CN111943232B - Salt-nitrate separation system and frozen nitrate production method using same - Google Patents
Salt-nitrate separation system and frozen nitrate production method using same Download PDFInfo
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- CN111943232B CN111943232B CN202010808078.1A CN202010808078A CN111943232B CN 111943232 B CN111943232 B CN 111943232B CN 202010808078 A CN202010808078 A CN 202010808078A CN 111943232 B CN111943232 B CN 111943232B
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Abstract
The invention discloses a salt and nitrate separation system which comprises a three-dimensional mining system for circularly leaching a nitrate-containing stratum, a slope nitrate freezing system for freezing nitrate treatment of brine collected by the three-dimensional mining system and a solid-liquid separation system for separating mother liquor and crystals output by the slope nitrate freezing system, wherein the slope nitrate freezing system is provided with a brine storage pool communicated with the three-dimensional mining system through a brine conveying pipeline, the brine storage pool is connected with a brine pumping distribution system arranged on the slope nitrate freezing system, and the solid-liquid separation system is positioned at the bottom of the slope nitrate freezing system. The method thoroughly separates the sodium sulfate in the mixed brine in a solid form by freezing the sodium sulfate at low temperature, optimizes the salt-nitrate separation operation flow by utilizing the natural force to cool and crystallize the falling film brine on the slope system, and has the characteristics of stable production output and simple device structure, thereby achieving the industrial aim of low-cost large-scale automatic production.
Description
Technical Field
The invention relates to the field of energy conservation, environmental protection and salt chemical industry, in particular to a salt-nitrate separation system and a frozen nitrate production method using the same.
Background
At present, the exploitation of nitrate ore and the production of sodium sulfate mainly use solid nitrate ore as raw material, and the nitrate ore is mined and transported to a factory area, and is subjected to hot melting, purification and recrystallization to produce anhydrous sodium sulfate (anhydrous sodium sulfate). A plurality of mine pits are left in the original mining area, and sand hills are piled up in the factory area, so that the environment is damaged. As for the general law of salt lake evolution, salt and saltpeter are the symbiotic relationships. Sodium sulfate has the property of having a particularly low solubility at low temperatures. Accordingly, the modern saltpeter industry makes extensive use of saltpeter ponds to freeze saltpeter to extract or remove sodium sulfate from mixed brines.
However, the problem of freezing the saltpeter in the saltpeter pool is that heat exchange between brine and cold air only occurs on a gas-liquid contact surface in winter, total energy exchange is limited, the heat capacity of the brine in the whole pool is large, and the freezing and crystallizing process of sodium sulfate is a heating process, so that the temperature of the brine in the whole pool can be reduced in winter, the total amount of sodium sulfate frozen and separated out in each year is limited, the accumulation of the frozen saltpeter for many years can be used for achieving economic exploitation amount, and a large amount of sandy soil precipitated in other seasons is contained in a frozen saltpeter interlayer formed every year, so that the cost is increased for exploitation and utilization of the frozen saltpeter. In addition, because the temperature of the whole nitre solution can not be reduced to the minimum, the content of sodium sulfate in the nitre solution is still quite high, which is not beneficial to the subsequent utilization of the mother solution, such as the operation of solar salt drying. The operation of evaporating, crystallizing and separating the brine of saltpeter by using temperature change is a mature scheme of the current industry. Through search, the China light International engineering Co., ltd Peng Saijun and the like disclose in the invention patent with the application number CN 201811472718.5: the invention discloses a process for producing salt nitrate by evaporating brine of a salt nitrate system, and provides a device for carrying out evaporation separation operation on salt nitrate brine by taking the brine of the salt nitrate system as a raw material and utilizing different evaporation devices and a process method using the device. However, the invention needs more process steps and corresponding devices, the operation flow needs to consume steam, the larger industrial production energy correspondingly needs larger device structure and larger energy consumption, the unit economic value of the produced main and auxiliary products is not too high, the possibility of large-scale quantitative production is restricted in industrial practical application, and the economic risk of the actual industrial production is improved. Therefore, the mature industrial market puts forward the actual demands for large-scale processing of mass production raw materials, reduction of various related costs, reduction of energy consumption in the process flow by utilizing natural force and more automatic and intelligent completion of industrial quantitative production in the field of salt and sodium sulfate production.
Disclosure of Invention
Aiming at the problems in the existing production process, the invention provides a salt and nitrate separation system which comprises a three-dimensional mining system for circularly leaching a nitrate-containing stratum, a slope nitrate freezing system for freezing nitrate treatment of brine collected by the three-dimensional mining system and a solid-liquid separation system for separating mother liquor and crystals output by the slope nitrate freezing system, wherein the slope nitrate freezing system is provided with a brine storage pool communicated with the three-dimensional mining system through a brine conveying pipeline, the brine storage pool is connected with a brine pumping and distributing system arranged on the slope nitrate freezing system, and the solid-liquid separation system is positioned at the bottom of the slope nitrate freezing system.
The leaching method is adopted to dissolve the sodium sulfate component in the nitrate-containing stratum, the solid mining is changed into ore district elution, the process of transporting a large amount of sandy soil to a factory is omitted, a large amount of pits cannot be left in the ore district, and the sandy mountain cannot be accumulated in the factory. The problems of environment and safety caused by the conventional solid exploitation can be solved or relieved; the investment and the operation cost of brine pumping are far lower than those of solid ore transportation, so the unit mining cost of the nitrate ore is reduced, the requirement on the ore forming content of a mining stratum is reduced, the mineable reserve is expanded, and the mineable life of the nitrate ore is prolonged; the nitre collecting method of the invention keeps the sandy soil in situ, and most of the salt in the leached soil is washed away, thus creating conditions for the future improvement of fertile farmland.
Preferably, the three-dimensional mining system comprises a brine leaching system for leaching the nitrate-containing stratum, a brine collecting tank arranged in the nitrate-containing stratum and a brine collecting groove network arranged in the nitrate-containing stratum and distributed in a net shape, wherein the brine collecting groove network is connected with the brine collecting tank, and the brine collecting tank is connected with the brine leaching system through a pipeline. In the technical scheme, according to the distribution and the mining plan of the nitrate-containing stratum, the three-dimensional mining system reasonably arranges the ditches and the excavation depth according to the distribution and the thickness of the nitrate-containing stratum in a mining area to form a brine collecting groove network, excavates a net-shaped distribution shallow trench or drilling holes in rows on the nitrate-containing stratum to form a spraying groove network, forms a brine three-dimensional leaching system together with the collecting groove network, and carries out limited crushing on the nitrate-containing stratum to improve the leaching efficiency; the brine leaching system is distributed on the nitrate-containing stratum, a spraying ditch net which is dug and distributed in the nitrate-containing stratum is connected with a brine collecting tank, and the brine collecting tank is connected with the brine leaching system through a pipeline.
Preferably, the brine collecting tank is connected with a brine storage pool arranged below the slope nitrate freezing system through the brine conveying pipeline. In this technical scheme, during brine accessible pipeline reinjects into brine leaching system in the brine collecting vat, through the repeated leaching to the formation that contains the nitre, can improve brine concentration in the brine collecting vat rapidly, reach follow-up technology and handle the technological requirement to the high-efficient nitre crystallization of freezing.
Preferably, the slope nitrate freezing system further comprises a crystallization slope and a solid-liquid collecting tank arranged at the bottom of the crystallization slope; and a liquid inlet of the brine pumping distribution system is connected with the brine storage pool, and a liquid outlet of the brine pumping distribution system is distributed at the top of the crystallization slope. In the technical scheme, high-concentration brine in the brine storage pool is conveyed to the top of the slope through the brine pumping distribution system, so that the brine is uniformly subjected to film falling on the surface of the slope, the utilization rate of natural low temperature and wind power in the brine freezing process is improved, crystals crystallized out roll to the solid-liquid collecting tank at the bottom of the slope along with mother liquor, and the automatic operation of the process flow is realized.
Preferably, the solid-liquid separation system comprises a solid-liquid separation tank, a solid lifting and conveying device arranged in the solid-liquid separation tank, a mother liquid level sensor and a mother liquid pump; the solid-liquid separation tank is arranged at the opening of the solid-liquid collecting tank. In the technical scheme, the sodium sulfate crystals and the mother liquor which automatically flow down from the upper surface of the slope can automatically flow into the solid-liquid separation tank, so that the automatic operation of the process flow is realized.
Preferably, an overflow weir is arranged in the solid-liquid separation tank, and the solid-liquid separation tank is divided into a solid settling tank and a mother liquor buffer tank by the overflow weir. In the technical scheme, the solid settling tank automatically guides the mother liquor into the mother liquor buffer tank through the arrangement of the overflow weir structure, so that the automatic separation of the mother liquor and sodium sulfate crystals is completed, and the automatic operation of the process flow is realized.
Preferably, the liquid level sensor and the mother liquor pump are arranged in the mother liquor buffer pool, the mother liquor buffer pool is connected with a liquid inlet pipeline of a heat exchanger arranged in the brine storage pool through a pumping pipeline, and a liquid outlet of the heat exchanger is communicated with the mother liquor reservoir through a pipeline. In this technical scheme, the mother liquor pump opens through level sensor control and stops, and the mother liquor automatic transfer in with the mother liquor buffer pool through heat exchanger is outside, sets up the heat exchanger that has passed through brine storage pond simultaneously and carries out the heat exchange with the brine in mother liquor and the brine storage pond, has optimized the crystallization efficiency of brine in the slope falling liquid film process through the temperature that reduces brine in the brine storage pond.
Preferably, the solid lifting and conveying device is arranged in the solid settling tank, and one end of the solid lifting and conveying device is positioned at the bottom of the solid settling tank. In this technical scheme, thereby solid promotes conveyor and passes through its inside helical structure of drive arrangement drive and rotates and carry solid material from one end to the other end, promotes conveyor and carries the sodium sulfate crystallization of bottom in the solid settling basin to the solid settling basin outer loading or transports to freezing nitre yard through other transport machinery through solid, has realized the automatic operation of high efficiency of process flow.
The invention also provides a frozen nitrate production method, which comprises the following process steps:
s1: extracting appropriate amount of surface water or well water of the mining area or supplementing frozen nitre mother liquor, directly spraying the surface water or well water or supplementing frozen nitre mother liquor to a spray ditch network on a nitre-containing stratum through a brine leaching system, and when enough downward-permeating brine is accumulated in a brine collecting tank, continuously spraying the brine extracted from the brine collecting tank by the brine leaching system to the spray ditch network for leaching circulation;
s2: when the brine concentration in the brine collecting tank reaches a target value, pumping brine into the brine storage tank through a brine conveying pipeline, and starting a new round S1;
s3: when weather conditions are suitable for freezing, pumping saltwater-containing brine from the brine storage pond through the brine pumping distribution system onto the top of the crystallization ramp; the brine flows down along the inclined crystallization surface to form a falling film, the falling film is quickly balanced with the environment, the sodium sulfate component in the falling film is supersaturated, and the sodium sulfate component is continuously crystallized, separated and grown;
s4: the mother liquor with precipitated crystals rolls down a crystallization slope, enters the solid-liquid collecting tank at the slope bottom, converges through an opening of the solid-liquid collecting tank, enters the solid-liquid separation tank, frozen nitrate crystals are precipitated in a solid settling tank in front of an overflow weir, and the mother liquor overflows the overflow weir and enters a mother liquor buffer tank; when a liquid level sensor arranged in a mother liquid buffer pool detects that the liquid level of the mother liquid reaches a set high level, a mother liquid pump is started to transfer the mother liquid to a mother liquid reservoir through a heat exchanger which is deposited in the brine storage pool until the liquid level in the mother liquid buffer pool reaches a set low level, the mother liquid pump stops working, and the next round of mother liquid transfer is waited;
s5: when enough frozen nitrate crystals are accumulated in the solid settling tank, the solid lifting and conveying device is started to directly lift and convey the frozen nitrate crystals to a solid settling tank external truck or other conveying machines to be transported to a frozen nitrate storage yard.
In the technical scheme, in the saltpeter freezing season, when rain, snow or weather is unfavorable for saltpeter freezing, brine is stopped to be pumped to the top of the slope, and circulation is continued from the step S3 after the environmental conditions are suitable. By utilizing the device, the system and the process of the invention to separate the salt and the nitrate, the industrialization of the whole process of mining, purifying, crystallizing, separating, enriching and recovering the nitrate ore is realized, the industrial targets of high purity, high efficiency, energy conservation and environmental protection are achieved, the automation of the whole process is realized, the manpower is saved, the nitrate-containing stratum is cleaned while the high-purity sodium sulfate and the salt-containing mother liquor are obtained in the industrial production through the large-scale and high-efficiency leaching of the nitrate-containing stratum, and more favorable conditions are provided for the subsequent land development.
Preferably, in order to utilize the characteristic that the solubility of the sodium sulfate rapidly rises along with the temperature, the step S1 is preferably arranged to be carried out in a warm season, or the water for leaching is heated, so that the leaching efficiency is effectively improved; in the step S4, the air blowing device can be arranged on the crystallization slope through the air flow rate on the outer surface of the slope, the evaporation efficiency of brine is improved, and the precipitation yield of frozen nitre crystals is increased. In the technical scheme, the leaching efficiency can be effectively improved by heating the leaching water, and a large amount of energy can be saved while the efficiency is improved by selecting the leaching operation in a warm season; through setting up the air flow rate on blast apparatus increase slope surface, can improve brine and cold air heat exchange's efficiency greatly, realize high purity, high yield, energy-concerving and environment-protective industry target.
The invention has the following advantages:
the leaching method is adopted to dissolve the sodium sulfate component in the nitrate-containing stratum, the solid is changed into mining for mining area elution, the process of transporting a large amount of sandy soil to a factory area is omitted, a large amount of pits cannot be left in the mine area, and sandy mountain cannot be accumulated in the factory area. The problems of environment and safety caused by the conventional solid exploitation can be solved or relieved;
the investment and operation cost of brine pumping are far lower than those of solid ore transportation, so that the unit mining cost of the nitre ore is reduced, the requirement on the ore forming content of a mining stratum is reduced, the exploitable reserve is expanded, and the exploitable life of the nitre ore is prolonged;
the nitre collecting method of the invention keeps the sandy soil in situ, and most of the salt in the leached soil is washed away, thereby creating conditions for changing into fertile farmland in future;
according to the invention, a slope crystallization separation system is utilized to form a brine falling film, so that the rapid balance between brine and air temperature is realized, the freezing saltpeter temperature can be flexibly and accurately selected according to the actual air temperature, sodium sulfate in brine is thoroughly separated out, the yield of the freezing saltpeter is almost the highest, and the content of the residual sodium sulfate in the frozen mother liquor is the lowest;
the frozen nitrate crystal is separated out in time by the frozen nitrate method, not only is the frozen nitrate process, but also the frozen nitrate solid is collected, and energy-saving and environment-friendly pumping is mainly utilized to replace the traditional mechanical crushing and excavation with easy pollution and high cost;
the frozen nitre crystals collected by the invention are not only uniform and loose and easy to transport, but also high in purity, and can be directly used for anhydrous sodium sulphate production without purification;
the method for freezing the mirabilite can utilize the low temperature at night, so that the method has longer available mirabilite freezing days per year; because the nitre is frozen and the nitre is harvested at the same time, the harvesting efficiency reaches the highest. The actual utilization of the traditional nitre pond freezing method is only the average temperature in winter, and even in any case, because the nitre can be exploited only by accumulation for many years, the frozen nitre formed in winter can be partially dissolved by the rising of the average water temperature of the nitre pond in other seasons;
if a detachable and movable slope crystallization separation system is adopted, the vast crust of the mining area can be fully utilized, and a mobile crystallization workshop can be conveniently built in the mined mining area;
if the traditional nitre pond freezing nitre method utilizes natural force to separate the salt and the nitre, the invention realizes the industrialization of the whole process of mining, purifying, crystallizing, separating, enriching and collecting the nitre ore when the natural force is utilized to separate the salt and the nitre, achieves all the aims of high purity, high yield, energy conservation and environmental protection, and can realize the intellectualization of the whole process;
nitrate-containing formations often contain a large amount of symbiotic other salts, especially sodium chloride, and the surface water or well water of a mining area used for leaching and leaching product brine are mixed solutions of sodium sulfate and sodium chloride, so that pure single salt products cannot be produced by direct evaporation crystallization. The process of the invention completely separates the sodium sulfate in the mixed brine in a solid form by freezing the nitrate at low temperature. Because the solubility of sodium chloride is reduced little along with the temperature and can not be frozen and crystallized, the quality of frozen saltpeter can not be influenced, and the freezing temperature of mother liquor is reduced in the process of separating the slope saltpeter crystal, so that the freezing temperature is lower, the content of sodium sulfate in the obtained mother liquor is lower, and the comprehensive utilization value of the mother liquor is higher.
Although the invention is mainly designed for freezing saltpeter, the invention can also be applied to the elution of other substances with similar physicochemical conditions, such as the remediation engineering of polluted soil, and the polluted substances eluted by steam or hot water are directly separated by a slope crystallization device.
Drawings
FIG. 1 is a schematic view of an assembled three-dimensional layout according to the present invention;
FIG. 2 is another perspective view of an assembled three-dimensional layout according to the present invention;
FIG. 3 is a schematic structural view of a collecting tank and a solid-liquid separation tank of the present invention;
in the drawings: 1-nitrate-containing stratum, 2-brine leaching system, 3-brine collecting tank, 4-brine conveying pipeline, 5-brine storage tank, 6-crystallization slope, 7-brine pumping distribution system, 8-solid-liquid collecting tank, 81-solid-liquid collecting tank opening, 9-solid-liquid separation tank, 91-solid settling tank, 92-overflow weir, 93-mother liquor buffer tank, 94-liquid level sensor, 95-solid lifting conveying device, 10-mother liquor pump, 11-heat exchanger and 12-mother liquor storage tank.
Detailed Description
The drawings are for illustrative purposes only and are not to be construed as limiting the patent; for the purpose of better illustrating the embodiments, certain features of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted. The positional relationships depicted in the drawings are for illustrative purposes only and are not to be construed as limiting the present patent.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there are terms such as "upper", "lower", "left", "right", "long", "short", etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the drawings, it is only for convenience of description and simplicity of description, but does not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationships in the drawings are only used for illustrative purposes and are not to be construed as limitations of the present patent, and specific meanings of the terms may be understood by those skilled in the art according to specific situations.
The technical scheme of the invention is further described in detail by the following specific embodiments in combination with the accompanying drawings:
example 1
As shown in fig. 1 to 3, a salt and nitrate separation system includes the three-dimensional mining system that is used for carrying out the circulation drip washing to nitre-containing stratum 1, is used for freezing the slope of nitre treatment to the brine that the three-dimensional mining system was collected and freezes nitre system and is used for freezing the solid-liquid separation system that mother liquor and the crystal of nitre system output carry out the separation to the slope, the slope freeze the nitre system be provided with through brine pipeline 4 with brine reservoir 5 that the three-dimensional mining system is linked together, brine reservoir 5 with set up be in brine pumping distribution system 7 on the slope freeze the nitre system is connected, solid-liquid separation system is located the bottom that the nitre system was frozen to the slope.
The three-dimensional mining system comprises a brine leaching system 2 for leaching the nitrate-containing stratum 1, a brine collecting tank 3 arranged in the nitrate-containing stratum 1 and a brine collecting groove network arranged in the nitrate-containing stratum 1 and distributed in a net shape, wherein the brine collecting groove network is connected with the brine collecting tank 3, and the brine collecting tank 3 is connected with the brine leaching system 2 through a pipeline.
In the embodiment, according to the distribution and the mining plan of the nitrate-containing stratum 1, the three-dimensional mining system reasonably arranges the channels and the excavation depth according to the distribution and the thickness of the nitrate-containing stratum 1 in a mining area to form a brine collecting groove network, excavates a net-shaped distribution shallow trench or rows of holes on the nitrate-containing stratum 1 to form a spraying groove network, and forms a brine three-dimensional leaching system together with the collecting groove network to perform limited crushing on the nitrate-containing stratum 1 so as to improve the leaching efficiency; the brine leaching system 2 is distributed on the nitrate-containing stratum 1, a spraying ditch net which is dug and distributed in the nitrate-containing stratum 1 is connected with a brine collecting tank 3, and the brine collecting tank 3 is connected with the brine leaching system 2 through a pipeline.
In addition, brine collecting tank 3 is connected with brine storage pond 5 that sets up the slope freezes nitre system below through brine pipeline 4. Brine in the brine collecting tank 3 can be injected into the brine leaching system 2 again through a pipeline, brine concentration in the brine collecting tank 3 can be rapidly improved through repeated leaching of the nitrate-containing stratum 1, and the process requirement of follow-up process treatment on efficient nitrate freezing crystallization is met.
The slope nitrate freezing system further comprises a crystallization slope 6 and a solid-liquid collecting tank 8 arranged at the bottom of the crystallization slope; the liquid inlet of brine pumping distribution system 7 with brine storage pond 5 is connected, the liquid outlet of brine pumping distribution system 7 distributes in the top of crystallization slope 6. High-concentration brine in the brine storage tank 5 is conveyed to the top of the crystallization slope 6 through the brine pumping distribution system 7, so that brine is uniformly subjected to film falling on the surface of the crystallization slope 6, the utilization rate of natural low temperature and wind power in a brine freezing process is improved, crystals crystallized out roll to a slope bottom solid-liquid collecting tank along with mother liquor, and the automatic operation of the process flow is realized.
In addition, the solid-liquid separation system includes a solid-liquid separation tank 9, a solid lifting and conveying device 95 provided in the solid-liquid separation tank 9, a mother liquor level sensor 94, and a mother liquor pump 10; the solid-liquid separation tank 9 is provided at a solid-liquid tank opening 81 of the solid-liquid tank 8. The sodium sulfate crystals and the mother liquor which automatically flow down from the upper surface of the crystallization slope 6 can automatically flow into the solid-liquid separation tank 9, so that the automatic operation of the process flow is realized.
The solid-liquid separation tank 9 is provided with an overflow weir 92, and the solid-liquid separation tank 9 is partitioned into a solid settling tank 91 and a mother liquor buffer tank 93 by the overflow weir 92. The solid settling tank 91 automatically guides the mother liquor into the mother liquor buffer tank 93 through the arrangement of the overflow weir 92 structure, so that the automatic separation of the mother liquor and sodium sulfate crystals is completed, and the automatic operation of the process flow is realized.
In addition, the liquid level sensor 94 and the mother liquor pump 10 are arranged in the mother liquor buffer pool 93, the mother liquor buffer pool 93 is connected with a liquid inlet pipeline of a heat exchanger 11 arranged in the brine storage pool 5 through the mother liquor pump 10, and a liquid outlet of the heat exchanger 11 is communicated with a mother liquor storage pool 12 through a pipeline. Mother liquor pump 10 opens through level sensor 94 control and stops, and the mother liquor automatic transfer in with mother liquor buffer pool 93 through heat exchanger 11 is outside, sets up simultaneously and has carried out the heat exchange with the brine in mother liquor and the brine reservoir pool 5 through heat exchanger 11 of brine reservoir pool 5, has optimized the crystallization efficiency of brine in the slope falling film process through the temperature that reduces brine in the brine reservoir pool 5.
The solid lifting and conveying device 95 is disposed in the solid settling tank 91, and one end of the solid lifting and conveying device 95 is located at the bottom of the solid settling tank 91. Thereby solid promotes conveyor 95 and passes through its inside helical structure of drive arrangement drive and rotates solid material from one end to the other end and carry, promotes conveyor 95 with the sodium sulfate crystallization of bottom in the solid sedimentation tank 91 through the solid and promotes and carry to the solid sedimentation tank 91 external loading car or through other transport machinery transports to freeze nitre yard, has realized the automatic operation of high efficiency of process flow.
Example 2
The production method of frozen mirabilite comprises the following process steps:
s1: extracting a proper amount of surface water or well water of the mining area or supplementing frozen saltpeter mother liquor, directly spraying the surface water or well water or the frozen saltpeter mother liquor to a spraying ditch network on a saltpeter-containing stratum 1 through a brine leaching system 2, and when enough downward-permeating brine is accumulated in a brine collecting tank 3, continuously spraying brine to the spraying ditch network by the brine leaching system 2 after the brine is extracted from the brine collecting tank 3, and performing leaching circulation;
s2: when the brine concentration in the brine collecting tank 3 reaches a target value, pumping brine into the brine storage tank 5 through a brine conveying pipeline 4, and starting a new cycle S1;
s3: when weather conditions are suitable for freezing, saltpeter brine is pumped from the brine holding pond 5 through the brine pumping distribution system 7 onto the top of the crystallization ramp 6; the brine flows down along the inclined plane of the crystallization slope 6 to form a falling film, the falling film is quickly balanced with the environment, the sodium sulfate component in the falling film is supersaturated, and the sodium sulfate component is continuously crystallized, separated out and grown up;
s4: the mother liquor with precipitated crystals rolls down the crystallization slope 6, enters the solid-liquid collecting tank 8 at the slope bottom, converges through the solid-liquid collecting tank opening 81, enters the solid-liquid separation tank 9, the frozen nitrate crystals are precipitated in the solid sedimentation tank 91 in front of the overflow weir 92, and the mother liquor overflows the overflow weir 92 and enters the mother liquor buffer tank 93; when a liquid level sensor 94 arranged in a mother liquid buffer pool 93 detects that the liquid level of the mother liquid reaches a set high level, a mother liquid pump 10 is started to transfer the mother liquid to a mother liquid reservoir 12 through a heat exchanger 11 which is deposited in the brine storage pool 5 until the liquid level in the mother liquid buffer pool 93 reaches a set low level, and the mother liquid pump 10 stops working to wait for the next round of mother liquid transfer;
s5: when sufficient frozen crystals of saltpeter have accumulated in the solids settling tank 91, the solids lift conveyor 95 is actuated to lift and convey the frozen crystals of saltpeter directly to an off-board vehicle of the solids settling tank 91 or by other conveying machinery to a frozen saltpeter storage yard.
In addition, in the saltpeter freezing season, when rain, snow or weather is unfavorable for saltpeter freezing, the pumping of the brine to the top of the slope is stopped, and the circulation is continued from the step S3 after the environmental conditions are suitable. By utilizing the device, the system and the process of the invention to separate the salt and the nitrate, the industrialization of the whole process of mining, purifying, crystallizing, separating, enriching and recovering the nitrate ore is realized, the industrial targets of high purity, high efficiency, energy saving and environmental protection are achieved, the automation of the whole process is realized, the manpower is saved, the nitrate-containing stratum is cleaned while the high-purity sodium sulfate and the salt-containing mother liquor are obtained in the industrial production through the large-scale and high-efficiency leaching of the nitrate-containing stratum, and more favorable conditions are provided for the subsequent land development.
In order to utilize the characteristic that the solubility of the sodium sulfate rapidly rises along with the temperature, the step S1 is preferably arranged to be carried out in a warm season, or the water for leaching is heated, so that the leaching efficiency is effectively improved; through set up blast apparatus on crystallization slope 6 in step S4, through increasing 6 surface air velocity of crystallization slope, improve the evaporation efficiency of brine, increase and freeze nitre crystal and precipitate out output. The leaching efficiency can be effectively improved by heating the leaching water, and a large amount of energy can be saved while the efficiency is improved by selecting the leaching operation in a warm season; through setting up the air flow rate on 6 surfaces in blast apparatus increase crystallization slope, can improve the efficiency of brine crystallization greatly, realize high purity, high yield, energy-concerving and environment-protective industrial objective.
In the detailed description of the above embodiments, various technical features may be arbitrarily combined, and for the sake of brevity, all possible combinations of the above technical features are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Although the invention is mainly designed for freezing nitre, the invention can also be applied to the elution of other substances with similar physicochemical conditions, such as the remediation engineering of polluted soil, and the polluted solution eluted by steam or hot water is directly separated by a slope crystallization device. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. A salt and nitrate separation system is characterized in that: the device comprises a three-dimensional mining system for circularly leaching a nitrate-containing stratum (1), a slope nitrate freezing system for freezing nitrate treatment of brine collected by the three-dimensional mining system and a solid-liquid separation system for separating mother liquor and crystals output by the slope nitrate freezing system, wherein the slope nitrate freezing system is provided with a brine storage pool (5) communicated with the three-dimensional mining system through a brine conveying pipeline (4), the brine storage pool (5) is connected with a brine pumping distribution system (7) arranged on the slope nitrate freezing system, and the solid-liquid separation system is positioned at the bottom of the slope nitrate freezing system; the three-dimensional mining system comprises a brine leaching system (2) for leaching the nitrate-containing stratum (1), a brine collecting tank (3) arranged in the nitrate-containing stratum (1) and a brine collecting groove net which is arranged in the nitrate-containing stratum (1) and is distributed in a net shape, wherein the brine collecting groove net is connected with the brine collecting tank (3), and the brine collecting tank (3) is connected with the brine leaching system (2) through a pipeline.
2. The salt and nitrate separation system of claim 1, wherein: the brine collecting tank (3) is connected with a brine storage pool (5) arranged below the slope nitrate freezing system through the brine conveying pipeline (4).
3. The salt and nitrate separation system of claim 1, wherein: the slope nitrate freezing system also comprises a crystallization slope (6) and a solid-liquid collecting tank (8) arranged at the bottom of the crystallization slope (6); the liquid inlet of the brine pumping distribution system (7) is connected with the brine storage pool (5), and the liquid outlet of the brine pumping distribution system (7) is distributed at the top of the crystallization slope (6).
4. The salt and nitrate separation system of claim 3, wherein: the solid-liquid separation system comprises a solid-liquid separation tank (9), a solid lifting and conveying device (95) arranged in the solid-liquid separation tank (9), a mother liquid level sensor (94) and a mother liquid pump (10); the solid-liquid separation tank (9) is arranged at a solid-liquid collecting tank opening (81) of the solid-liquid collecting tank (8).
5. The salt and nitrate separation system of claim 4, wherein: an overflow weir (92) is arranged in the solid-liquid separation tank (9), and the overflow weir (92) divides the solid-liquid separation tank (9) into a solid settling tank (91) and a mother liquor buffer tank (93).
6. The salt and nitrate separation system of claim 5, wherein: level sensor (94) and mother liquor pump (10) are located in mother liquor buffer pool (93), mother liquor buffer pool (93) are connected with the inlet pipe of heat exchanger (11) of locating brine storage pool (5) through the mother liquor pump, the liquid outlet of heat exchanger (11) is linked together through pipeline and mother liquor cistern (12).
7. The salt and nitrate separation system of claim 4, wherein: the solid lifting and conveying device (95) is arranged in the solid settling tank (91), and one end of the solid lifting and conveying device (95) is positioned at the bottom of the solid settling tank (91).
8. A frozen nitrate production method based on the salt and nitrate separation system of any one of claims 1 to 7, which is characterized by comprising the following process steps:
s1: extracting appropriate amount of surface water or well water of a mining area or supplementing frozen nitre mother liquor, directly spraying the surface water or well water or supplementing frozen nitre mother liquor onto a nitre-containing stratum (1) through a three-dimensional mining system, extracting brine again and repeatedly spraying the brine onto the nitre-containing stratum (1) when enough infiltrated brine is accumulated, and performing leaching circulation;
s2: when the concentration of the brine collected by the three-dimensional mining system reaches a target value, pumping the brine into the brine storage pool (5) through a brine conveying pipeline (4), and starting a new round S1;
s3: when weather conditions are suitable for freezing, pumping saltpeter-containing brine from the brine storage tank (5) through the brine pumping distribution system (7) onto the top of the slope saltpeter freezing system; the brine flows down along a crystallization slope in the slope nitrate freezing system to form a falling film, the falling film is quickly balanced with the environment, the sodium sulfate component in the falling film is supersaturated, and the sodium sulfate component is continuously crystallized, separated and grown;
s4: the mother liquor carries the precipitated crystals to roll down a crystallization slope in a slope nitrate freezing system, and the crystals enter the solid-liquid separation system at the slope bottom to separate the frozen nitrate crystals from the mother liquor;
s5: when enough frozen saltpeter crystals are accumulated in the solid-liquid separation system, the frozen saltpeter crystals are lifted and conveyed to the outside of the solid-liquid separation system for loading or are conveyed to a frozen saltpeter storage yard through other conveying machines.
9. The method for producing frozen mirabilite according to claim 8, wherein: in order to utilize the characteristic that the solubility of the sodium sulfate rapidly rises along with the temperature, the step S1 is preferably arranged to be carried out in a warm season, or the leaching water is heated, so that the leaching efficiency is effectively improved; in step S4, set up blast apparatus on the crystallization slope, through increase crystallization slope surface air velocity of flow, improve the evaporation efficiency of brine, increase and freeze nitre crystal and precipitate out output.
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| CN1045319C (en) * | 1994-03-03 | 1999-09-29 | 湖南化学工业设计院 | Method for preparing sodium hydroxide by brine electrolysis |
| CN202089783U (en) * | 2010-10-21 | 2011-12-28 | 天津科技大学 | Mirabilite brine freezing-crystallizing separating system |
| CN103949082B (en) * | 2014-04-25 | 2016-08-31 | 涂海军 | A kind of double cold cooling flowing crystallization apparatus |
| CN108298565B (en) * | 2018-02-09 | 2019-12-03 | 陕西省膜分离技术研究院有限公司 | A kind of concentration of spraying and sprinkling evaporation divides salt device and divides salt method |
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