CN111470519B - Method for preparing potassium chloride by using high-sodium carnallite - Google Patents
Method for preparing potassium chloride by using high-sodium carnallite Download PDFInfo
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Abstract
The invention discloses a method for preparing potassium chloride by using high-sodium carnallite. The method comprises the following steps: first enriched in MgCl2Mixing the substances with fresh water and carrying out preheating treatment to obtain a hot solvent; then carrying out selective hot-melting treatment on the high-sodium carnallite by using the hot solvent to obtain high-temperature potassium-rich saturated solution; and finally, carrying out stepped closed cooling crystallization and refining treatment on the obtained high-temperature potassium-rich saturated liquid to obtain the potassium chloride. According to the invention, the high-sodium carnallite is subjected to selective hot dissolution through the hot solvent, so that the rapid separation of sodium chloride and carnallite is realized, and meanwhile, the decomposition stage of carnallite is saved, and the water resource is saved; meanwhile, by controlling the process parameters, the high-efficiency and high-quality precipitation of the potassium chloride is ensured. The method provided by the invention has mild conditions and simple method, and is convenient for popularization and implementation of the technology.
Description
Technical Field
The invention belongs to the technical field of inorganic salt industry, and particularly relates to a method for preparing potassium chloride by using high-sodium carnallite.
Background
The potash fertilizer is a basic material for the stable growth of grain production, can effectively improve the quality of agricultural products and the stress resistance of crops, and is one of the nutrients necessary for the growth of the crops. With the reduction of the cultivated land area and the continuous increase of population, the potassium resource is developed on a large scale, the yield of the potassium fertilizer is improved, and the method has important food safety significance.
The potassium fertilizer product type is mainly potassium chloride fertilizer and accounts for more than 90 percent of the total amount of the potassium fertilizer. The raw materials for preparing the potassium chloride fertilizer mainly comprise sylvite and carnallite, and along with long-time scale development, the carnallite at the present stage is mainly high-sodium carnallite which comprises 30-60 percent of NaCl, 10-20 percent of KCl and MgCl2 15％～30％，H215 to 30 percent of O, and the mass ratio of the sodium chloride to the potassium chloride is as high as 1.5:1 to 6.0:1, thereby providing difficulty for preparing the potassium chloride fertilizer from the carnallite.
At present, the method for preparing potassium chloride by using carnallite mainly comprises the following steps:
(1) cold decomposition-washing method: the technological process includes decomposing carnallite completely to obtain artificial sylvine, washing with water and drying to obtain potassium chloride product. However, the technology is only suitable for carnallite with extremely low NaCl content, the water addition amount is increased along with the increase of the NaCl content, the KCl yield is gradually reduced, and the technology is eliminated;
(2) cold decomposition-flotation: the technical process comprises the steps of completely decomposing carnallite in fresh water or refined potassium mother liquor to obtain artificial sylvite, then carrying out flotation by adopting a positive flotation collector (mainly an amine collector), washing a solid phase after flotation by adding water, and drying to obtain a finished product of potassium chloride, wherein the technical process can be seen in figure 1. The technique is also applicable to carnallite mixed with sylvite (patent CN 1094466C). Further, patent CN102442687B adopts a rotary decomposer to perform cold decomposition, selectively fractionally separate coarse particle NaCl, and perform flotation on the remaining pulp to obtain qualified KCl concentrate; patent CN107188200B adopts a multi-stage screening system to separate cold decomposed slurry to sequentially obtain coarse grain NaCl, coarse grain KCl and fine grain KCl slurry, and the fine grain KCl slurry is subjected to flotation separation to obtain KCl concentrate; the two technologies greatly improve the product quality of the potassium chloride. Although the technology for producing potassium chloride saves energy sources, has less factory-building investment and simple and easily-mastered technology, the obtained product has fine granularity, poor physical properties and low potassium yield which is generally 50-60 percent. The product has poor physical properties, the granularity of more than 100 meshes in the product only accounts for 10-20 percent, and the product is gradually difficult to adapt to the requirements of the international market, the technology is greatly influenced by the type of carnallite, and when the NaCl content in the carnallite is high, the grade and yield of KCl are greatly reduced;
(3) reverse flotation-cold crystallization: the technical process comprises the steps of firstly removing NaCl from carnallite ore through reverse flotation to obtain low-sodium carnallite, carrying out cold decomposition and crystallization on the low-sodium carnallite, and then screening, filtering, washing and drying to obtain a potassium chloride product, wherein the technical process can be seen in figure 2. On the basis of the original process, the patents CN104058427A and CN107572552A introduce a screening system before reverse flotation, large-particle NaCl is preferentially screened, the NaCl content in the low-sodium carnallite is further reduced, and the stable operation of cold crystallization is ensured. Although the quality of the potassium chloride product produced by the technology is high and can reach about 95 percent, the product has coarse granularity and good appearance effect. But the process is complex, the operation is not easy (especially a crystallization system), the requirement on raw ores is high, and the dependence is strong;
(4) brine adding-speed controlling crystallization method: the technology is that mother liquor (carnallite saturation point) of potassium chloride, sodium chloride and carnallite cosaturation is mixed with mother liquor (bischofite saturation point) of magnesium chloride, sodium chloride and carnallite cosaturation, low-sodium carnallite is separated out due to supersaturation of potassium and magnesium, the mixture enters a crystallizer after concentration and liquid removal, high-grade potassium chloride is obtained after adding fresh water for decomposition and crystallization, and the technical flow of the halogen blending method can be seen in figure 3. Although the technology has the obvious advantages of simple process flow, excellent product quality, low capital construction investment, low production cost, high operation recovery rate, high resource utilization rate, no environmental pollution and the like, the technology takes decomposed mother liquor as a raw material, the production scale cannot be randomly enlarged, only depends on a large-scale flotation plant, and the yield is lower;
(5) sun-drying method: the technical process comprises the steps of dissolving carnallite ores obtained by solarizing intercrystalline brine again with fresh water, discharging the carnallite ores into a potassium salt pool, independently separating out potassium chloride in the potassium salt pool, concentrating the brine in the potassium salt pool until the sodium chloride is saturated, and carrying out solarization and cyclic utilization on the brine at the moment, wherein the brine is sylvite brine, and the technological process of the solarization method can be shown in a figure 4. Although the solarization method technology fully utilizes solar energy, no medicament is added, the product quality is good, the granularity of the precipitated potassium chloride is generally more than 0.2mm, the purity is high, the yield is low, and the influence of climate conditions is large;
(6) cold decomposition-hot melt crystallization method: the technical process comprises the steps that after carnallite is completely decomposed by fresh water to obtain artificial sylvite, according to the principle that the solubility of sodium chloride and potassium chloride has different trend along with the change of temperature, the sodium chloride in the artificial sylvite is removed by hot dissolution of the fresh water, and the mother liquor is cooled and crystallized to obtain the potassium chloride, and the technical process flow chart can be seen in figure 5. Although the potassium chloride product obtained by the technology has the advantages of large and uniform granularity, good physical property, high product purity, high potassium recovery rate and less equipment investment, the technology has the advantages of high energy consumption, high cost, serious equipment corrosion and more complex process operation, and is generally suitable for popularization and use in areas with low energy sources.
On the basis of the original process, the patent CN102583446B utilizes old brine to fully thermally dissolve low-sodium carnallite ore at high temperature to obtain a hot solution, and the hot solution is cooled to separate out potassium chloride; in the patent CN103193252B, carnallite is decomposed by high-temperature potassium-rich brine to obtain artificial sylvite, and then the artificial sylvite is treated by a hot-melt crystallization process to prepare potassium chloride, in the invention, carnallite hot-melt brine is adopted instead of carnallite decomposed by fresh water, and the decomposition efficiency of carnallite is extremely low because the concentration of K ions in the hot-melt brine is very high; meanwhile, a large amount of decomposed solid phase is still in the form of fine-grain sylvite except a small amount of large-grain KCl, and the overall effect is poor.
Generally, the technical effect of preparing potassium chloride from carnallite ore at the present stage is closely related to the content of sodium chloride in the carnallite ore, the higher the content of sodium chloride is, the lower the yield and grade of potassium chloride are, and particularly for high-sodium carnallite ore, the actual effect is not ideal.
Disclosure of Invention
The invention mainly aims to provide a method for preparing potassium chloride by using high-sodium carnallite, so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for preparing potassium chloride by using high-sodium carnallite, which comprises the following steps:
will be rich in MgCl2Mixing the substances with fresh water and carrying out preheating treatment to obtain a hot solvent;
carrying out selective hot-melting treatment on the high-sodium carnallite by using the hot solvent to obtain high-temperature potassium-rich saturated solution;
and carrying out stepped closed cooling crystallization and refining treatment on the high-temperature potassium-rich saturated solution to obtain potassium chloride.
In the invention, (1) the temperature of the initial hot solvent is increased by recycling heat in the cooling and crystallization process, so that high-concentration MgCl is ensured2The type thermal solvent (near saturation) has extremely strong uniformity and stability; (2) the advantage of increased solubility of potassium chloride and magnesium chloride can be fully exerted by high-temperature selective hot melting, so that the high-sodium carnallite is fully dissolved; controlling both liquid and solid of high sodium carnallite and hot solventThe mass ratio of the sodium chloride to the saturated solution is small, so that the selective dissolution of different phases in the high-sodium carnallite is realized; (3) by controlling the concentration of the hot solvent and the liquid-solid mass ratio in the hot dissolving process, the composition of a high-temperature potassium-rich saturated liquid obtained by hot dissolving is favorable to be close to the three-phase common saturation point of carnallite, potassium chloride and sodium chloride, the composition stability of the saturated liquid is strong, and the independent separation of potassium chloride in the cooling crystallization process is favorable; (4) the temperature difference between the hot melting and the cooling crystallization is large, so that the maximum separation of potassium chloride in the high-temperature potassium-rich saturated solution is ensured; (5) in the cooling crystallization process, the temperature is slowly reduced in a stepped manner in a closed space, and the amount of supplemented fresh water and/or refined potassium mother liquor is controlled, so that sodium chloride, magnesium chloride and other salts in the high-temperature potassium-rich saturated solution can be always stably remained in a liquid phase in the cooling process, and only potassium chloride is separated out; (6) the cooling crystallization temperature is the same as the washing temperature, which is favorable for perfect conjunction of the process stage.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention utilizes the characteristics of different solubility change trends of potassium chloride, magnesium chloride and sodium chloride to cooperate with MgCl2The solvent is used for carrying out selective hot-dissolving treatment on the high-sodium carnallite, and the mass ratio of sodium chloride to potassium chloride in the obtained potassium-rich saturated solution is only 0.30: 1-0.35: 1, so that the rapid separation of the sodium chloride and the carnallite is realized, and compared with the traditional decomposition process, the selective hot-dissolving process has the advantages of better separation effect, omission of the decomposing stage of the carnallite and water resource saving;
(2) according to the invention, by controlling the concentration of the hot solvent and the liquid-solid mass ratio in the hot dissolving process, the stability of the composition of the high-temperature potassium-rich saturated liquid obtained by hot dissolving and the unsaturation degree of other salts such as sodium chloride and magnesium chloride in the cooling crystallization process are ensured, and the efficient and high-quality precipitation of potassium chloride is facilitated;
(3) the method provided by the invention has mild conditions, no extremely high or low temperature or other special condition setting, simple method and convenience for popularization and implementation of the technology.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a technical flow diagram of a prior art intercooling decomposition-flotation process;
FIG. 2 is a technical flow diagram of a reverse flotation-cold crystallization process in the prior art;
FIG. 3 is a technical flow chart of a brine-adding controlled-rate crystallization method in the prior art;
FIG. 4 is a flow chart of a prior art solarization process;
FIG. 5 is a prior art process flow diagram of a cold decomposition-hot melt crystallization process;
fig. 6 is a schematic flow chart of a method for preparing potassium chloride by using high-sodium carnallite in one embodiment of the invention.
Detailed Description
The core stage of the technology for preparing potassium chloride from carnallite ore is the process of decomposing to obtain artificial sylvine, and the yield and grade of potassium chloride are closely related to the content of sodium chloride in the carnallite ore. The higher the sodium chloride content, the lower the potassium chloride yield and grade.
In view of the defects of the prior art, the inventor of the present invention provides a technical scheme of the present invention through long-term research and a large amount of practice, which mainly omits a decomposition stage, selectively thermally dissolves the high-sodium carnallite to obtain potassium-rich brine, and then cools and crystallizes to prepare a potassium chloride product, thereby simplifying a process flow and realizing the development and utilization of potassium resources in the high-sodium carnallite. The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
One aspect of an embodiment of the present invention provides a method for preparing potassium chloride from high-sodium carnallite, which includes:
will be rich in MgCl2Mixing the substances with fresh water and carrying out preheating treatment to obtain a hot solvent;
carrying out selective hot-melting treatment on the high-sodium carnallite by using the hot solvent to obtain high-temperature potassium-rich saturated solution;
and carrying out stepped closed cooling crystallization and refining treatment on the high-temperature potassium-rich saturated solution to obtain potassium chloride.
In some more specific embodiments, the method for preparing potassium chloride by using high sodium carnallite specifically comprises:
(1) will be rich in MgCl2Mixing the substances with fresh water and preheating to 40-50 ℃ to obtain a hot solvent, wherein MgCl is contained in the hot solvent2The concentration of (A) is 25-30 wt%;
(2) contacting the hot solvent obtained in the step (1) with high-sodium carnallite, carrying out selective hot-melting treatment at 75-100 ℃, and then carrying out solid-liquid separation on the obtained mixture to obtain high-temperature potassium-rich saturated solution and solid-phase sodium chloride;
(3) and (3) while supplementing fresh water, performing stepped closed cooling crystallization on the high-temperature potassium-rich saturated liquid obtained in the step (2), performing solid-liquid separation treatment to obtain crude potassium chloride and low-temperature potassium saturated liquid, and then refining the obtained crude potassium chloride to obtain potassium chloride.
In some more specific embodiments, the MgCl-enriched material is MgCl2The substance (b) includes any one of old brine and bischofite, but is not limited thereto.
Further, the components of the aged brine comprise the following components in percentage by mass: MgCl230～33wt％，NaCl 0.1～0.5wt％，KCl 0.1～0.5wt％。
Further, the mass ratio of the hot solvent to the high-sodium carnallite is 2: 1-3: 1.
Further, the components of the high-sodium carnallite comprise the following components in percentage by mass: 30-60 wt% of NaCl, 10-20 wt% of KCl, and MgCl2 15～30wt％、H2O 15～30wt％。
Further, the high-temperature potassium-rich saturated liquid comprises the following components in percentage by mass: 1.8-2.0 wt% of NaCl, 5.4-6.4 wt% of KCl, and MgCl2 28～30wt％、H2O 61～65wt％。
Furthermore, the mass ratio of NaCl to KCl in the high-temperature potassium-rich saturated solution is 0.30: 1-0.35: 1.
In some more specific embodiments, the step-wise closed cooling crystallization treatment in step (3) comprises: cooling the high-temperature potassium-rich saturated liquid to a cooling crystallization temperature at a selected cooling rate while replenishing fresh water, and performing stepped cooling and closed cooling crystallization, wherein the cooling crystallization temperature is 10-25 ℃, and the selected cooling rate is 0.3-0.5 ℃/min; preferably, the mass ratio of the fresh water to the high-temperature potassium-rich saturated liquid is 0.15: 1-0.20: 1; by controlling the addition amount of the fresh water, the method ensures that other salts such as sodium chloride, magnesium chloride and the like in the high-temperature potassium-rich saturated liquid can be stably remained in a liquid phase all the time in the cooling process, and only potassium chloride is separated out.
Further, the method further comprises: and preheating the hot solvent by using the heat released in the stepped closed cooling crystallization treatment process.
In some more specific embodiments, the crude potassium chloride in step (3) has a potassium chloride content of 80 to 85 wt%.
Further, the low-temperature potassium saturated liquid comprises the following components in percentage by mass: 1.5-2.0 wt% of NaCl, 2.5-3.5 wt% of KCl, and MgCl2 25～27wt％、H2O 69～70wt％。
In some more specific embodiments, the method further comprises: and (4) preparing the low-temperature potassium saturated solution in the step (3) to form the hot solvent.
In some more specific embodiments, the refining treatment in step (3) comprises: and washing, solid-liquid separation and drying the obtained crude potassium chloride.
Further, the washing liquid used in the washing process includes fresh water, and is not limited thereto.
Further, the liquid-solid mass ratio of the washing liquid to the crude potassium chloride is 0.20: 1-0.30: 1.
Further, the temperature of the washing treatment is 10-25 ℃.
Further, while the stepwise closed cooling crystallization treatment and the fine invention obtained by the solid-liquid separation treatment were carried out on the premise of the above-mentioned technical solutions, detailed embodiments and specific procedures were given, but the scope of the present invention is not limited to the following examples.
The experimental materials used in the examples used below were all available from conventional biochemical reagents companies, unless otherwise specified.
The following examples (examples 1-3) were all obtained by the following steps:
(1) and (4) preparing a hot solvent. The hot solvent is prepared from aged brine, bischofite or low-temperature potassium saturated solution rich in MgCl2Mixing the salt ore body with fresh water.
(2) And (4) selectively hot-dissolving the high-sodium carnallite to obtain high-temperature potassium-rich saturated solution. The selective hot-dissolving of high-sodium carnallite is carried out by using a hot solvent, and the phase composition of the hot solution is kept stable as the sign of the completion of the hot-dissolving. And after the selective hot melting is finished, carrying out solid-liquid separation to obtain high-temperature potassium-rich saturated liquid, wherein the rest solid phase is sodium chloride, and the carnallite completely enters the saturated liquid.
(3) Closing the high-temperature potassium-rich saturated liquid, cooling and crystallizing to obtain crude potassium chloride.
(4) Refining the crude potassium chloride to prepare a potassium chloride product. And washing and drying the crude potassium chloride to finally obtain a potassium chloride product.
Example 1
Example 2
Example 3
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the invention.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (10)
1. A method for preparing potassium chloride by using high-sodium carnallite is characterized by comprising the following steps:
(1) will be rich in MgCl2Mixing the substances with fresh water and preheating to 40-50 ℃ to obtain a hot solvent, wherein MgCl is contained in the hot solvent2The concentration of (A) is 25-30 wt%;
(2) contacting the hot solvent obtained in the step (1) with high-sodium carnallite, carrying out selective hot-dissolving treatment at 75-100 ℃, and then carrying out solid-liquid separation on the obtained mixture to obtain high-temperature potassium-rich saturated liquid and solid-phase sodium chloride; the mass ratio of the hot solvent to the high-sodium carnallite is 2: 1-3: 1, and the high-sodium carnallite comprises the following components in percentage by mass: 30-60 wt% of NaCl, 10-20 wt% of KCl, and MgCl2 15~30 wt%、H215-30 wt% of O; the high-temperature potassium-rich saturated liquid comprises the following components in percentage by mass: 1.8-2.0 wt% of NaCl, 5.4-6.4 wt% of KCl, and MgCl228~30 wt%、H2O 61~65 wt%；
(3) Step-type closed cooling crystallization is carried out on the high-temperature potassium-rich saturated liquid obtained in the step (2) while fresh water is supplemented, then solid-liquid separation treatment is carried out to obtain crude potassium chloride and low-temperature potassium saturated liquid, and then the obtained crude potassium chloride is refined to obtain potassium chloride;
wherein the step-type closed cooling crystallization treatment in the step (3) comprises the following steps: cooling the high-temperature potassium-rich saturated liquid to a cooling crystallization temperature at a selected cooling rate while replenishing fresh water, and performing stepped cooling and closed cooling crystallization, wherein the cooling crystallization temperature is 10-25 ℃, and the selected cooling rate is 0.3-0.5 ℃/min; the mass ratio of the fresh water to the high-temperature potassium-rich saturated liquid is 0.15: 1-0.20: 1.
2. The method for preparing potassium chloride by using high-sodium carnallite according to claim 1, characterized in that: said MgCl-rich2The substances of (a) include old brine and/or bischofite; the components of the aged brine comprise the following components in percentage by mass: MgCl230~33wt%、NaCl 0.1~0.5wt %、KCl 0.1~0.5wt %。
3. The method for preparing potassium chloride by using high-sodium carnallite according to claim 1, characterized in that: the mass ratio of NaCl to KCl in the high-temperature potassium-rich saturated solution is 0.30: 1-0.35: 1.
4. The method for preparing potassium chloride by using high-sodium carnallite according to claim 1, further comprising: and preheating the hot solvent by using the heat released in the stepped closed cooling crystallization treatment process.
5. The method for preparing potassium chloride by using high-sodium carnallite according to claim 1, characterized in that: and (3) the content of potassium chloride in the crude potassium chloride is 80-85 wt%.
6. The method for preparing potassium chloride by using high-sodium carnallite according to claim 1, characterized in that: the low-temperature potassium saturated liquid comprises the following components in percentage by mass: 1.5-2.0 wt% of NaCl, 2.5-3.5 wt% of KCl, and MgCl225~27wt%、H2O 69~70wt%。
7. The method for preparing potassium chloride by using high-sodium carnallite according to claim 1, characterized by further comprising: and (4) preparing the low-temperature potassium saturated solution in the step (3) to form the hot solvent.
8. The method for producing potassium chloride using high-sodium carnallite according to claim 1, wherein said refining treatment in step (3) comprises: and washing, solid-liquid separation and drying the obtained crude potassium chloride.
9. The method for preparing potassium chloride by using high-sodium carnallite according to claim 8, characterized in that: the washing liquid adopted in the washing treatment comprises fresh water; the liquid-solid mass ratio of the washing liquid to the crude potassium chloride is 0.20: 1-0.30: 1; the temperature of the washing treatment is 10-25 ℃.
10. The method for preparing potassium chloride by using high-sodium carnallite according to claim 1, characterized by further comprising: adding the refined potassium mother liquor obtained by the solid-liquid separation treatment into the stepped closed cooling crystallization treatment system while performing the stepped closed cooling crystallization treatment; the mass ratio of the refined potassium mother liquor to the high-temperature potassium-rich saturated liquor is 0.15: 1-0.20: 1.
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