Method for preparing carbon oxysulfide and co-producing sulfur-containing polymer

A technology of carbon oxysulfide and polymers, applied in the direction of carbon oxysulfide and carbon sulfur compounds, etc., can solve the problems of waste generation, long process, increased cost, etc., achieve good universality, reduce environmental impact, and avoid purification steps Effect

Inactive Publication Date: 2019-09-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The preparation method of the above patent documents has a relatively long process and produces many by-products, so a re...

Method used

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  • Method for preparing carbon oxysulfide and co-producing sulfur-containing polymer
  • Method for preparing carbon oxysulfide and co-producing sulfur-containing polymer
  • Method for preparing carbon oxysulfide and co-producing sulfur-containing polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Example 1 CS 2 / PO to prepare carbon oxysulfide and co-production with PO to prepare polymonothiocarbonate

[0050] Before the polymerization reaction, 10mL of reactor I and reactor II were dehydrated at 110°C for about 2 hours, cooled to room temperature in a desiccator, and connected through valves and pipelines; the valves were closed at the initial stage, and the reactors were supplied to reactor I in turn. Add some quality Lewis (Lewis) base 1 1,8-diazabicyclo[5.4.0]undec-7-decene (DBU); the molar ratio of Lewis base 1 to propylene oxide (PO) is 1 :10; add CS again 2 , PO(CS 2 with PO molar ratio 1:1) and 1 mL of toluene. Then the reactor I was closed and placed in an 80°C oil bath for 0.5h under autogenous pressure. After the reaction, the reactor I was cooled to room temperature. Several masses of PO, Lewis base 11,8-diazabicyclo[5.4.0]undec-7-decene (DBU) and Lewis acid triethylboron and 1 mL THF were added to Reactor II; Lewis base 1 Reactor II was closed...

Embodiment 2

[0052] Example 2 CS 2 / PO to prepare carbon oxysulfide and co-production with PO to prepare polymonothiocarbonate

[0053] Before the polymerization reaction, 10mL of reactor I and reactor II were dehydrated at 110°C for about 2 hours, cooled to room temperature in a desiccator, and connected through valves and pipelines; the valves were closed at the initial stage, and the reactors were supplied to reactor I in turn. Add some quality Lewis base 2 1,5,7-triazabicyclo[4.4.0]dec-5-ene (TBD); the molar ratio of Lewis base 2 and propylene oxide (PO) is 1 / 500; Rejoin CS 2 , PO(CS 2 with PO molar ratio 3:1) and 1 mL of toluene. Then the reactor I was closed and placed in an oil bath at 80° C. for 6.0 h under autogenous pressure. After the reaction, the reactor I was cooled to room temperature. Several masses of PO, Lewis base 2 1,5,7-triazabicyclo[4.4.0]dec-5-ene (TBD) and Lewis acid triethylboron and 1 mL of DMF were added to Reactor II; Lewis base 2 The molar ratio to propyl...

Embodiment 3

[0054] Example 3 CS 2 / PO to prepare carbon oxysulfide and co-production with PO to prepare polymonothiocarbonate

[0055] Before the polymerization reaction, the 10mL two reactors I and II were dehydrated at 110°C for about 2 hours, cooled to room temperature in a desiccator, and connected through valves and pipelines; the valves were closed at the initial stage, and the reaction Add some quality Lewis base 3 sodium methylate in the device I; the molar ratio of Lewis base 3 and propylene oxide (PO) is 1 / 500; add CS 2 , PO(CS 2 with PO molar ratio 10:1) and 1 mL of toluene. Then the reactor I was closed and placed in an oil bath at 100° C. for 0.5 h under autogenous pressure. After the reaction, the reactor I was cooled to room temperature. Add several masses of PO, Lewis base 3 sodium methoxide and Lewis acid tributylboron and 1 mL THF to reactor II; the molar ratio of Lewis base 3 to propylene oxide (PO) is 1 / 400, and the molar ratio of Lewis acid to The ratio is 1 / 5 an...

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Abstract

The invention discloses a method for preparing carbon oxysulfide and co-producing a sulfur-containing polymer. The method includes the following steps: using carbon disulfide and an oxygen-containingmonomer A as raw materials, under the catalysis and initiation effects of Lewis base M, obtaining COS by an oxygen-sulfur exchange reaction and generating an aliphatic polythioether, wherein the reaction temperature is 60-180 DEG C; and reacting the generated COS with an oxygen-containing monomer B under the catalysis effect of Lewis base N and/or Lewis acid to obtain poly(mono thiocarbonate), wherein the reaction temperature is 0-100 DEG C. The method uses an oxygen-sulfur exchange reaction between carbon disulfide and the oxygen-containing oxide to prepare carbon oxysulfide and a plurality of sulfur-containing polymers. The used catalysts can be purchased. No problems of metal residue and color residue exist. The method has good universality and is suitable for large-scale industrial production. Three products with high added value are obtained from two products. Therefore, the prepared aliphatic polythioethers and poly(mono thiocarbonate) are abundant in variety, and the types and applications of sulfur-containing polymers are expanded.

Description

technical field [0001] The invention relates to the technical fields of synthetic chemistry and macromolecular chemical synthesis, in particular to a method for preparing carbon oxysulfide and co-producing sulfur-containing polymers. Background technique [0002] Carbon oxysulfide (COS) can be used to produce urea, carbonate, thiocarbamate and heterocyclic compounds, etc. It is an important basic chemical raw material. In addition, COS is used more as a soil fumigant and as a fumigant for storing crop products. COS was first synthesized by Hungarian scientists in 1867, and in 1970, the Japanese Ihara Chemical Industry Company first realized large-scale industrial production. [0003] There are many synthetic methods of COS, including dry method and wet method. Dry synthesis mainly uses CO and sulfur vapor to generate COS under solvent-free conditions. The process of this method is simple and the yield is high. Considering the cost and source of raw materials, industrial p...

Claims

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Application Information

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IPC IPC(8): C08G75/28C08G75/02C01B32/77
CPCC01B32/77C08G75/02C08G75/28
Inventor 张兴宏张成建
Owner ZHEJIANG UNIV
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