperatures, the solubility of sodium chloride is hardly changed with temperature change, while the solubility of potassium chloride is remarkably increased with temperature rise, which is more remarkable when two salts are co-saturated.
Therefore, when the solid phase containing potassium chloride and sodium chloride obtained by the first separation device 7 enters the thermosol 81, high-temperature steam and saturated solution of sodium chloride are introduced, the temperature is heated to 100 ℃, most of the potassium chloride in the solid phase is dissolved into the liquid phase, most of the sodium chloride remains in the solid phase, even if a small part of the sodium chloride is dissolved, the dissolution amount is small, and when the potassium chloride is saturated in the high-temperature solution, the potassium chloride enters the vacuum crystallizer 82, fresh water is added, and vacuum crystallization is performed. Of course, the heating may be carried out to other temperatures, so that most of the potassium chloride is dissolved and most of the sodium chloride remains in the solid phase.
The vacuum crystallization is also called vacuum adiabatic cooling crystallization, which is a crystallization method of flash evaporation and adiabatic cooling of a solution under vacuum, wherein a high-temperature potassium chloride saturated solution is subjected to vacuum flash evaporation in a vacuum crystallizer, so that the temperature of the solution is reduced by flash evaporation, and the potassium chloride is crystallized and separated out after the supersaturation degree is reached, thereby realizing solid-liquid separation of the potassium chloride and mother liquor. By lowering the temperature, most of the potassium chloride crystals are precipitated, and even if sodium chloride is precipitated, the precipitation amount is small.
The underflow obtained after crystallization enters the second separation device 83, the solid phase after solid-liquid separation is more than 95% of potassium chloride, the liquid phase is sodium chloride saturated solution, and the solution returns to the thermosol 81, the vacuum crystallizer 82 and the first carnallite pond 103 for reuse.
Compared with the product obtained by tedding, the product contains potassium chloride and more sodium chloride, the sodium chloride and the potassium chloride in the product still need to be continuously separated through a flotation process, and the sodium chloride and the potassium chloride in the brine-blended ore pulp are separated according to different solubilities by solid-liquid separation-hot-melting crystallization, so that the high-quality potassium chloride is produced, and the step production is realized. Compared with salt field tedding, the production period is shorter, and no additional flotation agent is needed.
As shown in fig. 2 and 9, fig. 9 is a process flow chart of crushing and thermosol in the potassium chloride production method shown in fig. 2.
According to one embodiment of the application, the coarse potassium oversize produced by the first screening device 3 is crushed by the crushing device 9 and then sent to the thermosol device 8, and the coarse potassium oversize is a large-particle low-magnesium high-sodium potassium-containing intermediate product, and the coarse potassium oversize is crushed and thermosol to recycle the intermediate product to produce more than 98% KCl product.
The application also provides a potassium chloride production system, wherein the potassium chloride production system comprises:
the reverse flotation device 1 is used for carrying out reverse flotation on carnallite ore pulp to obtain low-sodium carnallite;
the cold crystallization device 2 is connected with the reverse flotation device 1 and is used for crystallizing the low-sodium carnallite to obtain crystallization underflow;
the first screening device 3 is connected to the cold crystallization device 2 and is used for screening the crystallization underflow to obtain coarse potassium undersize and coarse potassium oversize;
a second concentrating device 4 connected to the first sieving device 3 for concentrating the coarse potassium undersize to obtain a first underflow and a first overflow;
a repulping and washing device 5 which is connected with the second concentration device 4 and is used for washing the first underflow for a plurality of times to obtain potassium chloride;
the brine mixing device 6 is connected with the second concentration device 4 and is used for mixing the first overflow and the old brine to obtain brine mixing ore pulp containing solid-phase potassium chloride and solid-phase sodium chloride;
the first separation device 7 is connected with the brine mixing device 6 and is used for carrying out solid-liquid separation on the brine mixing pulp;
and the hot melting device 8 is connected with the first separation device 7 and is used for dissolving and crystallizing the solid phase obtained after the solid-liquid separation of the brine-blended ore pulp to obtain potassium chloride.
According to one embodiment of the application, the potassium chloride production system further comprises a crushing device 9, said crushing device 9 being arranged between the first screening device 3 and the thermosol device 8 for crushing the coarse potassium oversize.
The devices have been described and explained in detail above in connection with the method, and will not be described again here.
It should be noted that the above-mentioned embodiments illustrate rather than limit the application, and that those skilled in the art will be able to design alternative embodiments without departing from the scope of the appended claims. In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. The word "comprising" does not exclude the presence of elements or steps not listed in a claim.
Claims (8)
1. A method for producing potassium chloride is characterized in that: the potassium chloride production method comprises the following steps:
the method comprises the steps of firstly (S1) taking carnallite ore pulp as a raw material, sequentially conveying the carnallite ore pulp into a reverse flotation device (1), a cold crystallization device (2) and a first screening device (3), and sequentially carrying out reverse flotation, cold crystallization and screening to obtain coarse potassium undersize products and coarse potassium oversize products;
the second step (S2) is to concentrate the coarse potassium undersize in a second concentration device (4) to obtain a first underflow and a first overflow;
the third step (S3) is that the first bottom flow is washed for a plurality of times in a repulping and washing device (5) to obtain potassium chloride;
a fourth step (S4) of carrying out brine mixing on the first overflow and old brine in a brine mixing device (6) to obtain brine mixing ore pulp containing solid-phase potassium chloride and solid-phase sodium chloride;
fifthly, carrying out solid-liquid separation on the halogen-added ore pulp through a first separation device (7);
a sixth step (S6) of delivering the solid phase obtained after the solid-liquid separation into a hot melting device (8) for dissolution and crystallization to obtain potassium chloride;
the sixth step (S6) includes:
s61, heating the solid phase obtained after solid-liquid separation and a sodium chloride saturated solution to dissolve part of potassium chloride in the solid phase into the potassium chloride saturated solution, and leaving part of sodium chloride in the solid phase;
s62, reducing the temperature of the saturated potassium chloride solution to crystallize and separate out potassium chloride;
s63, separating the crystallized chlorinating agent saturated solution to obtain potassium chloride,
in the first step (S1), the cold crystallization includes:
the low-sodium carnallite obtained by reverse flotation of carnallite pulp is subjected to solid-liquid separation by a first centrifugal machine (21), a solid phase is obtained and sent to a first crystallizer (22) for decomposition, and a liquid phase is obtained and sent to a first belt machine (23) for solid-liquid separation;
the solid phase obtained after the solid-liquid separation of the first belt machine (23) is sent to a second crystallizer (24) for decomposition;
and the bottom flows after decomposition in the first crystallizer (22) and the second crystallizer (24) are sent to a third crystallizer (25) for crystallization to obtain crystallization bottom flows, and the crystallization bottom flows are sent to the first screening device (3) for screening.
2. The method for producing potassium chloride according to claim 1, wherein: in the first step (S1), the coarse potassium oversize is crushed by a crushing device (9) and then is sent to the hot melting device (8).
3. The method for producing potassium chloride according to claim 1, wherein: wherein the third step (S3) includes: the first bottom flows through the first-stage solid-liquid separation of the second centrifugal machine (51), the obtained solid phase is subjected to first repulping washing, the washed solid phase is subjected to second-stage solid-liquid separation of the third centrifugal machine (53), the obtained solid phase is potassium chloride with the mass fraction of more than 95%, wherein a part of the solid phase is subjected to second repulping washing, and the washed solid phase is subjected to third-stage solid-liquid separation of the fourth centrifugal machine (55), so that the potassium chloride with the mass fraction of more than 98% is obtained.
4. A method for producing potassium chloride according to claim 3, wherein: wherein, the liquid phase obtained by the first-stage solid-liquid separation, the liquid phase obtained by the second-stage solid-liquid separation and the liquid phase obtained by the third-stage solid-liquid separation are concentrated, the obtained bottom flow enters a second belt conveyor (57) for solid-liquid separation, and the obtained solid phase is potassium chloride with the mass fraction of more than 95%.
5. A potassium chloride production system, characterized in that: wherein, the potassium chloride production system includes:
the reverse flotation device (1) is used for carrying out reverse flotation on carnallite ore pulp to obtain low-sodium carnallite;
the cold crystallization device (2) is connected with the reverse flotation device (1) and is used for crystallizing the low-sodium carnallite to obtain crystallization underflow;
the first screening device (3) is connected to the back of the cold crystallization device (2) and is used for screening the crystallization underflow to obtain coarse potassium undersize products and coarse potassium oversize products;
a second concentrating device (4) connected after the first screening device (3) and used for concentrating the coarse potassium undersize to obtain a first underflow and a first overflow;
a repulping and washing device (5) connected after the second concentration device (4) and used for washing the first underflow for a plurality of times to obtain potassium chloride;
the brine mixing device (6) is connected with the second concentration device (4) and is used for mixing the first overflow and the old brine to obtain brine mixing pulp containing solid-phase potassium chloride and solid-phase sodium chloride;
the first separation device (7) is connected to the halogen adding device (6) and is used for carrying out solid-liquid separation on the halogen adding ore pulp;
a heat dissolving device (8) which is connected with the first separating device (7) and is used for dissolving and crystallizing the solid phase obtained after the solid-liquid separation of the brine-blended ore pulp to obtain potassium chloride,
the cold crystallization device (2) comprises:
-a first centrifuge (21) connected after said reverse flotation device (1) for solid-liquid separation of said low sodium carnallite;
a first crystallizer (22) connected after the first centrifuge (21) for decomposing the solid phase obtained by the first centrifuge (21);
a first belt conveyor (23) connected to the first centrifuge (21) and configured to separate the liquid phase obtained by the first centrifuge (21) from the solid-liquid phase;
a second crystallizer (24) connected after the first belt conveyor (23) for decomposing the solid phase obtained by the first belt conveyor (23),
and a third crystallizer (25) connected with the first crystallizer (22) and the second crystallizer (24) respectively and used for receiving and crystallizing the decomposed underflow in the first crystallizer (22) and the decomposed underflow in the second crystallizer (24).
6. The potassium chloride production system of claim 5, wherein: the potassium chloride production system further comprises a crushing device (9), wherein the crushing device (9) is arranged between the first screening device (3) and the hot melting device (8) and is used for crushing the coarse potassium oversize product.
7. The potassium chloride production system of claim 5, wherein: wherein the repulping and washing device (5) comprises:
a second centrifuge (51) connected to the second concentrating device (4) for performing a first-stage solid-liquid separation of the first underflow;
a first scrubber (52) connected to the second centrifuge (51) and configured to perform a first repulping and washing of the solid phase obtained by the first-stage solid-liquid separation;
a third centrifuge (53) connected after the first scrubber (52) for performing a second-stage solid-liquid separation of the liquid phase obtained by the first scrubber (52);
a second scrubber (54) connected to the third centrifuge (53) and configured to perform a second repulping and washing of the solid phase obtained by the second solid-liquid separation;
and a fourth centrifuge (55) connected to the second scrubber (54), wherein the third centrifuge is used for performing three-stage solid-liquid separation on the liquid phase obtained by the second scrubber (54) to obtain potassium chloride with a mass fraction of more than 98%.
8. The potassium chloride production system of claim 7, wherein: wherein the repulping washing device (5) further comprises:
a first concentrator (56) connected to the second centrifuge (51), the third centrifuge (53), and the fourth centrifuge (55), respectively, for concentrating a liquid phase obtained by the first-stage solid-liquid separation, a liquid phase obtained by the second-stage solid-liquid separation, and a liquid phase obtained by the third-stage solid-liquid separation;
and a second belt conveyor (57) connected to the first thickener (56) and used for carrying out solid-liquid separation on the bottom flow obtained by the first thickener (56) to obtain potassium chloride with a mass fraction of more than 95%.
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