Preparation method of sulfur dioxide and epoxide copolymer

A technology of epoxy compounds and sulfur dioxide, which is applied in the field of polymer material preparation, can solve the problems of harsh reaction conditions, low catalytic activity, and low molecular weight of copolymers, and achieve less catalyst consumption, shorter reaction time, and simple preparation methods Effect

Active Publication Date: 2016-01-06
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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  • Preparation method of sulfur dioxide and epoxide copolymer
  • Preparation method of sulfur dioxide and epoxide copolymer
  • Preparation method of sulfur dioxide and epoxide 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) Close the inlet and outlet valves after feeding, set the speed to 280r / min, the temperature to 50°C, and the reaction time to 6h;

[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 / mol, and the yield was 5.6...

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) Close the inlet and outlet valves after the feeding is completed, set the speed at 280r / min, the temperature at 60°C, and the reaction time at 8h;

[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, and the...

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) Close the inlet and outlet valves after feeding, set the speed to 280r / min, the temperature to 70°C, and the reaction time to 10h;

[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 8.35%.

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Abstract

The invention discloses a preparation method of a sulfur dioxide and epoxide copolymer. According to the method, a novel polysulfone material is prepared through copolymerization of sulfur dioxide and epoxide under the catalytic action of SalenMX, epoxide and SalenMX are sequentially added to a high-pressure reaction kettle, sulfur dioxide is introduced and has a reaction at the temperature of 50-100 DEG C for 8-48 h, then, a product, namely, the sulfur dioxide and epoxide copolymer is obtained, the product is dissolved with chloroform, a hydrochloric acid and methanol mixed solution is used for precipitation, amber precipitates are filtered and repeatedly washed with methanol for 2-4 times, the washed product is transferred to a vacuum drying box and dried in vacuum at the room temperature for 8-24 h, and the sulfur dioxide and epoxide copolymer with higher stereoregularity can be obtained. The preparation method is simple, few catalysts are used, the reaction temperature is mild, the yield is high, the structure regularity 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 Applications(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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