A kind of separation and recovery method of NMP and catalyst lithium chloride in polyphenylene sulfide production
The technology of a polyphenylene sulfide and a recovery method, which is applied in the direction of chemical recovery and the like, can solve the problems of low recovery rate of lithium chloride, affecting production costs and high prices, and achieve the effects of low cost, simple operation and high purity.
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Embodiment 1
[0015] Take 600ml polyphenylene sulfide polycondensation mother liquor, and carry out vacuum distillation at -0.096MPa pressure and 130°C in a rotary evaporator until it is completely evaporated to dryness. The evaporated solvent NMP is condensed with 20°C water to obtain 465.4g NMP and 121.2 g distillation residue, the total recovery of NMP was 96.9%.
[0016] Take 120ml of clear water, add it to the evaporator bottle, heat to 40°C, stir, and fully dissolve the distillation residue. The feed liquid was filtered, and the filter cake was washed twice with 160ml of clear water, and the combined filtrate and washing water were a mixed solution, a total of 222ml, and the Li concentration measured by an atomic absorption spectrophotometer was 3862mg / L.
[0017] Take 100ml of the mixed solution, add 2.3g of 80% phosphoric acid dropwise, react for 60min under stirring, and form white lithium phosphate precipitate, filter, wash with water and dry to obtain 2.05g of lithium phosphate w...
Embodiment 2
[0019] LiAlO 2 +HCl+H 2 O==LiCl+Al(OH) 3
[0020] The aluminum hydroxide precipitate was washed twice with water, and dried to obtain 8.94 g of aluminum hydroxide, with a content of 96.6%. Add 30% sodium hydroxide dropwise to make it fully dissolved, pH11-12.5, and use it repeatedly as a precipitating agent. The filtrate is a lithium chloride solution, which is reused in the polyphenylene sulfide polycondensation reaction. Take 600ml of polyphenylene sulfide polycondensation mother liquor, and carry out vacuum distillation at -0.085MPa pressure and 160°C in a rotary evaporator until it is completely evaporated to dryness. The evaporated solvent NMP is condensed with water at 20°C to obtain 462.7g of NMP and 123.4 g distillation residue, the total recovery of NMP is 95.2%.
[0021] Take 120ml of clear water, add it to the evaporator bottle, heat to 40°C, stir to fully dissolve the slag. The feed liquid is filtered, and washed twice with 160ml of clear water, and t...
Embodiment 3
[0027] Take 600ml of polyphenylene sulfide polycondensation mother liquor, and carry out vacuum distillation at -0.085MPa pressure and 160°C in a rotary evaporator until it is completely evaporated to dryness. The evaporated solvent NMP is condensed with water at 20°C to obtain 462.7g of NMP and 123.4 g distillation residue, the total recovery of NMP is 95.2%.
[0028] Take 150ml of clear water, add it to the evaporator bottle, heat to 40°C, stir to fully dissolve the slag. The feed liquid was filtered, and the filter cake was washed twice with 50ml of clear water, and the combined filtrate and washing water were a mixed solution of 160ml, and the Li concentration recorded by an atomic absorption spectrophotometer was 5453mg / L.
[0029] Take 200ml of mixed solution, drop into 30% sodium aluminate (NaAlO 2 ) 30ml, and reacted for 90min under stirring to form a white lithium aluminate precipitate, which was filtered, washed with water and dried to obtain lithium aluminate (LiAl...
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