Method for preparing poly(monothiocarbonate)
A technology of polymonothiocarbonate and carbon oxysulfide, applied in polycarbonate coatings, coatings, etc., to achieve the effect of clear structure, regular structure and wide application prospects
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Embodiment 1
[0044] Embodiment 1 COS / PO one-pot copolymerization synthesizes polymonothiocarbonate
[0045] Before the polymerization reaction, remove the water in a 10mL high-pressure reactor at 110°C for about 2 hours and cool it to room temperature in a desiccator; add several quantities of initiator 1 bis(triphenylphosphoryl) chloride to the reactor in sequence Ammonium chloride ([PPN]Cl) and triethylboron (TEB), the molar ratio of the two is 1:2; the molar ratio of initiator 1 and propylene oxide (PO) is 1 / 1000; add COS, PO ( COS to PO molar ratio 2:1) and 3 mL tetrahydrofuran (THF). Then the autoclave was closed and placed in an oil bath at 25°C for 8 hours under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with tetrahydrofuran, then precipitate the polymer in a mixture of ethanol / deionized water / hydrochloric acid, repeat washing three times, and vacuum-dry to constant weight. The content of each chain segment in the polymer was...
Embodiment 2
[0047] Example 2 One-pot copolymerization of COS / PO to synthesize polymonothiocarbonate
[0048] Before the polymerization reaction, the 10mL autoclave was dehydrated at 110°C for about 2 hours and cooled to room temperature in a desiccator; several quantities of initiator 2 dodecyltrimethylammonium bromide were added to the autoclave in sequence (DTMeAB) and triethylboron (TEB), the molar ratio of the two is 1:1; the molar ratio of initiator 2 and propylene oxide (PO) is 1 / 500; add COS, PO (COS and PO molar ratio 2:1) and 3 mL tetrahydrofuran (THF). Then the autoclave was closed and placed in an oil bath at 60°C for 6 hours under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with tetrahydrofuran, then precipitate the polymer in a mixture of ethanol / deionized water / hydrochloric acid, repeat washing three times, and vacuum-dry to constant weight. The content of each chain segment in the polymer was calculated by proton nucl...
Embodiment 3
[0049] Example 3 One-pot copolymerization of COS / PO into polymonothiocarbonate
[0050] Before the polymerization reaction, the 10mL autoclave was dehydrated at 110°C for about 2 hours and cooled to room temperature in a desiccator; several quantities of initiator 3 tetrabutylammonium chloride [N(iBu ) 4 Cl] and triethylboron (TEB), both molar ratio is 1:0.1; The molar ratio of initiator 3 and propylene oxide (PO) is 1 / 500; Add COS, PO again (COS and PO molar ratio 2 : 1) and 3 mL tetrahydrofuran (THF). Then the autoclave was closed and placed in an oil bath at 120° C. for 4 h under autogenous pressure. Cool to room temperature after the reaction, first dissolve the crude product with tetrahydrofuran, then precipitate the polymer in a mixture of ethanol / deionized water / hydrochloric acid, repeat washing three times, and vacuum-dry to constant weight. The content of each chain segment in the polymer was calculated by proton nuclear magnetic spectroscopy, and the molecular wei...
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