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Lithium salt recovery method

A recovery method and lithium salt technology, applied in the field of lithium salt recovery, can solve the problems of high process control requirements, long process routes and high energy consumption, and achieve the effects of avoiding high temperature decomposition, short process process and high efficiency

Active Publication Date: 2013-09-18
SHANDONG MINGHUA NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The lithium salt recovery method reported in the above literature not only has many problems such as long process route, low recovery rate of lithium salt, large amount of waste water and high energy consumption, but also needs to use the high-risk chemical substance hydrogen sulfide (H 2 S) Gas, which requires high process control and is dangerous

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 7.2g of sodium hydrosulfide to 419.7g of salt-containing liquid (containing 5g of water, 359g of NMP, 49.7g of NaCl, and 6g of LiCl) from the production of polyphenylene sulfide under the protection of nitrogen, and react at 45-55°C for 6 Hour. After the hydrosulfhydration reaction was completed, white insoluble matter was produced, which was sealed and filtered, and the filter cake was washed with 40 g of anhydrous NMP and dried to obtain 57 g of sodium chloride solid.

[0023] Filtrate 409 g of the obtained filtrate, raise the temperature to 135-150° C. under the protection of stirring and nitrogen (bubbling through the reactant), and decompose and transform for 6 hours. H produced during the reaction 2 S gas was absorbed with 30% NaOH solution. The obtained 406.5g NMP and lithium sulfide solution can be recycled for the synthesis of polyphenylene sulfide.

Embodiment 2

[0025] Add 66g of sodium hydrosulfide to 451g of salt-containing liquid (including 4g of water, 401g of NMP, and 46g of LiCl) from the production of polyphenylene sulfide under nitrogen protection, and react at 135-150°C for 2 hours. After the hydrosulfhydration reaction was completed, the white insoluble matter was airtightly filtered, and the filter cake was washed with 60 g of anhydrous NMP and dried to obtain 62.5 g of sodium chloride solid.

[0026] 512 g of the filtrate obtained by filtration was heated up to 160-180° C. under the protection of stirring and nitrogen gas (through bubbling), and reacted for 2 hours. H produced during the reaction 2 S gas was absorbed with 50% NaOH solution. The obtained 490g NMP and lithium sulfide solution can be recycled for the synthesis of polyphenylene sulfide.

Embodiment 3

[0028] Add 17g of potassium hydrogen sulfide to 517g of salt-containing liquid (containing 5g of water, 450g of NMP, 52g of NaCl, and 10g of LiCl) after the production of polyphenylene sulfide, under stirring and nitrogen protection, and react at 90-100°C for 3 hours. After the reaction, white insoluble matter was produced, which was airtightly filtered, and the filter cake was washed with 50 g of anhydrous NMP and dried to obtain 65 g of sodium chloride solid.

[0029] 516 g of the filtrate obtained by filtration was heated to 160-170° C. under the protection of stirring and nitrogen (or argon, bubbling through), and reacted for 4 hours. H produced during the reaction 2 S gas is absorbed with 40% KOH solution. The obtained 509g NMP and lithium sulfide solution can be recycled for the synthesis of polyphenylene sulfide.

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Abstract

The invention discloses a lithium salt recovery method which comprises the following steps of: firstly, carrying out a sulfohydrogenation reaction between a hydrosulfide and a lithium salt existing in an N-methylpyrrolidinone system in an inert gas environment, thereby converting the lithium salt into lithium hydrosulfide, and then performing solid-liquid separation; after solid-liquid separation, heating a N-methylpyrrolidinone solution containing the lithium hydrosulfide in the inert gas environment and decomposing and converting the lithium hydrosulfide into lithium sulfide precipitate, and collecting the lithium sulfide precipitate after solid-liquid separation. The method has the advantages that the production process is safer and more convenient because no high-risk hydrogen sulfide gas is utilized, and the recovery process is short, the investment is saved, the efficiency is high and the recovery rate of the lithium salt is higher than 99%. As the solvent NMP does not need to be evaporated at a high temperature, high-temperature decomposition of the solvent is also avoided. For polyarylene sulfide production, the lithium salt recovery method is suitable for different preparation processes / routes; and the recovered lithium sulfide can be recycled directly for polyarylene sulfide preparation.

Description

technical field [0001] The invention relates to a lithium salt recovery method, in particular to recovery of lithium salt in the preparation process of polyarylene sulfide including polyphenylene sulfide. Background technique [0002] Polyarylene sulfide, represented by polyphenylene sulfide, is a new type of functional polymer material with good high temperature stability, flame retardancy, chemical corrosion resistance, and good electrical and electronic properties, processability and Dimensional stability, can be processed into films, fibers, etc. for industrial production processes that are resistant to high temperature and chemical corrosion, and can also be processed into related components in the fields of machinery, automobiles, electronics, computers, etc. through extrusion molding and injection molding. is widely used. [0003] Taking polyphenylene sulfide as an example, dihalogenated aromatic compounds such as p-dichlorobenzene and m-dichlorobenzene are mostly u...

Claims

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Application Information

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IPC IPC(8): C08J11/00C08G75/02C08L81/02C08G75/0254
Inventor 李晶晶李朝祥罗芩杨琴
Owner SHANDONG MINGHUA NEW MATERIAL CO LTD
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