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Method for preparing potassium sulfate by using polyhalite

A technology for polyhalite and potassium sulfate, which is applied in the field of preparing potassium sulfate from high-sodium insoluble polyhalite, can solve the problems of high risk, long process flow, harsh reaction conditions, etc., and achieves less water consumption for leaching and source of raw materials. Wide, high K+ concentration effect

Active Publication Date: 2017-02-08
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

[0003] Due to the stable structure of polyhalite and poor water solubility, it needs certain treatment to utilize the potassium ions therein. Some literatures have reported the method of preparing potassium sulfate by utilizing polyhalite, for example, the Chinese patent application whose application number is 89101455.1 , disclose the method that utilizes same ion effect to extract potassium sulfate, magnesium sulfate, calcium sulfate from gypsum, polyhalite ore with 3.5% potassium sulfate solution, but this method needs to use 3.5% potassium sulfate as solvent, K + The utilization rate is low and the cost is high; US1956930 discloses a method for preparing potassium sulfate by reacting polyhalite and limestone in a sealed reactor, but the reaction conditions are harsh, the operation is complicated, and the risk is high; CN 103930371 A discloses that polyhalite and limestone are reacted to prepare potassium sulfate After the stone is calcined, the liquid that forms potassium sulfate and magnesium sulfate is first leached, and then the potassium-containing salts such as langbeinite are dissolved in the filtrate to increase the concentration of the solution. Part of the concentrated filtrate crystallizes to obtain potassium sulfate, and the other part precipitates to form anhydrous potassium langbeinite, decompose part of the obtained langbeinite to form langbeinite and return to the previous process to increase the concentration of the solution
The process of the method is longer, and the obtained langbeinite product needs to be redissolved, which wastes energy, and the market demand and value of the langbeinite product are relatively small

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] This embodiment takes polyhalite ore in a foreign place as an example, the NaCl content in the mineral is 38.9wt%, and specifically includes the following steps:

[0038] (1) Grinding: Grinding polyhalite to -150 mesh 92wt%;

[0039] (2) Washing: Wash the polyhalite with water equivalent to 0.4 times the weight of the polyhalite to remove sodium chloride in the polyhalite. After filtering, rinse the filter cake with water equivalent to 0.2 times the weight of the filter cake. After rinsing, the polyhalite The sodium chloride content in the medium is 0.42wt%;

[0040] (3) Roasting: Roast the washed minerals at 430°C for 40 minutes;

[0041] (4) Leaching: leaching the roasted polyhalite with secondary countercurrent with water, the liquid-solid mass ratio is 2:1; the leaching time is 40min; the leaching temperature is 80°C, and the leaching pulp is obtained;

[0042] (5) Solid-liquid separation: The leaching pulp obtained in step (4) is subjected to solid-liquid separat...

Embodiment 2

[0048] In this embodiment, polyhalite ore in a foreign country is taken as an example, the NaCl content in the mineral is 29.6wt%, and specifically includes the following steps:

[0049] (1) Grinding: Grinding polyhalite to -150 mesh 91wt%;

[0050] (2) Washing: Continue to wash the polyhalite with the solution that has washed the polyhalite in Example 1, and after filtering, rinse the filter cake with water equivalent to 0.2 times the weight of the polyhalite. After leaching, the polyhalite is chlorinated Sodium content 0.45%;

[0051] The average loss of potassium ions in the washing process is less than 5.0wt%;

[0052] (3) Roasting: Roast the washed minerals at 450°C for 30 minutes;

[0053] (4) Leaching: leaching the roasted polyhalite with secondary countercurrent with water, the liquid-solid mass ratio is 3:1, the leaching time is 50min, and the leaching temperature is 90°C; + Concentration is less than 2.5wt%, continue leaching polyhalite once with mother liquor, le...

Embodiment 3

[0059] This embodiment takes polyhalite ore in a certain place in my country as an example, the NaCl content in the mineral is 21.7wt%, and specifically includes the following steps:

[0060] (1) Grinding: Grinding polyhalite to -150 mesh 93wt%;

[0061] (2) Washing: wash with water equivalent to 0.3 times the weight of polyhalite to remove sodium chloride in polyhalite, and after filtration, rinse the filter cake with water equivalent to 0.2 times the weight of polyhalite. The sodium chloride content in the stone is 0.38wt%;

[0062] (3) Roasting: Roast the washed minerals at 470°C for 30 minutes;

[0063] (4) Leaching: leaching the roasted polyhalite with secondary countercurrent water, the liquid-solid mass ratio is 3.5:1, the leaching time is 60min, and the leaching temperature is 90°C; + Concentration is less than 2.5wt%, continue leaching polyhalite once with mother liquor, leaching condition is the same as first time, must leaching ore pulp;

[0064] (5) Solid-liquid...

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Abstract

The invention provides a method for preparing potassium sulfate by using polyhalite. The method comprises the following steps of: (1) grinding ores: grinding the polyhalite till 90wt% of the polyhalite are over 150 meshes in size; (2) washing: washing with water to remove the sodium chloride in the polyhalite; (3) roasting: roasting washed minerals at a high temperature; (4) leaching: leaching to extract potassium in the polyhalite; (5) solid-liquid separation: subjecting the ore pulp obtained through the leaching step to solid-liquid separation so as to obtain a mother liquor containing K+; (6) conversion: evaporating the mother liquor, adding potassium chloride and a potassium mixed salt, preparing potassium sulfate through the conversion method, and filtering to obtain a potassium sulfate product and the mother liquor; (7) evaporation: continuously evaporating the mother liquor, filtering to obtain a potassium mixed salt, and returning the potassium mixed salt to the conversion process. According to the method, the potassium sulfate is prepared by using the polyhalite. The process is simple, wide in source of raw materials and low in cost, wherein the sodium chloride in the polyhalite can be effectively removed. Meanwhile, the leaching rate of K+ is high and the water consumption of leaching is reduced. The concentration of K+ in the leaching mother liquor is high, and the energy consumption of the subsequent evaporation and crystallization step is reduced. Obtained potassium sulfate products are high in purity.

Description

technical field [0001] The invention relates to a process for preparing potassium sulfate with potassium-containing minerals, in particular to a process for preparing potassium sulfate with high-sodium insoluble polyhalite. Background technique [0002] Polyhalite (K 2 SO 4 · MgSO 4 2CaSO 4 2H 2 O), is a kind of insoluble potassium ore, which is light gray or dark gray, widely distributed in sulfate-type potassium ore, and its theoretical potassium content (K 2 O) reaches 15.6%, which is an important potash resource. The polyhalite resources in the world are very rich, and the geological ages of its production are mainly concentrated in the Permian, Triassic and Tertiary. In terms of geological plane distribution, they are relatively concentrated in the ring belt of 25°-50° north latitude . Our country is just located in the regular ring zone where polyhalite resources are relatively rich in the world. It has been found that Sichuan, Hubei, Jiangsu, Shandong, Shanxi, ...

Claims

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Application Information

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IPC IPC(8): C01D5/00
CPCC01D5/00C01P2006/80
Inventor 冯文平高文远李昱昀孙成高谢晶磊季荣汤建良郑贤福
Owner CHANGSHA DESIGN & RES INST OF CHEM IND MIN
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