CN113247920A - Method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate - Google Patents
Method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate Download PDFInfo
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- CN113247920A CN113247920A CN202110565133.3A CN202110565133A CN113247920A CN 113247920 A CN113247920 A CN 113247920A CN 202110565133 A CN202110565133 A CN 202110565133A CN 113247920 A CN113247920 A CN 113247920A
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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
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
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Abstract
The invention discloses a method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate, belonging to the field of salt chemical industry, firstly injecting sulfate type brine into a sodium chloride stage salt field for carrying out stage solarization to obtain potash mixed salt ore and carnallite, and then crushing, ball-milling, converting, floating and filtering the potash mixed salt ore by a potash magnesium sulphate fertilizer system to obtain potash magnesium sulphate fertilizer; decomposing, floating and filtering carnallite ore by a potassium chloride system to obtain potassium chloride; adding water into the potash magnesium sulphate fertilizer and the potassium chloride, stirring, performing fresh water conversion reaction, crystallizing and filtering to obtain the potassium sulfate, and achieving the purpose of co-producing the potash magnesium sulphate fertilizer, the potassium chloride and the potassium sulfate.
Description
Technical Field
The invention relates to a production method for sun-curing potassium mixed salt and carnallite ore by sulfate brine in sections and co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulfate, belonging to the field of salt chemical industry.
Background
The potash fertilizer is essential nutrient for crop growth, scientific and reasonable fertilization is important for crop yield increase and efficiency increase according to the requirements of different crops and soil, and in order to meet the diversity of crop potash fertilizer products, the market development trends of three products, namely potash magnesium sulphate fertilizer, potassium chloride and potassium sulfate are different, and different potash fertilizer products can be flexibly regulated and produced according to the market development trends.
The potassium mixed salt ore and the carnallite ore are prepared from the sulfate type brine, and the prepared potassium mixed salt ore and the carnallite ore have larger difference of chemical components due to the early-late temperature difference of a lake region and the grade difference of surface water and inter-crystal brine of the brine lake. Therefore, the quality of the produced potash magnesium sulphate fertilizer, especially the quality of potassium chloride, fluctuates greatly along with the change of the content of the sulphate in the carnallite ore, so that the quality of the product is difficult to regulate and control, and the yield of potassium ions is lower. In order to comprehensively, scientifically and reasonably utilize raw ores of salt lake potassium resources and avoid the waste of the salt lake potassium resources, the production of different potassium fertilizers is reasonably adjusted according to the raw ores with different components.
Disclosure of Invention
The invention aims to provide a method for co-producing a potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate, which takes sulfate type brine to sun-cure potassium mixed salt and carnallite ore as raw materials to co-produce the potash magnesium sulphate fertilizer, the potassium chloride and the potassium sulphate.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for coproducing a potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate comprises the following steps:
injecting sulfate brine into a sodium chloride stage salt field for beach drying in stages, wherein the sulfate brine comprises the following ions in mass fraction: [ K ]+]0.4-0.81wt％、[Mg2+]0.9-2.45wt％、[SO4 2-]1.22-2.85wt％、[Cl-]13.88-15.51wt％；
The first stage is to solarize part of sulfate brine naturally until meeting the indexes of potassium mixed salt stage, wherein the indexes are that the mass fraction of ions in the brine is as follows: [ K ]+]≥2.16wt％、[Mg2+]≥4wt％、[SO4 2-]≥4.2wt％、[Cl-]Not less than 15.2 wt%, and then injecting into potassium mixed salt field and naturally solarizing into potassium mixed salt mine;
and the second stage is to naturally solarize part of the sulfate brine to meet the index of the carnallite stage, wherein the index refers to the mass fraction of ions in the brine: [ K ]+]≤1.81wt％、[Mg2+]≥6.3wt％、[SO4 2-]≤3.94wt％、[Cl-]Not less than 17.7 wt%, and then injecting into carnallite salt field to naturally solarize into carnallite;
and the third stage is to naturally dry the remaining sulfate brine on the beach to meet the index of the old brine stage, wherein the index refers to the mass fraction of ions in the brine as follows: [ K ]+]≤0.11wt％、[Mg2+]≥8.2wt％、[SO4 2-]≤2.83wt％、[Cl-]Not less than 22.4 wt%, and then injecting into old brine salt field;
crushing, ball-milling, converting, floating and filtering the potassium mixed salt ore by a potassium magnesium sulfate fertilizer system to obtain a potassium magnesium sulfate fertilizer;
decomposing, floating and filtering carnallite ore by a potassium chloride system to obtain potassium chloride;
adding water into the potash magnesium sulphate fertilizer and the potassium chloride, stirring, performing fresh water conversion reaction, crystallizing and filtering to obtain the potassium sulphate.
Further, the mass fraction of ions in the potassium mixed salt ore: [ K ]+]3.5-7.5wt％、[Mg2+]3-8wt％、[SO4 2-]12-28wt％、 [Cl-]20-35wt％。
Further, the mass fraction of ions in the carnallite: [ K ]+]4.0-10wt％、[Mg2+]5-10wt％、[SO4 2-]1-15wt％、 [Cl-]20-35wt％。
Further, in the process of crushing, ball-milling, converting, floating and filtering the potassium mixed salt ores to obtain the potash magnesium sulphate fertilizer, the content of chloride ions in the potash magnesium sulphate fertilizer product is regulated and controlled according to the yield of potassium chloride; when the yield of potassium chloride is higher than the proportion of the yield of the potash magnesium sulphate fertilizer, the content of chloride ions in the potash magnesium sulphate fertilizer is regulated to be 2.5-4 wt% and the potash magnesium sulphate fertilizer is used for producing potassium sulphate with the mixture of potassium chloride; when the yield of the potassium chloride is lower than the yield proportion of the potash magnesium sulphate fertilizer, water is added to regulate the content of chloride ions in the potash magnesium sulphate fertilizer to be less than or equal to 2.5 wt%.
Further, in the process of decomposing, floating and filtering the carnallite ore to obtain potassium chloride, the potassium chloride content in the potassium chloride product is regulated and controlled according to the yield of the potash magnesium sulphate fertilizer; when the yield of the potash magnesium sulphate fertilizer is higher than the proportion of the yield of potassium chloride, regulating and controlling the potassium chloride content in the potassium chloride product to be 50-75 wt% for producing potassium sulphate with the potash magnesium sulphate fertilizer; when the yield of the potash magnesium sulphate fertilizer is lower than the proportion of the potassium chloride yield, water is added to regulate the potassium chloride content in the potassium chloride product to be more than or equal to 80 wt%.
Further, the potassium magnesium sulfate fertilizer product conforms to GB/T20937-2018, the potassium chloride product conforms to GB/T37918-2019, and the potassium sulfate product conforms to GB/T20406-2017.
Further, the sulfate type brine contains K+、Na+、Mg2+、Cl-、SO4 2-And (3) plasma.
Furthermore, the concentration of the ball milling slurry of the potash magnesium sulphate fertilizer system is 60-70 wt%, and the granularity of solid at the ball milling outlet is more than or equal to 60% under the 60-mesh standard sieve.
Furthermore, the conversion time of the potash magnesium sulphate fertilizer system is 1-1.5 hours, the conversion temperature is 15-25 ℃, and the index of the conversion solution is not limited.
Furthermore, the decomposition temperature of the potassium chloride system is 5-20 ℃, the decomposition time is 1-1.5 hours, and the indexes of the decomposition liquid are not limited.
Further, the mass ratio of the potassium chloride to the potash magnesium sulphate fertilizer to the water is 1 (1.1-1.5) to 1.5-2.0.
Furthermore, the conversion temperature of the fresh water is 25-37 ℃, the conversion time of the fresh water is 1-2 hours, and the index of the conversion solution is not limited.
Further, drying the obtained potassium chloride and potassium sulfate, wherein the drying temperature of the potassium sulfate and the potassium chloride is 350-380 ℃.
Further, the high-potassium tail liquid left after the potassium sulfate is obtained is introduced into the conversion stage of the potash magnesium sulfate fertilizer system and the decomposition stage of the potassium chloride system again.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method can produce the potash magnesium sulphate fertilizer, the potassium chloride and the potassium sulfate in a combined manner, wherein the potassium chloride and the potassium sulfate can share the same drying system, the utilization rate of equipment is improved, and the investment cost is reduced. The potash magnesium sulphate fertilizer product can produce granular potash magnesium sulphate fertilizer and improve the yield of the potash magnesium sulphate fertilizer. (2) The high potassium filtrate obtained after solid-liquid separation in the potassium sulfate section by a centrifuge can be according to K+、 Na+、Mg2+//Cl-、SO4 2-—H2And (4) calculating an O five-membered water-salt system phase diagram, and respectively returning to the conversion of the potassium magnesium sulfate fertilizer system and the decomposition of the potassium chloride system, so that zero emission of high-potassium tail liquid of potassium sulfate is realized, and the recovery rate is improved. (3) The whole potassium sulfate production system has the same requirements on the processes of potassium chloride and potassium magnesium sulfate fertilizer, the production process is simplified, and the cost is lower. (4) The whole process flow is slightly influenced by the air temperature, continuous production can be realized, and the cost is saved. (5) The prior art has single product, and the invention flexibly regulates and controls the production of potash magnesium sulphate fertilizer, potassium sulphate and potassium chloride products according to the market development trend.
Drawings
FIG. 1 is a process flow diagram of the present invention for co-production of potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate.
Detailed Description
In order to make the technical solution of the present invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
The embodiment discloses a method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate, which utilizes low-grade potassium mixed salt ore and low-grade carnallite ore for co-production, and mainly produces the potassium sulphate, and the production requirements are as follows: (1) the production process of the potash magnesium sulphate fertilizer controls the content of chloride ions in the potash magnesium sulphate fertilizer product to be 2.5-4 wt% and the water content of the potash magnesium sulphate fertilizer product to be 13-15 wt%. (2) The production process of the potassium chloride controls the potassium chloride content in the potassium chloride product to be 50-75 wt% and the water content of the product to be 11-13 wt%. (3) The potassium sulfate production control potassium sulfate product meets the requirements of GB/T20406-2017. In the embodiment, the preparation is carried out by adopting each step of the method, and the method is mainly divided into two large processes of beach drying by stages and fertilizer co-production, wherein relevant data indexes of beach drying by stages refer to the technical scheme of the invention and are not described again; the fertilizer co-production process is shown in fig. 1, and the related data indexes are shown in table 1:
TABLE 1
From table 1, it can be seen that the low-grade potassium mixed salt ore and the low-grade carnallite are used for co-producing the potash magnesium sulphate fertilizer, the potassium chloride and the potassium sulphate products, the potassium sulphate is mainly produced, the chloride ions of the potash magnesium sulphate fertilizer product are not easy to control, the potassium recovery rate is low, the potassium chloride content of the potassium chloride product is low, the potassium yield is low, but the total potassium recovery rate of the potassium chloride product is up to 32% after the potassium sulphate is produced by the potassium mixed salt ore and the low-grade carnallite are respectively returned to a potassium magnesium sulphate fertilizer and potassium chloride system.
Example 2
The embodiment discloses another method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate, which adopts high-grade potassium mixed salt ore and low-grade carnallite ore for co-production, mainly produces the potash magnesium sulphate fertilizer and the potassium sulphate, and has the production requirements as follows: (1) the production process of the potash magnesium sulphate fertilizer controls the content of chloride ions in the potash magnesium sulphate fertilizer product to be less than or equal to 2.5 wt% and the water content of the potash magnesium sulphate fertilizer product to be 10-12 wt%. (2) The production process of the potassium chloride controls the potassium chloride content in the potassium chloride product to be 50-75 wt% and the water content of the product to be 11-13 wt%. (3) The potassium sulphate magnesium fertilizer production control method is characterized in that after being dried, a potassium sulphate magnesium fertilizer product is required to meet the requirement of GB/T20937-2018, and after being dried, a potassium sulphate product is required to meet the requirement of GB/T20406-2017. In the embodiment, the preparation is carried out by adopting each step of the method, and the method is mainly divided into two large processes of beach drying by stages and fertilizer co-production, wherein relevant data indexes of beach drying by stages refer to the technical scheme of the invention and are not described again; the relevant data indexes of the fertilizer co-production process are shown in table 2:
TABLE 2
From table 2, it can be seen that, in the co-production of the potash magnesium sulphate fertilizer, the potassium chloride and the potassium sulphate products from the high-grade potassium mixed salt ore and the low-grade carnallite ore, the potash magnesium sulphate fertilizer and the potassium sulphate are mainly produced, the chloride ions of the potash magnesium sulphate fertilizer product are easy to control, the potassium recovery rate can reach 60%, the potassium chloride product has low potassium chloride content and low potassium yield, but the total potassium recovery rate can reach 38% when the conversion liquid returns to the potash magnesium sulphate fertilizer and potassium chloride systems respectively after the potassium sulphate is produced.
Example 3
The embodiment discloses a method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate, which adopts high-grade potassium mixed salt ore and high-grade carnallite ore for co-production, and the main production can flexibly regulate and control different potash fertilizer products according to the market development trend, and the production requirements are as follows: (1) the production process of the potash magnesium sulphate fertilizer controls the content of chloride ions in the potash magnesium sulphate fertilizer product to be less than or equal to 2.5 wt% and the water content of the potash magnesium sulphate fertilizer product to be 10-12 wt%. (2) The production process of the potassium chloride controls the potassium chloride content in the potassium chloride product to be more than or equal to 80 wt% and the water content of the product to be 11-13 wt%. And (3) controlling the potassium sulphate magnesium fertilizer product to meet the requirement of GB/T20937-2018 after the potassium sulphate magnesium fertilizer is dried, controlling the potassium sulphate product to meet the requirement of GB/T20406-2017 after the potassium sulphate product is dried, and controlling the potassium chloride product to meet the requirement of GB/T37918-2019. In the embodiment, the preparation is carried out by adopting each step of the method, and the method is mainly divided into two large processes of beach drying by stages and fertilizer co-production, wherein relevant data indexes of beach drying by stages refer to the technical scheme of the invention and are not described again; the relevant data indexes of the fertilizer co-production process are shown in table 3:
TABLE 3
From table 3, it can be seen that the high-grade potassium mixed salt ore and the high-grade carnallite are used for co-producing the potash magnesium sulphate fertilizer, the potassium chloride and the potassium sulphate products, the main production of the potash mixed salt ore and the high-grade carnallite can flexibly regulate and control the production of the potash magnesium sulphate fertilizer, the potassium chloride and the potassium sulphate according to the market development trend, the chloride ions of the potash magnesium sulphate fertilizer product are easy to control, the potassium recovery rate can reach 70%, the potassium yield of the potassium chloride product is 75%, but the total potassium recovery rate of the conversion liquid after the potassium sulphate production returns to the potash magnesium sulphate fertilizer and the potassium chloride system respectively can reach 45%.
The production of the low-grade potassium mixed salt ore and the high-grade carnallite ore can be flexibly regulated and controlled according to the market development trend to produce potash magnesium sulphate fertilizer, potassium sulfate and potassium chloride, and because the potassium chloride product and the potassium sulfate product drying system are shared, the potassium chloride product can be stored firstly and then dried at the later stage, which can not be exhausted in the invention, but is only illustrated by way of example.
The particular embodiments of the present invention disclosed above are illustrative only and are not intended to be limiting, since various alternatives, modifications, and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The invention should not be limited to the disclosure of the embodiments in the present specification, but the scope of the invention is defined by the appended claims.
Claims (10)
1. A method for coproducing a potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate is characterized by comprising the following steps:
injecting sulfate brine into a sodium chloride stage salt field for beach drying in stages, wherein the sulfate brine comprises the following ions in mass fraction: [ K ]+]0.4-0.81wt％、[Mg2+]0.9-2.45wt％、[SO4 2-]1.22-2.85wt％、[Cl-]13.88-15.51wt％；
The first stage is to solarize part of sulfate brine naturally until meeting the indexes of potassium mixed salt stage, wherein the indexes are that the mass fraction of ions in the brine is as follows: [ K ]+]≥2.16wt％、[Mg2+]≥4wt％、[SO4 2-]≥4.2wt％、[Cl-]Not less than 15.2 wt%, and then injecting into potassium mixed salt field and naturally solarizing into potassium mixed salt mine;
and the second stage is to naturally solarize part of the sulfate brine to meet the index of the carnallite stage, wherein the index refers to the mass fraction of ions in the brine: [ K ]+]≤1.81wt％、[Mg2+]≥6.3wt％、[SO4 2-]≤3.94wt％、[Cl-]Not less than 17.7 wt%, and then injecting into carnallite salt field to naturally solarize into carnallite;
and the third stage is to naturally dry the remaining sulfate brine on the beach to meet the index of the old brine stage, wherein the index refers to the mass fraction of ions in the brine as follows: [ K ]+]≤0.11wt％、[Mg2+]≥8.2wt％、[SO4 2-]≤2.83wt％、[Cl-]Not less than 22.4 wt%, and then injecting into old brine salt field;
crushing, ball-milling, converting, floating and filtering the potassium mixed salt ore by a potassium magnesium sulfate fertilizer system to obtain a potassium magnesium sulfate fertilizer;
decomposing, floating and filtering carnallite ore by a potassium chloride system to obtain potassium chloride;
adding water into the potash magnesium sulphate fertilizer and the potassium chloride, stirring, performing fresh water conversion reaction, crystallizing and filtering to obtain the potassium sulphate.
2. The method of claim 1, wherein the mass fraction of ions in the potash mixed salt ore: [ K ]+]3.5-7.5wt％、[Mg2+]3-8wt％、[SO4 2-]12-28wt％、[Cl-]20-35 wt%; mass fraction of ions in carnallite: [ K ]+]4.0-10wt％、[Mg2+]5-10wt％、[SO4 2-]1-15wt％、[Cl-]20-35wt％。
3. The method of claim 1, wherein during the process of crushing, ball milling, converting, floating and filtering the potash mixed salt ore to obtain the potash magnesium sulphate fertilizer, the chloride ion content in the potash magnesium sulphate fertilizer product is regulated according to the yield of potassium chloride: when the yield of potassium chloride is higher than the proportion of the yield of the potash magnesium sulphate fertilizer, the content of chloride ions in the potash magnesium sulphate fertilizer is regulated to be 2.5-4 wt% and the potash magnesium sulphate fertilizer is used for producing potassium sulphate with the mixture of potassium chloride; when the yield of the potassium chloride is lower than the yield proportion of the potash magnesium sulphate fertilizer, adding water to regulate the content of chloride ions in the potash magnesium sulphate fertilizer to be less than or equal to 2.5 wt%;
in the process of decomposing, floating and filtering carnallite ore to obtain potassium chloride, regulating and controlling the potassium chloride content in a potassium chloride product according to the yield of a potash magnesium sulphate fertilizer: when the yield of the potash magnesium sulphate fertilizer is higher than the proportion of the yield of potassium chloride, regulating and controlling the potassium chloride content in the potassium chloride product to be 50-75 wt% for producing potassium sulphate with the potash magnesium sulphate fertilizer; when the yield of the potash magnesium sulphate fertilizer is lower than the proportion of the potassium chloride yield, water is added to regulate the potassium chloride content in the potassium chloride product to be more than or equal to 80 wt%.
4. The method of claim 1, wherein the potassic magnesium sulfate fertilizer system ball milling slurry concentration is 60-70 wt%, and the ball milling outlet particle size solids are 60% or more under a standard sieve 60 mesh.
5. The method of claim 1, wherein the potash magnesium sulphate fertilizer system conversion time is 1-1.5 hours and the conversion temperature is 15-25 ℃.
6. The process according to claim 1, wherein the decomposition temperature of the potassium chloride system is 5 to 20 ℃ and the decomposition time is 1 to 1.5 hours.
7. The method of claim 1 wherein the mass ratio of potassium chloride to potash magnesium sulphate fertilizer to water is 1 (1.1-1.5) to (1.5-2.0).
8. The method of claim 1, wherein the freshwater conversion temperature is from 25 ℃ to 37 ℃ and the freshwater conversion time is from 1 hour to 2 hours.
9. The method as claimed in claim 1, wherein the potassium chloride and potassium sulfate are dried at a temperature of 350-380 ℃.
10. The method of claim 1, wherein the high potassium tail solution remaining after potassium sulfate is obtained is reintroduced into the conversion stage of the potash magnesium sulfate fertilizer system and the decomposition stage of the potassium chloride system.
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| CN113200767A (en) * | 2021-04-02 | 2021-08-03 | 青海联宇钾肥有限公司 | Method for preparing granular potash magnesium sulphate fertilizer by using potassium mixed salt ore |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113200767A (en) * | 2021-04-02 | 2021-08-03 | 青海联宇钾肥有限公司 | Method for preparing granular potash magnesium sulphate fertilizer by using potassium mixed salt ore |
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