Poly(monothiocarbonic ester) containing crystals and preparation method of poly(monothiocarbonic ester)

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: 2016-12-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, there have been no reports of biodegradable

Method used

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  • Poly(monothiocarbonic ester) containing crystals and preparation method of poly(monothiocarbonic ester)
  • Poly(monothiocarbonic ester) containing crystals and preparation method of poly(monothiocarbonic ester)
  • Poly(monothiocarbonic ester) containing crystals and preparation method of poly(monothiocarbonic ester)

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 1 (Salen) CrX catalyst catalyzed the one-pot copolymerization of COS / OX into polymonothiocarbonate

[0042] Before the polymerization reaction, the 10mL autoclave was heated at 110°C for about 2 hours to remove the water and cooled to room temperature in a desiccator; in turn, several masses of SalenCrX catalyst 1a and co-catalyst bis(triphenylphosphorane) were added to the reactor. Base) ammonium chloride ([PPN]Cl), the two are equal in moles; the molar ratio of catalyst to monomer OX is 1 / 250; then 3.8gCOS and 2.0mL OX (COS to OX molar ratio 2:1) are added. Then the autoclave was sealed and placed in an oil bath at 120°C for 4h reaction under autogenous pressure. After the reaction, it was cooled to room temperature, and a yellow product was taken out. First use DMSO to heat to 130°C to dissolve the crude product, then precipitate the polymer in methanol, repeat the washing three times to obtain a white product, and vacuum dry to constant weight. The conversion...

Example Embodiment

[0043] Example 2 (Salen) CrX catalyst catalyzed the one-pot copolymerization of COS / OX into polymonothiocarbonate

[0044] Before the polymerization reaction, the 10 mL autoclave was heated at 110°C for about 2 hours to remove water and cooled to room temperature in a desiccator. Sequentially add several masses of SalenCrX catalyst 1a and co-catalyst 1,5,7-diazabicyclo[5.4.0]undec-7-carbene (TBD) into the reactor, with equal moles. 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, it was cooled to room temperature, and a yellow product was taken out. First use DMSO to heat to 130°C to dissolve the crude product, then precipitate the polymer in methanol, repeat the washing three times to obtain a white product, and vacuum dry to constant weight. The conversion rate is calculated by the...

Example Embodiment

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

[0046] Before the polymerization reaction, the 10 mL autoclave was heated at 110°C for about 2 hours to remove water and cooled to room temperature in a desiccator. Several masses of SalenCrX catalyst 1b and co-catalyst cetyltrimethylammonium bromide (CTAB) were sequentially added to the reactor, and the two were equimolar. 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 reaction under autogenous pressure for 24 hours. After the reaction, it was cooled to room temperature, and a yellow product was taken out. First use DMSO to heat to 130°C to dissolve the crude product, then precipitate the polymer in methanol, repeat the washing three times to obtain a white product, and vacuum dry to constant weight. The conversion rate is...

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Abstract

The invention discloses poly(monothiocarbonic ester) containing crystals and a preparation method of poly(monothiocarbonic ester), and belongs to the field of polymer materials. The method includes the steps of adding carbon oxysulfide, oxetane, third monomer, chain transfer agent, catalyst and promoter into a dry high-pressure reaction still, conducting copolymerization reaction for 0.5-24 hours on a body or a solution under the self-generated pressure at a temperature of 0-150 DEG C, and conducting purifying and drying to obtain poly(monothiocarbonic ester) containing crystals. Prepared poly(monothiocarbonic ester) containing crystals contains sphero-crystal structures in the crystals and has the crystallinity of 13-85%, the crystallization temperature of 60-110 DEG C, the melting temperature of 100-135 DEG C and the melting enthalpy value of 4-90 J/g. By means of the method, oxygen-sulfur exchange reaction is completely restrained at high polymerization temperature, poly(monothiocarbonic ester) clear in structure and adjustable in crystallization property is obtained, and poly(monothiocarbonic ester) has a degradable thiocarbonic ester structure, can crystallize like high density polyethylene, has a wide processing window and 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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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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