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Polythiocarbonate and preparation method thereof

A technology of polymonothiocarbonate and carbon oxysulfide, applied in the field of polymonothiocarbonate and its preparation, can solve the problems of lack of catalyst, inability to effectively inhibit oxygen-sulfur exchange reaction and the like, and achieve 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 may be that there is no suitable catalyst and the inability to effectively inhibit the oxygen-sulfur exchange reaction

Method used

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  • Polythiocarbonate and preparation method thereof
  • Polythiocarbonate and preparation method thereof
  • Polythiocarbonate and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Before the polymerization reaction, the 10 mL autoclave was vacuum-dried at 110° C. for 2 hours to remove water, and then cooled to room temperature. Add 1.0 mg of Zn-Co DMCC (catalyst addition is 0.01% of the total mass of epoxy monomers) to the reactor in turn, then add 2.0 mL of 1,2-propylene oxide (PO) and pass through the specified mass of COS (COS / PO molar ratio 0.5:1). Then the autoclave was closed and placed in an oil bath at 20 °C for 1 h under autogenous pressure. After the reaction was completed, it was cooled to room temperature, and the yellow product was taken out. First remove the solvent under reduced pressure, then use 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 polymer was calculated by proton nuclear magnetic spectrum. The test results are shown in Tab...

Embodiment 2

[0036] Adopt the method of embodiment 1, the only difference is that the epoxide added is 1,2-epoxybutylene. The test results are shown in Table 2.

Embodiment 3

[0038] Before the polymerization reaction, the 10 mL autoclave was vacuum-dried at 110° C. for 2 hours to remove water, and then cooled to room temperature. Add Zn-Co DMCC (the amount of catalyst added is 0.05% of the total mass of epoxy monomers) to the reactor in sequence, then add 2.0 mL of isobutylene oxide, and introduce a specified mass of COS (COS / epoxy molar ratio 1:1). Then the autoclave was closed and placed in an oil bath at 60 °C for 1 h under autogenous pressure. Other treatments are the same as in Example 1, and the test results are shown in Table 2.

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Abstract

The invention relates to the field of high molecular material synthesis and aims at providing polythiocarbonate and a preparation method thereof. The preparation method comprises the following steps of: adding an epoxide, carbon oxysulfide and a catalyst into a dry high-pressure reaction kettle, carrying out reaction for 1-12 hours at 20-150 DEG C and self-generated pressure, purifying the generated product and drying the generated product to obtain a polythiocarbonate product, wherein the catalyst is a zinc-cobalt double-metal cyanide complex or a silicon dioxide loaded zinc-cobalt double-metal cyanide complex. The polythiocarbonate provided by the invention has wide purposes, the refractive index of the polymerized product is obviously higher than that of a general polymer, such as a COS (Carbon Oxysulfide)-cyclohexene oxide copolymer, and is 1.66, and therefore the polythiocarbonate has potential use in the aspect of a light-guide fiber.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and specifically relates to a degradable polymonothiocarbonate synthesized by one-step addition polymerization of carbon oxysulfide and epoxy compounds under catalytic conditions 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 rin...

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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