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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

Active Publication Date: 2017-06-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalytic system can be obtained only by compounding, and there is no problem of metal residue and color residue

Method used

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  • Method for preparing poly(monothiocarbonate)
  • Method for preparing poly(monothiocarbonate)
  • Method for preparing poly(monothiocarbonate)

Examples

Experimental program
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Effect test

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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Abstract

The invention discloses a method for preparing poly(monothiocarbonate). According to the method, carbon oxysulfide and oxygen-containing monomers are used as raw materials; a catalysis system consisting of initiators and Lewis acid is used; after the bulk polymerization or solution polymerization, poly(monothiocarbonate) is obtained; the oxygen-containing monomers are selected from at least one kind of materials of epoxy compounds, oxetane and 3-substituted oxetane; the initiators are selected from quaternary ammonium salt, quaternary phosphonium salts or organic alkali. The preparation method of synthesizing the poly(monothiocarbonate) through anion ring-opening polymerization by using a catalytic system formed by at least one kind of materials from quaternary ammonium salt, quaternary phosphonium salts or organic alkali, and the Lewis acid; the poly(monothiocarbonate) with the specific chain structures can be obtained through preparation. The catalysis system can be obtained only through compounding; the metal residue and color residue problems do not exist.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and in particular relates to a polymonothiocarbonate and a preparation method thereof. Background technique [0002] Polythiocarbonate is a sulfur-containing polymer with excellent optical properties, chemical stability and good heavy metal ion adsorption capacity. It has broad application prospects in high-performance optical fiber manufacturing, adhesives and wastewater treatment containing heavy metal ions . Usually polythiocarbonate is prepared by reacting dithiol with phosgene or chloroform in an organic solvent. Due to the toxicity of the raw materials phosgene, chloroform and solvents used, this synthetic route is difficult to survive. Another method for synthesizing polythiocarbonates is through the ring-opening polymerization of five- or six-membered rings of mono-, di-, and trithiopropylene carbonates. However, these five-membered ring or six-membered ring compounds are usual...

Claims

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Application Information

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IPC IPC(8): C08G64/38C08G64/20C08L69/00C09D169/00
CPCC08G64/20C08G64/38C08L69/00C09D169/00
Inventor 张兴宏杨嘉良张滢滢吴海林李洋
Owner ZHEJIANG UNIV
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