Preparation method of polymonosulfo-carbonate with regular chain structure

A technology of polymonothiocarbonate and chain structure, which is applied in the field of preparation of polymonothiocarbonate, can solve the problems of inability to effectively inhibit the oxygen-sulfur exchange reaction and lack of catalyst, and achieve easy operation, simple polymerization method, The effect of high catalytic efficiency

Active Publication Date: 2013-09-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main reason is that there is no suitable catalyst for regioselective polymeriz

Method used

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  • Preparation method of polymonosulfo-carbonate with regular chain structure
  • Preparation method of polymonosulfo-carbonate with regular chain structure
  • Preparation method of polymonosulfo-carbonate with regular chain structure

Examples

Experimental program
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Effect test

Embodiment 1

[0043] 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 some quality SalenCrX catalyst 1a (such as figure 1 ) and cocatalyst N-methylimidazole (N-MeIm), both in equimolar numbers. The total molar ratio of the catalyst to the epoxy monomer is 1 / 10000. Then add 2.0 mL of 1,2-propylene oxide and the specified mass of COS (the molar ratio of COS to epoxy monomer is 0.5 / 1). Then the autoclave was closed and placed in an oil bath at 30 °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 solvent was removed under reduced pressure, and then CH 2 Cl 2 The crude product was dissolved, the polymer was precipitated in methanol, and the yellow product was obtained after vacuum drying. The conversion rate was calculated by weighing method, and the content of each chain segment in the polyme...

Embodiment 2

[0045] 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 some quality SalenCrX catalyst 2a (such as figure 1 ) and cocatalyst 4-dimethylaminopyridine (DMAP), both in equimolar numbers. The total molar ratio of the catalyst to the epoxy monomer is 1 / 10000. Then add 2.0 mL of 1,2-epoxybutane and the specified mass of COS (the molar ratio of COS to epoxy monomer is 0.5 / 1). Then the autoclave was closed and placed in an oil bath at 30 °C for 6 h under autogenous pressure. Other treatments are the same as in Example 1. The test results are shown in Table 1.

Embodiment 3

[0047] 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 some quality SalenCrX catalysts 3a (such as figure 1 ) and cocatalyst bis(triphenylphosphoryl)ammonium chloride ([PPN]Cl), both in equimolar numbers. The total molar ratio of the catalyst to the epoxy monomer is 1 / 2000. Then add 2.0 mL of α-n-pentene oxide and the specified mass of COS (the molar ratio of COS to epoxy monomer is 1 / 1). Then the autoclave was closed and placed in an oil bath at 30 °C for 6 h under autogenous pressure. Other treatments are the same as in Example 1. The test results are shown in Table 1.

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Abstract

The invention relates to the field of synthesis of a high polymer material and aims to provide a preparation method of polymonosulfo-carbonate with a regular chain structure. The preparation method comprises the following steps of: adding epoxide, carbonyl sulfide, a catalyst and a catalyst promoter to a dry high-pressure reaction kettle, reacting for 0.5 hour -12.0 hours under self pressure at 0 DEG C-80 DEG C; and purifying and drying to obtain polymonosulfo-carbonate. The catalyst adopted by the preparation method disclosed by the invention has very high catalytic efficiency, and the method which is provided by the invention is different from a ring opening polymerization method for synthesizing polymonosulfo-carbonate in a controllable manner. The polymerization method is simple and easy to operate, and capable of accurately adjusting the polymer structure by adjusting the reaction conditions. The polymonosulfo-carbonate provided by the invention can be used more extensively; and the obtained product has a higher refractive index, for example, the COS-PO copolymer has the refractive index of 1.63, which is remarkably higher than that of the common copolymer, and therefore, the preparation method has a potential application to special optical materials such as adhesives.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and specifically relates to a method for preparing polymonothiocarbonate with regular chain structure, which is synthesized by one-step addition polymerization of carbon oxysulfide as C1 monomer and epoxy compound under catalytic conditions. 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...

Claims

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Application Information

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IPC IPC(8): C08G64/38
Inventor 张兴宏罗铭杜滨阳戚国荣
Owner ZHEJIANG UNIV
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