CN113772691B - Method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite - Google Patents
Method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite Download PDFInfo
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- CN113772691B CN113772691B CN202111074012.5A CN202111074012A CN113772691B CN 113772691 B CN113772691 B CN 113772691B CN 202111074012 A CN202111074012 A CN 202111074012A CN 113772691 B CN113772691 B CN 113772691B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01D3/04—Chlorides
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01D3/22—Preparation in the form of granules, pieces, or other shaped products
- C01D3/24—Influencing the crystallisation process
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses a method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite, which comprises the following steps: crushing low-sodium carnallite, adding the crushed low-sodium carnallite into a dissolving device, adding ultrapure water, and heating to completely dissolve the low-sodium carnallite to obtain a carnallite supersaturated solution; adding circulating mother liquor into a crystallizer in advance, and then adding carnallite supersaturated liquor into a first-stage crystallizer for crystallization to obtain first-stage crystal slurry; adding the first-stage crystal slurry into a second-stage crystallizer, and then adding carnallite supersaturated solution for crystallization to obtain a second-stage crystal slurry; adding the second-stage crystal slurry into a third-stage crystallizer, and then adding carnallite supersaturated solution for crystallization to obtain a third-stage crystal slurry; and (3) carrying out solid-liquid separation on the third-stage crystal slurry, recycling the obtained mother liquor, and washing and vacuum drying the obtained crystals sequentially to obtain the large-particle potassium chloride. The invention can obtain large-particle-size potassium chloride, and effectively solves the problems of small potassium chloride crystal, high moisture content, easy hardening and the like in the existing preparation method.
Description
Technical Field
The invention relates to the technical field of potassium chloride preparation, in particular to a method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite.
Background
The Chinese is a large agricultural country, and the development of agriculture is not separated from chemical fertilizers. According to investigation, 84% of land in China is deficient in potassium, which becomes one of important factors affecting agricultural development in China. Thus, the demand for potash fertilizer is enormous.
The biggest potash fertilizer production area in China is the Qinghai Bohr sweat salt lake, which is the biggest salt lake in China and is a typical chloride salt lake, and the potassium chloride production in the area mainly adopts reverse flotation and forward flotation processes, and also adopts hot melting crystallization and brine mixing processes. The reverse flotation-cold crystallization process is an advanced process, and the process technology is reliable, so that the produced potassium chloride product has a large content, a yield of about 60%, low energy consumption, low moisture content and other series of outstanding advantages, and becomes a main process route for producing the potassium chloride. However, the powder potassium chloride prepared by the process has fine particles, the average particle size is 0.1-0.2mm, and the potassium fertilizer cannot be ensured to completely enter the soil around the plant root system due to the defects of light weight, easy hardening after long-term placement, easy wind blowing and the like in the use of the potassium fertilizer, so that the resource waste is caused.
The most important characteristics in the crystallization process are high purity, uniform particle size distribution, stable reaction conditions, easy operation, low energy consumption and the like. The method for preparing large-particle potassium chloride by using continuous crystallization is a new way for improving the use efficiency of the potash fertilizer.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing large-particle potassium chloride by continuously crystallizing low-sodium carnallite, which can obtain large-particle potassium chloride and effectively solve the problems of small potassium chloride crystal, high moisture content, easy hardening and the like in the existing preparation method.
In order to achieve the above purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: there is provided a process for the preparation of large particle potassium chloride by continuous crystallization of low sodium carnallite comprising the steps of:
(1) Crushing low-sodium carnallite, adding the crushed low-sodium carnallite into a dissolving device, adding ultrapure water, and heating to 50-60 ℃ to completely dissolve the low-sodium carnallite to obtain a carnallite supersaturated solution;
(2) Adding circulating mother liquor into a first-stage crystallizer, a second-stage crystallizer and a third-stage crystallizer of the crystallizer in advance, and then adding the carnallite supersaturated liquor obtained in the step (1) into the first-stage crystallizer for crystallization to obtain first-stage crystal slurry; adding the first-stage crystal slurry into a second-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a second-stage crystal slurry; adding the second-stage crystal slurry into a third-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a third-stage crystal slurry;
(3) And (3) carrying out solid-liquid separation on the third-stage crystal slurry obtained in the step (2), recycling the mother liquor, and washing and vacuum drying the obtained crystals sequentially to obtain large-particle potassium chloride.
Further, in the step (1), the mass ratio of the low-sodium carnallite to the ultrapure water is 82-85:100.
Further, the mass ratio of low sodium carnallite to ultrapure water was 83:100.
Further, the circulating mother liquor is carnallite saturated liquor at normal temperature.
Further, the crystallizer is a jacketed crystallizer.
Further, in the step (2), the circulating mother liquor and the carnallite supersaturated liquor are mixed according to a volume ratio of 150:100.
Further, the temperatures of the first stage crystallizer, the second stage crystallizer and the third stage crystallizer were kept constant at room temperature.
Further, in the first-stage crystallizer, the second-stage crystallizer and the third-stage crystallizer, the stirring speed is 400-600r/min, the feeding speed is 3-3.5mL/min, and the residence time is 1-2h.
Further, in the first stage crystallizer, the second stage crystallizer and the third stage crystallizer, the stirring speed was 500r/min, the feeding rate was 3.3mL/min, and the residence time was 1h.
Further, the obtained crystals were washed with ethanol and then dried in vacuo at a temperature of 40-60℃for 24 hours.
Further, in the obtained large-particle potassium chloride, the ratio of crystal grains having a particle diameter of 1.0mm or more in the crystal was 50.28%, and the maximum particle diameter was 1.7mm.
In summary, the invention has the following advantages:
1. the invention prepares large-particle potassium chloride by continuously crystallizing low-sodium carnallite, directly mixing high-temperature carnallite saturated liquid with low-temperature carnallite saturated liquid, and preparing large-particle potassium chloride by natural crystallization; the large-particle-size potassium chloride effectively solves the problems of small potassium chloride crystal, high moisture content, easy hardening and the like in the existing preparation method.
2. The large-particle potassium chloride obtained by the invention has the crystal grain ratio of more than 1.0mm in the obtained crystal of 50.28 percent and the maximum particle size of 1.7mm, and solves the problems of more fine potassium chloride crystals, high moisture content, easy hardening and the like. During preparation, the three-stage crystallizers are connected in series, so that the cycle times of the mother liquor are improved, the growth time of potassium chloride crystals is prolonged, and the carnallite is directly used for preparing large-particle potassium chloride.
3. The invention prepares large-particle potassium chloride by a continuous crystallization method, circulates mother liquor for a plurality of times, effectively saves the production resource of potash fertilizer and provides a new way; the crystallization process has the advantages of stable reaction condition, easy operation, low energy consumption and the like.
4. The large-particle-size potassium chloride product obtained by the method has high purity, large particles, uniform particle size distribution and low moisture content, and effectively improves the utilization rate of the potassium fertilizer. The large-particle potassium chloride obtained by the method effectively solves the problems of small potassium chloride particles, easy hardening, high moisture content, high drying energy consumption cost, too fast slow release of the potassium fertilizer, too low use efficiency of the potassium fertilizer and the like.
Drawings
FIG. 1 is a graph showing the distribution of potassium chloride particle size in different processes;
FIG. 2 shows the average particle size of potassium chloride in different processes;
FIG. 3 shows the water content of potassium chloride in different processes.
Detailed Description
Example 1
A method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite, comprising the following steps:
(1) Crushing low-sodium carnallite, adding the crushed low-sodium carnallite into a dissolving device, adding ultrapure water, and heating to 50 ℃ to completely dissolve the low-sodium carnallite to obtain a carnallite supersaturated solution; the mass ratio of the low-sodium carnallite to the ultrapure water is 82:100;
(2) Adding circulating mother liquor into a first-stage crystallizer, a second-stage crystallizer and a third-stage crystallizer of the crystallizer in advance, wherein the circulating mother liquor is carnallite saturated liquid at normal temperature, and then adding the carnallite supersaturated liquid obtained in the step (1) into the first-stage crystallizer for crystallization to obtain first-stage crystal slurry; adding the first-stage crystal slurry into a second-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a second-stage crystal slurry; adding the second-stage crystal slurry into a third-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a third-stage crystal slurry; mixing the circulating mother liquor and carnallite supersaturated liquor according to the volume ratio of 150:100, wherein the temperatures of the first-stage crystallizer, the second-stage crystallizer and the third-stage crystallizer are kept constant at room temperature, the stirring speed is 500r/min, the feeding rate is 3.3mL/min, and the residence time is 1h;
(3) And (3) carrying out solid-liquid separation on the third-stage crystal slurry obtained in the step (2), recycling the mother liquor, washing with ethanol, and then carrying out vacuum drying at 50 ℃ for 24 hours to obtain large-particle potassium chloride.
Example 2
A method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite, comprising the following steps:
(1) Crushing low-sodium carnallite, adding the crushed low-sodium carnallite into a dissolving device, adding ultrapure water, and heating to 55 ℃ to completely dissolve the low-sodium carnallite to obtain a carnallite supersaturated solution; the mass ratio of the low-sodium carnallite to the ultrapure water is 83:100;
(2) Adding circulating mother liquor into a first-stage crystallizer, a second-stage crystallizer and a third-stage crystallizer of the crystallizer in advance, wherein the circulating mother liquor is carnallite saturated liquid at normal temperature, and then adding the carnallite supersaturated liquid obtained in the step (1) into the first-stage crystallizer for crystallization to obtain first-stage crystal slurry; adding the first-stage crystal slurry into a second-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a second-stage crystal slurry; adding the second-stage crystal slurry into a third-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a third-stage crystal slurry; mixing the circulating mother liquor and carnallite supersaturated liquor according to the volume ratio of 150:100, wherein the temperatures of the first-stage crystallizer, the second-stage crystallizer and the third-stage crystallizer are kept constant at room temperature, the stirring speed is 500r/min, the feeding rate is 3.3mL/min, and the residence time is 1h;
(3) And (3) carrying out solid-liquid separation on the third-stage crystal slurry obtained in the step (2), recycling the mother liquor, washing with ethanol, and then carrying out vacuum drying at 50 ℃ for 24 hours to obtain large-particle potassium chloride.
Example 3
A method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite, comprising the following steps:
(1) Crushing low-sodium carnallite, adding the crushed low-sodium carnallite into a dissolving device, adding ultrapure water, and heating to 60 ℃ to completely dissolve the low-sodium carnallite to obtain a carnallite supersaturated solution; the mass ratio of the low-sodium carnallite to the ultrapure water is 85:100;
(2) Adding circulating mother liquor into a first-stage crystallizer, a second-stage crystallizer and a third-stage crystallizer of the crystallizer in advance, wherein the circulating mother liquor is carnallite saturated liquid at normal temperature, and then adding the carnallite supersaturated liquid obtained in the step (1) into the first-stage crystallizer for crystallization to obtain first-stage crystal slurry; adding the first-stage crystal slurry into a second-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a second-stage crystal slurry; adding the second-stage crystal slurry into a third-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a third-stage crystal slurry; mixing the circulating mother liquor and carnallite supersaturated liquor according to the volume ratio of 150:100, wherein the temperatures of the first-stage crystallizer, the second-stage crystallizer and the third-stage crystallizer are kept constant at room temperature, the stirring speed is 500r/min, the feeding rate is 3.3mL/min, and the residence time is 1h;
(3) And (3) carrying out solid-liquid separation on the third-stage crystal slurry obtained in the step (2), recycling the mother liquor, washing with ethanol, and then carrying out vacuum drying at 50 ℃ for 24 hours to obtain large-particle potassium chloride.
Experimental example
The existing technology for producing potassium chloride comprises reverse flotation-cold crystallization, cold crystallization-forward flotation, hot melting vacuum crystallization, brine-blended cold crystallization and the like, wherein the reverse flotation-cold crystallization method is the technology which is preferentially selected by potash fertilizer production enterprises. The results of reverse flotation-cold crystallization and potassium chloride prepared by the method are characterized by the conventional preparation method, and the results are shown in figure 1. In FIG. 1, the highest peaks are reverse flotation-cold crystallization, 55 ℃, 50 ℃ and 60 ℃ in that order from left to right.
As can be seen from FIG. 1, the potassium chloride prepared by the conventional method has small particle size and average particle size of 0.15mm, and the preparation method has remarkable effect on increasing the particle size of the potassium chloride. By changing the key conditions (initial cooling temperature) in the preparation method, the result shows that the particle size is larger as the initial cooling temperature is higher, and when the initial cooling temperature is 50 ℃, the crystal grain ratio of more than 1mm in the crystal is 14.7%, and the average particle size is 0.621mm. When the initial cooling temperature is 55 ℃, the grain ratio of more than 1mm in the obtained crystal is 22.28%, and the average grain diameter is 0.637mm; when the initial cooling temperature is 60 ℃, the grain with the grain diameter of more than 1mm in the obtained crystal accounts for 50.28 percent. The average particle diameter was 0.875mm.
And the water content and average particle size of the potassium chloride prepared by the conventional method and the application are characterized, and the results are respectively shown in figures 2-3. In fig. 3, the reverse flotation-cold crystallization and the process of the present application are shown from top to bottom, respectively.
As can be seen from FIGS. 2 and 3, the wet content of the potassium chloride crystals prepared by the conventional method is as high as 6.93%, the crystals are more fine, and the average particle size is 0.15mm; the moisture content of the potassium chloride crystal prepared by the method is 2.67%, and the average particle size is 0.875mm.
Although specific embodiments of the invention have been described in detail with reference to the accompanying drawings, it should not be construed as limiting the scope of protection of the present patent. Various modifications and variations which may be made by those skilled in the art without the creative effort are within the scope of the patent described in the claims.
Claims (9)
1. A process for the preparation of large-particle potassium chloride by continuous crystallization of low sodium carnallite, comprising the steps of:
(1) Crushing low-sodium carnallite, adding the crushed low-sodium carnallite into a dissolving device, adding ultrapure water, and heating to 50-60 ℃ to completely dissolve the low-sodium carnallite to obtain a carnallite supersaturated solution;
(2) Adding circulating mother liquor into a first-stage crystallizer, a second-stage crystallizer and a third-stage crystallizer of the crystallizer in advance, and then adding the carnallite supersaturated liquor obtained in the step (1) into the first-stage crystallizer for crystallization to obtain first-stage crystal slurry; adding the first-stage crystal slurry into a second-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a second-stage crystal slurry; adding the second-stage crystal slurry into a third-stage crystallizer, and then adding the carnallite supersaturated solution obtained in the step (1) for crystallization to obtain a third-stage crystal slurry; the circulating mother liquor is carnallite saturated liquor at normal temperature;
(3) And (3) carrying out solid-liquid separation on the third-stage crystal slurry obtained in the step (2), recycling the mother liquor, and washing and vacuum drying the obtained crystals sequentially to obtain large-particle potassium chloride.
2. The method for producing large-particle potassium chloride from continuous crystallization of low-sodium carnallite according to claim 1, wherein in the step (1), the mass ratio of low-sodium carnallite to ultrapure water is 82 to 85:100.
3. The method for producing large-particle potassium chloride by continuous crystallization of low-sodium carnallite according to claim 2, wherein the mass ratio of low-sodium carnallite to ultrapure water is 83:100.
4. The method for preparing large-particle potassium chloride from continuous crystallization of low-sodium carnallite according to claim 1, wherein the crystallizer is a jacketed crystallizer.
5. The method for preparing large-particle potassium chloride from low-sodium carnallite continuous crystallization according to claim 1, wherein in step (2), the circulating mother liquor and the carnallite supersaturated solution are mixed in a volume ratio of 150:100.
6. The method for preparing large-particle potassium chloride from continuous crystallization of low-sodium carnallite according to claim 1, wherein the temperatures of the first stage crystallizer, the second stage crystallizer, and the third stage crystallizer are kept constant at room temperature.
7. The method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite according to claim 1, wherein the stirring speed is 400-600r/min, the feeding speed is 3-3.5mL/min and the residence time is 1-2h in the first stage crystallizer, the second stage crystallizer and the third stage crystallizer.
8. The method for preparing large-particle potassium chloride from continuous crystallization of low-sodium carnallite according to claim 1, wherein the obtained crystals are washed with ethanol and then dried in vacuum at a temperature of 40 to 60 ℃ for 24 hours.
9. The method for preparing large-particle potassium chloride by continuous crystallization of low-sodium carnallite according to claim 1, wherein the obtained potassium chloride crystals have a grain ratio of 50.28% of 1mm or more, an average grain size of 0.875mm and a maximum grain size of 1.7mm.
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| US8282898B2 (en) * | 2009-11-23 | 2012-10-09 | Karnalyte Resources Inc. | Process for the formulation of potassium chloride from a carnallite source |
| CN102491373B (en) * | 2011-12-22 | 2013-08-14 | 化工部长沙设计研究院 | Method for producing potassium chloride, sodium chloride and magnesium sheet from bittern extracted from carnallite mine |
| CN104058428B (en) * | 2014-07-10 | 2015-08-26 | 青海盐湖工业股份有限公司 | KCl production system and method produced by a kind of novel carnallitite |
| CN107739037A (en) * | 2017-11-16 | 2018-02-27 | 中国科学院青海盐湖研究所 | A kind of method that carnallite prepares big particle diameter potassium chloride |
| CN108862328B (en) * | 2018-06-29 | 2021-04-30 | 青海盐湖工业股份有限公司 | Process for producing potassium chloride by utilizing carnallite ore |
| CN111170336B (en) * | 2020-02-24 | 2022-04-22 | 青海盐湖工业股份有限公司 | Method for preparing potassium chloride from carnallite raw ore |
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