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Method for preparing high-purity potassium sulfate from waste residue raw material obtained after extraction of lithium from lepidolite

A technology of lepidolite, potassium sulfate, applied in chemical instruments and methods, alkali metal sulfites/sulfites, alkali metal compounds, etc., to achieve the effects of easy cleaning, cost reduction, and production cost reduction

Active Publication Date: 2020-03-24
YICHUN KEYUAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, there are few domestic and foreign research literature reports on the synthesis of high-purity potassium sulfate by using lepidolite to extract lithium and rubidium and cesium to extract alum.

Method used

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  • Method for preparing high-purity potassium sulfate from waste residue raw material obtained after extraction of lithium from lepidolite
  • Method for preparing high-purity potassium sulfate from waste residue raw material obtained after extraction of lithium from lepidolite

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Embodiment 1

[0046] The lepidolite acid waste slag described in the embodiments of the present invention is mainly solid alum and may also be a high-temperature solution of alum. Lepidolite acid waste is the waste produced in the process of lithium extraction by sulfuric acid method. It is the waste generated after the rubidium and cesium high value-added elements are extracted from the waste by means of recrystallization; the solid alum in the present invention refers to the potassium alum produced in the process of extracting lithium by using lepidolite.

[0047] The method for preparing high-purity potassium sulfate from the waste residue raw material after lepidolite extracts lithium of the present invention is carried out according to the following processing steps:

[0048] 1) In a 500L enamel reaction kettle, add 300L process water. The process water described in the embodiments of the present invention refers to the water produced by filtration, separation, concentration, evaporati...

Embodiment 2

[0057] 1) Add 300L of process water to a 500L enamel reaction kettle and heat it to above 60°C, keep it warm and stir, put in 150kg of lithium extraction acid waste residue, stir and dissolve, filter while hot to remove insoluble matter to obtain a solution for removing impurities.

[0058] 2) Cool the filtrate of the impurity-removing solution to 55°C, heat it in a desktop filter for 1 hour and then filter it, and send the filter residue to the rubidium and cesium enterprise, and the filtrate at this time is the filtered clear liquid;

[0059] 3) Add the filtrate of the filtered clear liquid to the enamel reaction kettle while it is hot with a pump, then add 32L of calcium hydroxide emulsion of 666g / L, adjust the pH of the solution to 8, boil at normal pressure for more than 1 hour, and keep stirring for 1 hour to obtain Reaction solution 1;

[0060] 4) Filtrate while hot, the filter residue is mainly aluminum hydroxide and calcium sulfate, and the filtrate at this moment is ...

Embodiment 3

[0065] 1) Add 300L process water to a 500L enamel reaction kettle and heat it to above 700C. Insulated and stirred, put into 140kg of lithium extraction acidic waste residue, after stirring and dissolving, filter while hot to remove insolubles to obtain impurity-removing solution;

[0066] 2) Cool down the impurity-removing liquid of the filtrate in the previous step to 53° C., keep warm in a desktop filter for 1 hour and then filter, and send the filter residue to the rubidium and cesium enterprise, and the filtrate at this time is filtered into the supernatant;

[0067] 3) Use a pump to add the filtrate from the previous step to the enamel reaction kettle while it is hot, then add 32L of 666g / L calcium oxide emulsion, adjust the pH of the solution to 7.5, boil at normal pressure for more than 1 hour, keep stirring for 1 hour, Obtain reaction solution 1;

[0068] 4) The reaction solution 1 is filtered while it is hot, the filter residue is mainly aluminum hydroxide and calci...

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Abstract

The invention provides a method for preparing high-purity potassium sulfate from a waste residue raw material obtained after extraction of lithium from lepidolite. Waste residues generated in the lithium extraction process of lepidolite, which are used as a raw materials react with auxiliary materials such as calcium oxide and calcium carbonate to produce the high-purity potassium sulfate at a lowcost and a high efficiency. Acidic wastes generated in the lithium extraction process are used as the main raw material, the lithium extraction and alum separation process is utilized efficiently, soenergy is saved; and the high-purity potassium sulfate is produced through a neutralization reaction, impurity removal filtration, concentration, crystallization, centrifugation and drying. The production process is simple, the requirement on devices is not high, and the high-purity potassium sulfate can be finally prepared at a high yield. The method has the advantages of wide raw material source, low energy demand, no newly generated waste, environmental friendliness, realization of the product purity of above 99.5%, simple and convenient production process, improvement of the economic values of the lepidolite, and reduction of the production cost of ore lithium extraction, and can be comprehensively applied to industrial production.

Description

Technical field: [0001] The invention relates to a method for preparing high-purity potassium sulfate, in particular to a method for preparing high-purity potassium sulfate from waste residue raw materials after lepidolite extraction of lithium. Background technique: [0002] At present, the production methods of potassium sulfate in the world mainly include Mannheim furnace method, double decomposition method, association method and comprehensive utilization method of potassium ore. More than half of the raw materials used in the production of ordinary potassium sulfate are processed from natural potassium ore. The double decomposition of potassium chloride and sulfate-containing raw materials to produce potassium sulfate is a very important method. Such as the Chinese patent announcement number is No. CN 103803586 A, "The Production Method of Potassium Sulfate Concentrated in Sections" is one of them, but the above-mentioned method is only a production method for preparing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D5/00
CPCC01D5/00C01P2006/80
Inventor 彭平席文龙席文峰段小勋
Owner YICHUN KEYUAN CHEM CO LTD
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