A kind of preparation method of sulfur dioxide and epoxy compound copolymer

An epoxy compound and sulfur dioxide technology, which is applied in the field of polymer material preparation, can solve the problems of low molecular weight of the copolymer, low catalytic activity, harsh reaction conditions, etc., and achieves a simple preparation method, shortened reaction time, and low catalyst dosage. Effect

Active Publication Date: 2017-08-25
KUNMING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the current harsh conditions for the copolymerization of epoxy compounds and sulfur dioxide, the defects of low catalytic activity and low copolymer molecular weight, using epoxy compounds and sulfur dioxide as monomers, using SalenMX as a catalyst, under milder conditions Preparation of Copolymer of Epoxy Compound and Sulfur Dioxide

Method used

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  • A kind of preparation method of sulfur dioxide and epoxy compound copolymer
  • A kind of preparation method of sulfur dioxide and epoxy compound copolymer
  • A kind of preparation method of sulfur dioxide and epoxy compound copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 20mL of epoxycyclohexane and 118.6mg of SalenCr into a 50ml autoclave Ⅲ Cl catalyst;

[0025] (2) Introduce 99.0% nitrogen into the sealed autoclave, and after repeating the nitrogen twice, then inject sulfur dioxide with a purity of 99.0% into the autoclave, and the pressure of sulfur dioxide is 0.1MPa;

[0026] (3) After the feeding is completed, close the inlet and outlet valves, set the speed at 280 r / min, the temperature at 50°C, and the reaction time at 6 hours;

[0027] (4) Dissolve the obtained product in chloroform, add hydrochloric acid methanol mixture (volume ratio, methanol / hydrochloric acid = 6) for precipitation, obtain an amber precipitate after filtration, wash with methanol for 3 times, and place the washed precipitate in a vacuum In a drying oven, vacuum dry at room temperature for 8 hours to obtain a copolymer of sulfur dioxide and epoxy compounds. The number-average molecular weight determined by gel permeation chromatography was 6320 g / mo...

Embodiment 2

[0029] (1) Add 30mL of epoxycyclohexane and 177.9mg of SalenMn into a 50ml autoclave Ⅱ Cl catalyst;

[0030] (2) Introduce 99.0% nitrogen gas into the sealed autoclave, repeat nitrogen gas three times, and then inject sulfur dioxide with a purity of 99.0% into the autoclave, and the pressure of sulfur dioxide is 0.3MPa;

[0031] (3) After the feeding is completed, close the inlet and outlet valves, set the speed at 280 r / min, the temperature at 60°C, and the reaction time at 8 hours;

[0032] (4) Dissolve the obtained product in chloroform, add hydrochloric acid methanol mixture (volume ratio, methanol / hydrochloric acid = 6) for precipitation, obtain an amber precipitate after filtration, wash with methanol for 3 times, and place the washed precipitate in a vacuum In a drying oven, vacuum-dry at room temperature for 12 hours to obtain a copolymer of sulfur dioxide and epoxy compound. Its number-average molecular weight measured by gel permeation chromatography is 4400g / mol, ...

Embodiment 3

[0034] (1) Add 20mL of epoxycyclohexane and 59.3mg of SalenCo into a 50ml autoclave Ⅱ Cl catalyst;

[0035] (2) Introduce 99.0% nitrogen into the sealed autoclave, repeat nitrogen 3 times, then inject sulfur dioxide with a purity of 99.0% into the autoclave, the pressure of sulfur dioxide is 0.2MPa;

[0036] (3) After the feeding is completed, close the inlet and outlet valves, set the speed at 280 r / min, the temperature at 70°C, and the reaction time at 10 hours;

[0037] (4) Dissolve the obtained product in chloroform, add hydrochloric acid methanol mixture (volume ratio, methanol / hydrochloric acid = 6) for precipitation, obtain an amber precipitate after filtration, wash with methanol 4 times, and place the washed precipitate in a vacuum In a drying oven, vacuum dry at room temperature for 24 hours to obtain a copolymer of sulfur dioxide and epoxy compound. The number-average molecular weight determined by gel permeation chromatography was 5850 g / mol, and the yield was 8....

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Abstract

The invention discloses a preparation method of a copolymer of sulfur dioxide and epoxy compounds; a novel polysulfone material is prepared by using SalenMX to catalyze the copolymerization of sulfur dioxide and epoxy compounds, adding epoxy compounds and SalenMX into a high-pressure reactor in sequence, and then injecting sulfur dioxide into the React at 50~100°C, react for 8~48 hours to obtain the product, namely sulfur dioxide and epoxy compound copolymer, dissolve the product in chloroform and precipitate with hydrochloric acid methanol mixture, filter the amber precipitate and wash it repeatedly with methanol for 2~4 times , the washed product is moved to a vacuum drying oven for 8 to 24 hours at room temperature and vacuum-dried to obtain a copolymer of sulfur dioxide and epoxy compounds with higher tacticity; the preparation method involved in the present invention is simple, the catalyst consumption is small, and the reaction The temperature is mild, the yield is high, the structure of the product is good, the cost is low, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a polymer material preparation technology, in particular to a preparation method of a copolymer of sulfur dioxide and epoxy compound. Background technique [0002] Polysulfone is a white or amber granular object, and a series of polysulfone resins with unique structures can be obtained by copolymerization of sulfur dioxide and organic matter. Polysulfone plays a huge role in medical treatment, sanitation, chiral resolution, chiral catalysis and other fields, and has broad application prospects. Especially in organisms in nature, the unique asymmetric structure of chiral polymers plays a decisive role in maintaining life processes, metabolism, species reproduction, evolution, etc. The asymmetric copolymerization of sulfur dioxide and organic matter to form chiral polysulfone has better chiral characteristics, biocompatibility and tissue compatibility that match the characteristics of life, so it can be better used in the fields...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/20
Inventor 贾庆明支云飞陕绍云刘鑫伍水生
Owner KUNMING UNIV OF SCI & TECH
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