CN110734078A - method for preparing potassium chloride by using low-energy consumption of low-grade potassium resource ore - Google Patents
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Abstract
method for preparing potassium chloride by using low energy consumption of low-grade potassium resource ore, relating to the technical field of inorganic salt, the specific technical scheme comprises the steps of decomposing the low-grade potassium resource ore, evaporating and dissolving potassium brine to prepare sylvite and carnallite, preparing artificial sylvite, preparing sylvite solution, diluting the sylvite solution, constructing a solar cell, filling the solar cell in a layered horizontal manner, operating the solar cell, dissolving sylvite in heat, filtering, cooling and crystallizing in a tenth step, and recycling low-temperature mother liquid.
Description
Technical Field
The invention relates to the technical field of inorganic salt, in particular to technologies for preparing potassium chloride by utilizing low-energy consumption of low-grade potassium resource ores.
Background
Potassium chloride is an important fertilizer and chemical raw material with strategic significance, is a main variety of potassium fertilizer, and contains an effective component K2The content of O is usually about 60 percent, the fertilizer is a quick-acting potassium fertilizer with chemical neutrality and physiological acidity, is widely used for field crops such as rice, wheat, corn, cotton and the like, the potassium salt resource quantity in China is relatively short, the national potassium chloride basic reserve only accounts for about 2 percent of the global reserve, the fertilizer is mainly liquid ore, 95 percent of the potassium chloride basic reserve is distributed in Qinghai Chailada wood basins in the west and Xinjiang Apocynum North depression, the national potassium-deficient farmland accounts for 56 percent of the total cultivated land area, the potassium element distribution in the soil structure in China is unbalanced, particularly, the potassium deficiency is common in the soil in the south and large areas in the Yangtze river basin in China, and the potassium content is more than 8000 ten thousand hm2The medium and low yield field needs to be reformed, and the insufficient application of the potash fertilizer becomes which is a main limiting factor for increasing the yield of crops by steps in China, China is the market with the largest global potash fertilizer demand, and the annual potash fertilizer demand is about 800-900 ten thousand tons (by K)2O) with about 50% dependence on the inlet.
The potassium fertilizer industry develops rapidly in recent years, the yield is improved continuously, high-grade sylvite ore is consumed completely, resources are in short supply, the sustainable development of the potash fertilizer industry is restricted, the potassium resource of the salt lake in the Yanda basin is mined for no more than 50 years according to the current productivity, meanwhile, considerable low-grade and high-silt potassium ore resources in the Yanda basin are not utilized, potassium fertilizer enterprises in China mainly use carnallite as a raw material and produce potassium chloride by adopting a flotation process, tail salt is produced no matter direct flotation or reverse flotation, unused potassium elements still exist in the tail salt more or less, the most advanced reverse flotation process for producing potassium chloride in China produces potassium chloride by using 1.2 tKCl mass fraction in about 2-7% flotation process, tail salt discharged by other flotation processes is discharged as tail salt, and more tail salt discharged by other processes has great significance, and the quality of potassium chloride is discharged in the production of the whole Yanda basin, and the tail salt produced by the flotation process has great significance of recovering potassium chloride in ten million potassium chloride in the past ten thousand-million-ton production process.
At present, in the aspect of utilization of low-grade potassium resource ores, a hot melting-cold crystallization potassium chloride production process is researched and developed, and is a main way for recycling low-grade potassium ores at present, but the problems of high energy consumption, severe scaling and corrosion of hot melting equipment and the like are encountered, the economic benefit is poor, and technological innovation and upgrading are needed.
Disclosure of Invention
Aiming at the technical problems, the energy consumption in the production process is reduced by adopting a solar pond technology, and the invention provides methods for preparing potassium chloride by utilizing low-energy consumption of low-grade potassium resource ores, which comprise the following preparation steps:
, decomposing low-grade potassium resource ores, dissolving quantitative flotation tailings in water at a solid-to-liquid ratio of 1: 0.7-1, and filtering to remove solid phases such as silt and undissolved substances to prepare potassium-dissolved brine for later use;
evaporating the potassium-dissolved brine to prepare sylvite and carnallite, taking quantitative potassium-dissolved brine, naturally evaporating and filtering to prepare a solid phase of sylvite and carnallite for later use;
thirdly, preparing artificial sylvite, namely mixing quantitative sylvite and carnallite into a solid phase, adding water for decomposition, wherein the solid-liquid ratio is 1: 0.3-0.6, further reduces the content of magnesium chloride, improves the content of potassium chloride, and filtering to obtain the artificial sylvite for later use;
fourthly, preparing a sylvite solution, taking quantitative artificial sylvite, adding water for dissolving, and obtaining the sylvite solution with the concentration of 28-degree Be' and the turbidity of less than 5NTU for later use through clarification and filtration;
fifthly, diluting the sylvite solution, adding water into quantitative sylvite solution with 28-degree Be 'concentration to dilute the sylvite solution to 18-23-degree Be' for later use;
building a solar pond, selecting cuboid evaporation ponds with the length of 1.00m, the width of 0.60m and the depth of 0.55m as the sylvite solar ponds, adding an insulating layer, alternately and horizontally placing pipe ends at the bottom of the ponds for sealing, arranging a liquid taking and replenishing coil pipe with small holes on the whole body, covering layers of small stones on the pipe, and spreading a solid sylvite layer with the thickness of 3cm on the stones;
the seventh step: and (5) horizontally pouring the solar pond layer by layer. Taking 0.06-0.08 m of sylvite solution with turbidity less than 5NTU and concentration of 28-degree Be' obtained in the fourth step3Horizontally perfusing the troposphere below the solar pond; taking 0.16-0.18 m of the sylvite solution with the concentration of 18-23 degrees Be' obtained in the fifth step3Horizontally filling the solar pond with a salt gradient layer, and filling the solar pond with a convection layer of 0.03m3Fresh water;
eighth step: the solar pond is operated. The solar pond is operated under the natural condition that the average daily temperature is 15 ℃ and the relative humidity is 20%, the illumination in the daytime and the closing at night are performed, and when the solution temperature of the lower troposphere is stable, the temperature of the solution is 45-50 ℃. The concentration and the temperature of each layer of solution are regularly detected during the operation of the solar pond, and when the upper convection layer is thinned due to water evaporation, a proper amount of fresh water is supplemented to keep the stable operation of the solar pond;
the ninth step, hot-melting sylvite, namely extracting quantitative sylvite solution with the temperature of 45-50 ℃ from the bottom of the solar pond, adding quantitative solid sylvite into the solution, heating the solution to 90-93 ℃, and further dissolving the sylvite in the step;
the tenth step: and (5) filtering. Filtering the sylvite solution obtained in the ninth step, and removing suspended impurities such as sodium chloride and the like to obtain high-temperature mother liquor for later use;
and a tenth step of cooling and crystallizing, namely naturally cooling the high-temperature mother liquor obtained in the tenth step to 15-20 ℃, separating out potassium chloride crystals, filtering and drying to obtain a potassium chloride product, and filtering to obtain a low-temperature mother liquor for later use.
And twelfth step, performing liquid cooling recycling on the low-temperature mother liquor, adding quantitative 28-degree Be' sylvite solution into the low-temperature mother liquor obtained in the tenth step, and adding the mixture into a convection layer below the solar pond for recycling.
The invention has the beneficial effects that a solar pond is constructed by utilizing a sylvite solution, the gathered solar energy is used for hot-dissolving sylvite, low-energy consumption recycling of low-grade potassium resources is realized, the construction method and the operation rule of the sylvite solar pond are researched and explored, types of sylvite filled at the bottom are invented, the heat storage performance of the solar pond can be optimized, the potassium dissolving amount of the sylvite solar pond can be improved, the solution with higher concentration and temperature of a convection layer under the solar pond is taken out to carry out steps of hot-dissolving sylvite, filtering and separating sodium chloride, cooling and crystallizing to separate out potassium chloride, and filtering and drying to prepare the potassium chloride meeting the national standard.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a mass balance diagram of example 1;
FIG. 3 is a mass balance diagram of example 2;
FIG. 4 is a mass balance diagram of example 3.
Detailed Description
Embodiment 1, as shown in fig. 1 and fig. 2, the present invention provides methods for preparing potassium chloride using low-grade potassium resource ore with low energy consumption, and the specific technical scheme includes the following preparation steps:
, decomposing low-grade potassium resource ores, dissolving 940.00kg of flotation tailings in water at a solid-to-liquid ratio of 1: 0.8, and filtering to remove 377.88kg of solid phases such as silt and undissolved substances to obtain 562.12kg of potassium-dissolved brine for later use;
the second step is that: evaporating the potassium-dissolved brine to prepare sylvite and carnallite. 562.12kg of potassium-dissolved brine is taken, naturally evaporated and filtered to prepare 213.85kg of mixed solid phase of sylvite and carnallite for later use;
thirdly, preparing artificial sylvite, namely mixing 213.85kg of sylvite and carnallite into a solid phase, adding water for decomposition, wherein the solid-liquid ratio is 1: 0.5, reducing the content of magnesium chloride and increasing the content of potassium chloride by steps, and filtering to prepare 128.31kg of artificial sylvite for later use;
the fourth step: preparing a sylvite salt solution. Dissolving 76.07kg of artificial sylvite in water, clarifying, and filtering to obtain 215.12kg of solution with concentration of 28-degree Be' and turbidity of less than 5NTU for later use;
the fifth step: diluting the sylvite solution. 140.67kg of 28-degree Be 'sylvite solution is taken and diluted by adding water to 19-degree Be' to obtain 207.29kg of solution for later use;
building a solar pond, selecting cuboid evaporation ponds with the length of 1.00m, the width of 0.60m and the depth of 0.55m as the sylvite solar ponds, adding a heat-insulating layer, alternately and horizontally placing pipe ends at the bottom of the ponds for sealing, arranging a liquid taking and replenishing coil pipe with small holes on the whole body, covering layers of small stones on the pipe, and spreading 41.48kg of solid sylvite with the thickness of 3cm on the stones;
the seventh step: and (5) horizontally pouring the solar pond layer by layer. 74.45kg (0.06 m) of 28 ℃ Be' sylvine solution with turbidity less than 5NTU obtained in the fourth step3) Horizontally perfusing the troposphere below the solar pond; 207.29kg (0.18 m) of the 19 ℃ Be' potassium salt solution obtained in the fifth step3) Horizontally pouring the salt gradient layer in the solar pond; 30kg (0.03 m) of perfusion is filled into the troposphere on the solar pond3) Fresh water;
eighth step: the solar pond is operated. The solar pond is operated under the natural conditions of simulating the daily average temperature of 15 ℃ and the relative humidity of 20 percent, the illumination in the daytime and the closing at night are carried out, and when the solution temperature of the lower troposphere reaches the stability, the temperature of the solution of the lower troposphere is 45 ℃; the concentration and the temperature of each layer of solution are regularly detected during the operation of the solar pond, and when the upper convection layer is thinned due to water evaporation, a proper amount of fresh water is supplemented to keep the stable operation of the solar pond;
the ninth step is that the sylvite is hot-dissolved, 67.01kg of sylvite solution with the temperature of 45 ℃ is extracted from the bottom of the solar pond, 10.76kg of solid sylvite is added into the sylvite solution, and the mixture is heated to 93 ℃ to further dissolve the sylvite in steps;
the tenth step: and (5) filtering. Filtering the sylvite solution obtained in the ninth step, removing 25.31kg of suspended impurities such as sodium chloride and the like, and evaporating 1.04kg of water to obtain 51.42kg of high-temperature mother liquor for later use;
and a tenth step of cooling and crystallizing, namely naturally cooling 51.42kg of the high-temperature mother liquor obtained in the tenth step to 15 ℃, crystallizing and separating out potassium chloride, filtering to obtain 41.46kg of filtrate, and drying the filter cake to obtain 9.76kg of 96.35% potassium chloride, which meets the indexes of GB6549-2011 potassium chloride I type industrial potassium chloride and the like.
And twelfth, recycling the low-temperature mother liquor in a cooling way, adding 25.55kg of sylvite solution with the concentration of 28-degree Be' into 41.46kg of filtrate obtained in the tenth step to obtain 67.01kg of low-temperature mother liquor, and adding the low-temperature mother liquor into a lower convection layer of the solar pond for recycling.
Embodiment 2, as shown in fig. 1 and fig. 3, the present invention provides methods for preparing potassium chloride using low-grade potassium resource ore with low energy consumption, and the specific technical scheme includes the following preparation steps:
, decomposing low-grade potassium resource ores, dissolving 1104.84kg of flotation tailings in water at a solid-to-liquid ratio of 1: 0.9, and filtering to remove 441.94kg of solid phases such as silt and undissolved substances to obtain 662.90kg of potassium-dissolved brine for later use;
the second step is that: evaporating the potassium-dissolved brine to prepare sylvite and carnallite. 662.90kg of potassium-dissolved brine is taken, naturally evaporated and filtered to prepare 251.35kg of mixed solid phase of sylvite and carnallite for later use;
thirdly, preparing artificial sylvite, namely mixing 251.35kg of sylvite and carnallite into a solid phase, adding water for decomposition, wherein the solid-liquid ratio is 1: 0.6, reducing the content of magnesium chloride and increasing the content of potassium chloride by steps, and filtering to prepare 150.81kg of artificial sylvite for later use;
the fourth step: preparing a sylvite salt aqueous solution. Taking 83.57kg of artificial sylvite, adding water for dissolving, clarifying and filtering to obtain 236.33kg of solution with the concentration of 28-degree Be' and the turbidity of less than 5NTU for later use;
the fifth step: diluting the sylvite solution. 139.88kg of 28-degree Be 'sylvite solution is taken and diluted by adding water to 21-degree Be' to obtain 186.56kg of solution for later use;
building a solar pond, selecting cuboid evaporation ponds with the length of 1.00m, the width of 0.60m and the depth of 0.55m as the sylvite solar ponds, adding a heat-insulating layer, alternately and horizontally placing pipe ends at the bottom of the ponds for sealing, arranging a liquid taking and replenishing coil pipe with small holes on the whole body, covering layers of small stones on the pipe, and spreading 41.48kg of solid sylvite with the thickness of 3cm on the stones;
the seventh step: and (5) horizontally pouring the solar pond layer by layer.96.45kg (0.078 m) of 28 ℃ Be' sylvine solution with turbidity less than 5NTU obtained in the fourth step3) Horizontally perfusing the troposphere below the solar pond; 186.56kg (0.162 m) of the sylvite solution with the concentration of 21 DEG Be' obtained in the fifth step3) The salt gradient layer is horizontally poured in the solar pond, and the troposphere on the solar pond is poured by 30kg (0.03 m)3) Fresh water;
eighth step: the solar pond is operated. The solar pond is operated under natural conditions that the daily average temperature is 15 ℃ and the relative humidity is 20%, the sunlight is turned off in the daytime and at night, and when the sunlight is stable, the temperature of the lower troposphere solution is 47 ℃; the concentration and the temperature of each layer of solution are regularly detected during the operation of the solar pond, and when the upper convection layer is thinned due to water evaporation, a proper amount of fresh water is supplemented to keep the stable operation of the solar pond;
the ninth step, hot-melt sylvite, 86.81kg of sylvite solution with the temperature of 47 ℃ is extracted from the bottom of the solar pond, 26.06kg of solid sylvite is added into the sylvite solution, and the mixture is heated to 90 ℃ to further dissolve the sylvite steps;
the tenth step: and (5) filtering. Filtering the sylvite salt solution obtained in the ninth step, removing 36.73kg of suspended impurities such as sodium chloride and the like, and evaporating 1.51kg of water to obtain 74.63kg of high-temperature mother liquor for later use;
and a tenth step of cooling and crystallizing, namely naturally cooling 74.63kg of the high-temperature mother liquor obtained in the tenth step to 17 ℃, crystallizing and separating out potassium chloride, filtering to obtain 60.45kg of filtrate, and drying the filter cake to obtain 14.18kg of potassium chloride with the content of 95.81%, wherein the potassium chloride meets the indexes of industrial potassium chloride and the like in GB6549-2011 potassium chloride I class.
Twelfth step, the low-temperature mother liquor is cooled and recycled, 26.36kg of sylvine solution with the concentration of 28 degrees Be' is added into 60.45kg of filtrate obtained in the tenth step to obtain 86.81kg of low-temperature mother liquor, and the low-temperature mother liquor is added into the lower convection layer of the solar pond for recycling
Embodiment 3, as shown in fig. 1 and 4, the present invention provides methods for preparing potassium chloride using low-grade potassium resource ore with low energy consumption, and the specific technical scheme includes the following preparation steps:
, decomposing low-grade potassium resource ores, dissolving 1115.83kg of flotation tailings in water at a solid-to-liquid ratio of 1: 0.7, and filtering to remove 457.49kg of solid phases such as silt and undissolved substances to obtain 658.34kg of potassium-dissolved brine for later use;
the second step is that: evaporating the potassium-dissolved brine to prepare sylvite and carnallite. 658.34kg of potassium-dissolving brine is taken, naturally evaporated and filtered to prepare 253.85kg of mixed solid phase of sylvite and carnallite for later use;
thirdly, preparing artificial sylvite, namely mixing 253.85kg of sylvite and carnallite into a solid phase, adding water for decomposition, wherein the solid-liquid ratio is 1: 0.4, further , reducing the content of magnesium chloride, increasing the content of potassium chloride, and filtering to obtain 152.31kg of artificial sylvite for later use;
the fourth step: preparing a sylvite salt aqueous solution. 89.62kg of artificial sylvite is taken, dissolved in water, clarified and filtered to obtain 253.45kg of solution with the concentration of 28-degree Be' and the turbidity of less than 5NTU for later use;
the fifth step: diluting the sylvite solution. 164.12kg of 28-degree Be 'sylvite solution is taken and diluted by adding water to 23-degree Be' to obtain 199.85kg of solution for later use;
building a solar pond, selecting cuboid evaporation ponds with the length of 1.00m, the width of 0.60m and the depth of 0.55m as the sylvite solar ponds, adding a heat-insulating layer, alternately and horizontally placing pipe ends at the bottom of the ponds for sealing, arranging a liquid taking and replenishing coil pipe with small holes on the whole body, covering layers of small stones on the pipe, and spreading 41.48kg of solid sylvite with the thickness of 3cm on the stones;
the seventh step: and (5) horizontally pouring the solar pond layer by layer. 89.33kg (0.072 m) of sylvite solution with turbidity less than 5NTU and concentration of 28 ° Be' obtained in the fourth step3) Horizontally perfusing the troposphere below the solar pond; 199.85kg (0.1682 m) of the sylvine solution with the concentration of 23 DEG Be' obtained in the fifth step3) The water is horizontally poured into a solar pond salt gradient layer, and the troposphere on the solar pond is poured with 30kg of fresh water (0.03 m)3)；
Eighth step: the solar pond is operated. The solar pond is operated under natural conditions that the daily average temperature is 15 ℃ and the relative humidity is 20%, the illumination in the daytime and the closing at night are carried out, and when the solution reaches a stable state, the temperature of the lower troposphere solution is 49 ℃; the concentration and the temperature of each layer of solution are regularly detected during the operation of the solar pond, and when the upper convection layer is thinned due to water evaporation, a proper amount of fresh water is supplemented to keep the stable operation of the solar pond;
the ninth step is to thermally dissolve the sylvite, 80.40kg of sylvite solution with the temperature of 49 ℃ is extracted from the bottom of the solar pond, 21.21kg of solid sylvite is added into the sylvite solution, and the mixture is heated to 91 ℃ to further dissolve the sylvite in the steps;
the tenth step: and (5) filtering. Filtering the sylvite solution obtained in the ninth step, removing 33.06kg of suspended impurities such as sodium chloride and the like, and evaporating 1.36kg of water to obtain 67.19kg of high-temperature mother liquor for later use;
and a tenth step of cooling and crystallizing, namely naturally cooling 67.19kg of the high-temperature mother liquor obtained in the tenth step to 16 ℃, crystallizing and separating out potassium chloride, filtering to obtain 54.42kg of filtrate, and drying the filter cake to obtain 12.77kg of potassium chloride with the content of 96.04%, which meets the product indexes of GB6549-2011 potassium chloride I type industrial potassium chloride and the like.
And twelfth step, performing liquid cooling recycling on the low-temperature mother liquor, adding 25.98kg of sylvite solution with the concentration of 28-degree Be' into 54.42kg of filtrate obtained in the tenth step to obtain 80.40kg of low-temperature mother liquor, and adding the low-temperature mother liquor into the lower convection layer of the solar pond for recycling.
Claims (1)
1, method for preparing potassium chloride by using low energy consumption of low-grade potassium resource ore, which is characterized by comprising the following preparation steps:
, decomposing low-grade potassium resource ores, namely dissolving quantitative flotation tailings in water at a solid-to-liquid ratio of 1: 0.7-1, and filtering to remove solid phases such as silt and undissolved substances to prepare potassium-dissolved brine for later use;
secondly, evaporating the potassium-dissolved brine to prepare sylvite and carnallite, namely taking quantitative potassium-dissolved brine, naturally evaporating and filtering to prepare a solid phase of sylvite and carnallite for later use;
thirdly, preparing artificial sylvite, namely adding water into quantitative mixed solid phase of the sylvite and carnallite for decomposition, wherein the solid-liquid ratio is 1: 0.3-0.6, further reduces the content of magnesium chloride, improves the content of potassium chloride, and filtering to prepare the artificial sylvite for later use;
fourthly, preparing a sylvite solution, namely dissolving quantitative artificial sylvite in water, and clarifying and filtering to obtain a sylvite solution with the concentration of 28-degree Be' and the turbidity of less than 5NTU for later use;
fifthly, diluting the sylvite solution, namely adding water into quantitative sylvite solution with the concentration of 28-degree Be 'to dilute the sylvite solution to 18-23-degree Be' for later use;
sixthly, building a solar pond, namely selecting cuboid evaporation ponds with the length of 1.00m, the width of 0.60m and the depth of 0.55m as the sylvine solar pond, adding a heat-insulating layer, alternately and horizontally placing pipe ends at the bottom of the solar pond for sealing, arranging a liquid taking and replenishing coil pipe with small holes on the whole body, covering layers of small stones on the pipe, and flatly paving a solid sylvine layer with the thickness of 3cm on the small stones;
and seventhly, horizontally pouring the solar pond layer by layer: taking 0.06-0.08 m of sylvite solution with turbidity less than 5NTU and concentration of 28-degree Be' obtained in the fourth step3Horizontally perfusing the troposphere below the solar pond; taking 0.16-0.18 m of the sylvite solution with the concentration of 18-23 degrees Be' obtained in the fifth step3Horizontally filling the solar pond with a salt gradient layer, and filling the solar pond with a convection layer of 0.03m3Fresh water;
the eighth step is to operate the solar pond: the method comprises the steps that the solar pond is operated under natural conditions of simulated daily average temperature of 15 ℃ and relative humidity of 20%, illumination is carried out in the daytime, the solar pond is closed at night, when the temperature of a solution of a lower convection layer is stable, the temperature is 45-50 ℃, the concentration and the temperature of each layer of solution are detected periodically during the operation of the solar pond, and when an upper convection layer is thinned due to water evaporation, a proper amount of fresh water is supplemented to keep the stable operation of the solar pond;
the ninth step of hot dissolving the sylvite, namely extracting quantitative sylvite solution with the temperature of 45-50 ℃ from the bottom of the solar pond, adding quantitative solid sylvite into the solution, heating the solution to 90-93 ℃, and further dissolving the sylvite in the step;
the tenth step is filtration: filtering the sylvite solution obtained in the ninth step, and removing suspended impurities such as sodium chloride and the like to obtain high-temperature mother liquor for later use;
cooling and crystallizing in a tenth step, namely naturally cooling the high-temperature mother liquor obtained in the tenth step to 15-20 ℃, separating out potassium chloride crystals, filtering and drying to obtain a potassium chloride product, and filtering to obtain low-temperature mother liquor for later use;
and a twelfth step of low-temperature mother liquor cold recycling, namely supplementing quantitative 28-degree Be' sylvite solution into the low-temperature mother liquor obtained in the tenth step, and adding the mixture into a convection layer below a solar pond for recycling.
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Cited By (1)
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| CN113135580A (en) * | 2021-06-01 | 2021-07-20 | 吉林海资生物工程技术有限公司 | Process for preparing artificial carnallite and potassium chloride by extracting potassium from corn soaking solution |
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| US5300136A (en) * | 1991-08-13 | 1994-04-05 | Imco Recycling, Inc. | Potassium fertilizer from aluminum reclamation by-products |
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| CN113135580A (en) * | 2021-06-01 | 2021-07-20 | 吉林海资生物工程技术有限公司 | Process for preparing artificial carnallite and potassium chloride by extracting potassium from corn soaking solution |
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Application publication date: 20200131 |