Preparation method of polyphenylene sulfide
A technology of polyphenylene sulfide and p-dichlorobenzene, which is applied in the field of preparation of polyphenylene sulfide, can solve the problems of low solvent recovery rate, high price, and large consumption, and achieve the effect of improving the hue
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Embodiment 1
[0027] 1. Mix 120g sodium sulfide (Na 2 S·9H 2 O), 178g of N-methylpyrrolidone (NMP), 1.68g of lithium chloride, and 3.62g of sodium thiosulfate were added to the polymerization kettle, and the inert gas was used to replace the air, followed by heating and dehydration, and the dehydration rate was stopped when the dehydration rate reached 82%.
[0028] 2. Add 116g of p-dichlorobenzene (P-DCB) in NMP solution (containing 75.7g of P-DCB) to the system after dehydration in step (1), and react at 230°C for 5h. After the reaction is finished, a mixed slurry containing PPS resin, solvent, oligomer and inorganic salt is obtained.
[0029] 3. Filter the mixed slurry, add the filter cake into boiled pure water, stir and wash and ultrasonically treat for 15~30min. Repeat this operation 3 times to obtain PPS resin after drying.
[0030] The PPS resin product is white, with a yield of 94.1%, a melting point of 294°C, and an ignition residue of 0.19%.
Embodiment 2
[0032] With embodiment 1, difference is:
[0033] In step (1), sodium thiosulfate is 2.57g, and the dehydration rate is 89%;
[0034] The reaction in step (2) was carried out at 210° C. for 4 h.
[0035] The PPS resin product is white, with a yield of 89.7%, a melting point of 282°C, and an ignition residue of 0.17%.
Embodiment 3
[0037] With embodiment 1, difference is:
[0038] Step (1), the dehydration rate is 80%;
[0039] The PPS resin product is white, with a yield of 91.2%, a melting point of 284°C, and an ignition residue of 0.18%.
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