Method for preparing aliphatic polythioether

Patent metadata

Field	Value
Publication number	US-11440995-B2
Application number	US-202117233413-A
Country	US
Kind code	B2
Filing date	Apr 16, 2021
Priority date	Oct 31, 2018
Publication date	Sep 13, 2022
Grant date	Sep 13, 2022

Abstract

A method for preparing aliphatic polythioether is provided. In the method, aliphatic polythioether is obtained by polymerization reaction using a sulfur-carbon compound and an oxygen-containing monomer as raw materials and using Lewis base as a catalyst, and the polymerization reaction is performed under a self-generated pressure at 80˜180° C. Based on the defects of the traditional preparation process of aliphatic polythioether, a bran-new synthetic routine is provided, in which a new process for preparing polythioether in one-pot reaction is achieved through oxygen-sulfur exchange reaction between the sulfur-carbon compound and the oxygen-containing monomer.

First claim

We claim:

1. A method for preparing aliphatic polythioether, which is obtained by polymerization reaction using a sulfur-carbon compound and an oxygen-containing monomer as raw materials and using only bis(triphenylphosphoranyl) ammonium chloride as a catalyst;
the polymerization reaction is performed under a self-generated pressure at 130˜180° C.;
a molar ratio of the sulfur-carbon compound to the oxygen-containing monomer is 1 5:1;
a molar ratio of the catalyst to the oxygen-containing monomer is 1:10˜500;
the sulfur-carbon compound is selected from at least one of carbon disulfide and carbon oxysulfide;
the oxygen-containing monomer is selected from at least one of epoxide, oxetane and 3-substituted oxetane.

2. The method for preparing aliphatic polythioether according to claim 1 ,
wherein the epoxide is ethylene oxide;
the 3-substituted oxetane is selected from at least one of 3,3-dimethlyoxetane, 3-methyl-3-benzyloxymethyloxetane,3-chloromethyl-3-methlyxetane,3-methyl-3-oxetane methanol,3-oxetanone, 3-(allyloxy) oxetane and 3-bromooxetane.

3. The method for preparing aliphatic polythioether according to claim 1 , wherein the polymerization reaction is bulk polymerization.

4. The method for preparing aliphatic polythioether according to claim 1 , wherein the polymerization reaction is solution polymerization, a solvent is dichloromethane.

5. The method for preparing aliphatic polythioether according to claim 1 , specifically comprising:
polymerizing in a high-pressure reactor under dry and oxygen-free conditions by using the sulfur-carbon compound and the oxygen-containing monomer as polymerization monomers and using the Lewis base as the catalyst, followed by adding alcohol-hydrochloric acid solution and posttreating to obtain the aliphatic polythioether.

Assignees

• Univ Zhejiang

Inventors

• Zhang Xinghong
• Zhang Chengjian

Classifications

• C08G75/0268

  using disulfides · CPC title

• C08G75/0272

  using other sulfur sources · CPC title

• C08G75/0209 Primary

  derived from monomers containing one aromatic ring · CPC title

• C08G75/02 Primary

  Polythioethers · CPC title