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Process using polyhalite extraction mother liquor to produce potassium sulfate

A technology of polyhalite and potassium sulfate, applied in the field of potassium sulfate production technology, can solve the problems of low yield of potassium products, increase of potassium sulfate production, large amount of entrainment of mother liquor, etc., achieve high output and added value, and be easy for industrial production , The effect of simple process

Active Publication Date: 2016-06-15
CHANGSHA DESIGN & RES INST OF CHEM IND MIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the research on extracting potassium sulfate by leaching mother liquor, most of them adopt the process of evaporation, concentration and crystallization, but the output of potassium sulfate is extremely small, and most of potassium sulfate is crystallized in the form of potassium-magnesium mixed salt, and the separation of potassium and magnesium is difficult and difficult to realize. Thorough Separation of Potassium Sulfate and Magnesium Sulfate
If it is directly sold as a potassium-magnesium fertilizer product, not only the product grade is low, but also the market sales are not ideal; Reaction raw materials, increase production costs, but also produce a large amount of constantly expanding high-potassium mother liquor that is difficult to digest, affecting the economic benefits of enterprises
[0004] Such as CN104755426A discloses a kind of method and related system of processing potassium sulfate and magnesium sulfate solution to produce potassium sulfate, is to utilize the mother liquor that contains potassium sulfate and magnesium sulfate after leaching polyhalite to mix with circulating crystal crystallization, thereby make the first concentrated solution Concentration can reduce the evaporation energy consumption of the first concentrated solution to a certain extent and increase the output of potassium sulfate, but it cannot fundamentally realize the complete separation of potassium sulfate and magnesium sulfate. Regardless of low-temperature evaporation or forced evaporation, a large amount of potassium salt It is also precipitated in the form of langbeinite or anhydrous langbeinite, which reduces the product grade and market price, and repeated evaporation crystallization and re-dissolution greatly increases energy consumption costs
CN102030487A discloses a new process of normal temperature carbonization and low-temperature pyrolysis of high-purity magnesium oxide. The combined process of carbonization and pyrolysis can realize the precipitation and separation of magnesium, but the obtained pyrolysis product magnesium carbonate is easily hydrolyzed to precipitate magnesium hydroxide with lower solubility. The particles are fine, the separation is difficult, and the mother liquor has a large amount of entrainment. If this technology is used to separate the polyhalite leaching mother liquor, the entrainment of the magnesium salt mother liquor will be large, and the yield of potassium products will be low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Adjust the pH value: pass ammonia gas with a volume concentration of 92% into 2000g (volume 1750mL) of polyhalite leaching mother liquor (K + : 2.2wt%, Mg 2+ : 0.8wt%, Ca 2+ : 0.03wt%), until the pH value is 10.85, 1800mL Mg(OH) 2 slurry;

[0031] (2) CO 2 Carbonization: CO with a volume concentration of 95% 2 With the pressure of 0.3MPa and the speed of 4.8L / L solution h, pass through the 1800mLMg(OH) obtained in step (1) 2 Carry out carbonization reaction at room temperature at 20°C in the slurry, and stop the reaction when the pH value is 7.6 to obtain the carbonization mother liquor;

[0032] (3) Pyrolysis separation: heat and decompose the carbonized mother liquor obtained in step (2) at 45°C for 40 minutes, and separate solid and liquid to obtain MgCO 3 ·3H 2 O solid salt and pyrolysis separation mother liquor;

[0033] (4) Causticization separation: In the pyrolysis separation mother liquor obtained in step (3), calcium oxide and NH in the pyrolysis s...

Embodiment 2

[0038] (1) Adjust the pH value: pass ammonia gas with a volume concentration of 95% into 1000g (volume 850mL) of polyhalite leaching mother liquor (K + : 4.48wt%, Mg 2+ : 1.63wt%, Ca 2+ : 0.08wt%), to pH 11.3, 910mL Mg(OH) 2 slurry;

[0039] (2) CO 2 Carbonization: CO with a volume concentration of 88% 2 With the pressure of 0.2MPa and the speed of 0.8L / L solution h, pass through the 910mL Mg(OH) obtained in step (1) 2 In the slurry, carry out carbonization reaction at room temperature at 30°C, and terminate the reaction when the pH value is 7.8, to obtain the carbonization mother liquor;

[0040] (3) Pyrolysis separation: heat and decompose the carbonized mother liquor obtained in step (2) at 70°C for 30 minutes, and separate solid and liquid to obtain MgCO 3 ·3H 2 O solid salt and pyrolysis separation mother liquor;

[0041] (4) Causticization separation: In the pyrolysis separation mother liquor obtained in step (3), calcium oxide and NH in the pyrolysis separation ...

Embodiment 3

[0046] (1) Adjust the pH value: pass ammonia gas with a volume concentration of 99% into 1000g (volume 900mL) of polyhalite leaching mother liquor (K + : 3.29wt%, Mg 2+ : 1.50wt%, Ca 2+ : 0.05wt%), to pH 11.5, 940mL Mg(OH) 2 slurry;

[0047] (2) CO 2 Carbonization: CO with a volume concentration of 85% 2 With the pressure of 0.5MPa and the speed of 3.6L / L solution h, pass through the 940mLMg(OH) obtained in step (1) 2 In the slurry, carry out carbonization reaction at room temperature at 25°C, and terminate the reaction when the pH value is 7.9, to obtain the carbonization mother liquor;

[0048] (3) Pyrolysis separation: heat and decompose the carbonized mother liquor obtained in step (2) at 60°C for 40 minutes, and separate solid and liquid to obtain MgCO 3 ·3H 2 O solid salt and pyrolysis separation mother liquor;

[0049] (4) Causticization separation: In the pyrolysis separation mother liquor obtained in step (3), calcium hydroxide and NH in the pyrolysis separati...

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Abstract

The invention relates to a process using polyhalite extraction mother liquor to produce potassium sulfate.The process includes the steps of firstly, feeding ammonia gas into the polyhalite polyhalite extraction mother liquor to regulate pH to 10.0-12.0 so as to obtain Mg(OH)2 slurry; secondly, feeding CO2 until the pH is 7.5-8.0 to obtain carbonized mother liquor; thirdly, performing pyrolysis and solid-liquid separation to obtain MgCO3.3H2O solid salt and mother liquor after pyrolysis and separation; fourthly, adding calcium oxide slurry or calcium hydroxide slurry into the mother liquor after pyrolysis and separation, heating, stirring, and performing solid-liquid separation to obtain mother liquor after causticization separation; fifthly, performing forcible evaporation, and crystalizing to separate out potassium sulfate.The K2O content of the potassium sulfate obtained by the process reaches up to 51.9%, potassium ion yield reaches up to 91.7%, byproducts such as high-purity magnesium oxide and gypsum can be coproduced, and the process is simple in process flow, simple in needed equipment, easy in industrial production and low in cost.

Description

technical field [0001] The invention relates to a production process of potassium sulfate, in particular to a process for producing potassium sulfate by leaching mother liquor with polyhalite. Background technique [0002] Polyhalite (K 2 SO 4 · MgSO 4 2CaSO 4 2H 2 O), is an important insoluble potassium-containing salt ore, which is rich in reserves, with the largest amount in Sichuan and Hubei, and only (Sichuan) eastern (eastern) polyhalite resources are equivalent to K 2 The reserve of O is more than 20 billion tons, which is an important supplementary resource for my country's potash fertilizer industry. With the development of high-grade salt lake brine resources, available high-quality potassium-containing resources are increasingly scarce, and insoluble polyhalite potassium-containing salt ore resources are bound to become the focus of future potassium salt development and research hotspots. [0003] At present, the research on polyhalite leaching technology is...

Claims

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Application Information

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IPC IPC(8): C01D5/16C01F5/24C01F5/06C01F11/46
CPCC01D5/16C01F5/06C01F5/24C01F11/46C01P2006/80Y02P20/141
Inventor 高文远冯文平蒋世鹏汤建良宁晚云郑贤福邹娟杨清
Owner CHANGSHA DESIGN & RES INST OF CHEM IND MIN
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