A method for comprehensive recovery and utilization of lithium containing mixed salts in a polyphenylene sulfide production process

A production process, polyphenylene sulfide technology, applied in lithium halide, alkali metal chloride, organic chemistry, etc., can solve the problem of low product purity and yield, cumbersome recovery process, and the inability to realize comprehensive recycling of by-product slurry and other issues, to achieve the effect of easy industrial production

Active Publication Date: 2017-04-19
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY +1
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Problems solved by technology

It is worth noting that there are certain defects in the current relevant recycling methods, such as the inability to realize the comprehensive recycling of the by-product slurry, or the low purity of some recovered products, etc.
In addition, after the PPS polymerization reaction is completed, although most of the NMP can be recovered by conventional methods, the remaining 25% to 30% of the NMP will combine with LiCl to form a complex sim

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  • A method for comprehensive recovery and utilization of lithium containing mixed salts in a polyphenylene sulfide production process
  • A method for comprehensive recovery and utilization of lithium containing mixed salts in a polyphenylene sulfide production process

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Embodiment Construction

[0023] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0024] by figure 1 The shown process scheme recycles the PPS by-product slurry, and after the slurry is distilled and dried under reduced pressure, NaCl, Li 2 CO 3 , organic matter were 80.81%, 12.47% and 6.72%.

[0025] Concentrated HCl and methanol solution were mixed to prepare acidic methanol solution, and the secondary extraction was carried out under the condition that the solid-liquid ratio was 1:1. The single extraction time was 1 hour, and the pH of the solution after the reaction was about 2. Then use 5% NaOH solution to adjust the pH of the leaching solution after the reaction to about 6.5, and separate by filtration to obtain a wet solid phase and a liquid phase.

[0026] The above wet solid phase was air-dried at 70° C. for 30 minutes to remove entrained methanol. Then under the condition of solid-liquid 1:1.3, dissolve and ext...

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Abstract

A method for comprehensive recovery and utilization of lithium containing mixed salts in a polyphenylene sulfide (PPS) production process is disclosed. Na<2>CO3 is added into PPS byproduct slurry, rectification is performed to separate and recover a solvent that is NMP, then obtained lithium containing mixed salts are subjected to dissolution and leaching through an acidic methanol solution, and a wet solid phase and a liquid phase are obtained after pH adjustment and filtration. The wet solid phase is dried, dissolved with water and purified to obtain a refined NaCl solution. The liquid phase is subjected to rectification, ethanol leaching, evaporation, water leaching, purification and evaporative crystallization to obtain a high-purity water-free LiCl product. The method can be used for comprehensive recovery and utilization of the lithium containing mixed salts in the PPS production process. The recovered refined NaCl solution can be directly used for ionic membrane electrolysis to prepare caustic soda, and the LiCl can be directly used as a PPS production auxiliary agent for cyclic use.

Description

technical field [0001] The invention belongs to the production field of polyphenylene sulfide (PPS), and relates to a method for comprehensive recovery and utilization of by-products in the industrial production of polyphenylene sulfide, especially a method for comprehensive recovery and utilization of lithium-containing mixed salts in the production process of polyphenylene sulfide . Background technique [0002] In the process of producing PPS with sodium sulfide and p-dichlorobenzene as raw materials, a large amount of NaCl will be produced by-product, and because the process needs to add N-methylpyrrolidone (NMP) as a solvent and LiCl as an auxiliary agent, after separating PPS The slurry contains NaCl, LiCl, NMP and other components. Since LiCl and NMP are expensive, if they are not recycled effectively, the production cost will increase dramatically. [0003] For the recovery of by-products, solvents, additives, etc. in the PPS production process, there are currently...

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Application Information

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IPC IPC(8): C07D207/267C01D3/04C01D15/04
CPCC01D3/04C01D15/04C07D207/267
Inventor 余晓平邓天龙李珑王士强郭亚飞李乾华吕天生胡洪铭陈尚敬谢晓鸿张思思
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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