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A kind of crystal-containing polymonothiocarbonate and preparation method thereof

A technology of polymonothiocarbonate and crystal, which is applied in the field of polymonothiocarbonate containing crystals and its preparation, and can solve problems such as unsatisfactory crystalline polymers.

Active Publication Date: 2021-04-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there have been no reports of biodegradable crystalline polymers that meet the above conditions

Method used

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  • A kind of crystal-containing polymonothiocarbonate and preparation method thereof
  • A kind of crystal-containing polymonothiocarbonate and preparation method thereof
  • A kind of crystal-containing polymonothiocarbonate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 (Salen) CrX catalyst catalyzes COS / OX one-pot copolymerization into polymonothiocarbonate

[0042] 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 masses of SalenCrX catalyst 1a and cocatalyst bis(triphenylphosphorane base) ammonium chloride ([PPN]Cl), the two are equimolar; the molar ratio of the catalyst to the monomer OX is 1 / 250; then add 3.8g COS and 2.0mL OX (the molar ratio of COS to OX is 2:1). Then the autoclave was closed and placed in an oil bath at 120° C. for 4 h under autogenous pressure. After the reaction was completed, it was cooled to room temperature, and the yellow product was taken out. The crude product was first dissolved by heating to 130°C with DMSO, and then the polymer was precipitated in methanol. The white product was obtained by repeated washing three times, and dried in vacuo to constant weight. Calculate the conversion r...

Embodiment 2

[0043] Embodiment 2 (Salen) CrX catalyst catalyzes COS / OX one-pot copolymerization into polymonothiocarbonate

[0044] 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 masses of SalenCrX catalyst 1a and co-catalyst 1,5,7-diazabicyclo[5.4.0]undec-7-decene (TBD) were sequentially added into the reactor, both in equal molar numbers. The molar ratio of catalyst to monomer OX is 1 / 5000. Then add 4.8g COS and 1.0mL OX (the molar ratio of COS to OX is 5:1). Then the autoclave was closed and placed in an oil bath at 150° C. for 0.5 h under autogenous pressure. After the reaction was completed, it was cooled to room temperature, and the yellow product was taken out. The crude product was first dissolved by heating to 130°C with DMSO, and then the polymer was precipitated in methanol. The white product was obtained by repeated washing three times, and dried in vacuo to constant wei...

Embodiment 3

[0045] Embodiment 3 (Salen) CrX catalyst catalyzes COS / OX one-pot copolymerization into polymonothiocarbonate

[0046] Before the polymerization reaction, the 10mL autoclave was dehydrated at 110°C for about 2 hours and cooled to room temperature in a desiccator. Add several qualities of SalenCrX catalyst 1b and co-catalyst cetyltrimethylammonium bromide (CTAB) in the reactor in sequence, both in equimolar numbers. The molar ratio of catalyst to monomer OX is 1 / 2500. Then add 1.4g COS and 3.0mL OX (the molar ratio of COS to OX is 0.5:1). Then the autoclave was closed and placed in an ice bath at 0 °C for 24 h under autogenous pressure. After the reaction was completed, it was cooled to room temperature, and the yellow product was taken out. The crude product was first dissolved by heating to 130°C with DMSO, and then the polymer was precipitated in methanol. The white product was obtained by repeated washing three times, and dried in vacuo to constant weight. Calculate the...

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Abstract

The invention discloses a crystal-containing polymonothiocarbonate and a preparation method thereof, belonging to the field of polymer materials. The method of the present invention is as follows: carbon oxysulfide, oxetane, the third monomer, chain transfer agent, catalyst and cocatalyst are added into a dry high-pressure reactor, and the bulk or solution Copolymerize for 0.5 to 24 hours, and then obtain crystal-containing polymonothiocarbonate after purification and drying; the obtained crystal-containing polymonothiocarbonate: crystals contain spherulite structure, and the degree of crystallinity is 13-85%, The crystallization temperature is 60-110°C, the melting temperature is 100-135°C, and the melting enthalpy value is 4-90J / g. This method achieves the complete inhibition of oxygen-sulfur exchange reaction at higher polymerization temperature, and obtains polymonothiopolycarbonate with clear structure and adjustable crystallinity, which has a degraded thiocarbonate structure and can be as high as Density polyethylene is crystal-like, has a wide processing window, and also has high strength and toughness.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and in particular relates to a crystal-containing 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/38
CPCC08G64/38C08G2230/00
Inventor 张兴宏杨嘉良吴海林李洋张滢滢
Owner ZHEJIANG UNIV
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