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Preparation method of sulfur dioxide, carbon dioxide and epoxide copolymer

An epoxy compound and carbon dioxide technology, which is applied in the field of thermoplastic and degradable polymer polymer material preparation, can solve the problems of never seen ternary copolymerization of carbon dioxide and epoxy compound, harsh preparation conditions, complicated preparation process, etc., and achieve product structure. The effect of good regularity, simple preparation method and less catalyst dosage

Active Publication Date: 2016-01-06
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Similarly, some people use zinc-based catalysts to catalyze the copolymerization of sulfur dioxide and propylene oxide. Although the catalyst has high activity, good catalytic effect, and the molecular weight of the obtained product is large, because the zinc-based catalyst is very sensitive to water, it is not easy to preserve, the preparation process is complicated, and the preparation conditions very harsh
[0004] The aliphatic polycarbonate obtained by the copolymerization of carbon dioxide and epoxy compound has good mechanical properties and biodegradability, so it has a wide range of applications as a polymer material. Traditionally, aliphatic polycarbonate is synthesized by phosgene method, but Raw materials are expensive and difficult to operate
[0005] At present, there are many related reports on the copolymerization of sulfur dioxide or carbon dioxide and epoxy compounds, and the technology of SalenXM catalytic copolymerization of carbon dioxide and epoxy compounds is relatively mature, but there is still no use of SalenXM to catalyze the terpolymerization of sulfur dioxide, carbon dioxide and epoxy compounds. related reports

Method used

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  • Preparation method of sulfur dioxide, carbon dioxide and epoxide copolymer
  • Preparation method of sulfur dioxide, carbon dioxide and epoxide copolymer
  • Preparation method of sulfur dioxide, carbon dioxide and epoxide copolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) Add 20mL of epoxycyclohexane and 118.6mg of SalenCr into a 50ml autoclave Ⅲ Cl catalyst and 59.3 mgPPNCl;

[0026] (2) Introduce 99.0% nitrogen gas into the sealed autoclave, repeat nitrogen gas twice, and then in turn introduce sulfur dioxide with a purity of 99.0% and carbon dioxide with a purity of 99.0%, sulfur dioxide and carbon dioxide into the autoclave The molar ratio is 1:4;

[0027] (3) When the pressure reaches 0.5MPa, close the inlet and outlet valves of the high-pressure reactor, set the speed at 280r / min, the temperature at 50°C, and the reaction time at 6h;

[0028] (4) Use chloroform to dissolve the product obtained after the reaction, add hydrochloric acid methanol solution (volume ratio, methanol / hydrochloric acid = 6) for precipitation, obtain an amber precipitate after filtration, wash with methanol 3 times, and place the washed precipitate In a vacuum drying oven, vacuum-dry at room temperature for 8 hours to obtain a terpolymer of sulfur diox...

Embodiment 2

[0030] (1) Add 30mL of epoxycyclohexane and 177.9mg of SalenCr to a 50ml autoclave Ⅲ Cl catalyst and 44.5 mgPPNCl;

[0031] (2) Introduce 99.0% nitrogen gas into the sealed autoclave, repeat nitrogen gas three times, and then in turn into the autoclave with 99.0% purity of sulfur dioxide and 99.0% carbon dioxide, the mole of sulfur dioxide and carbon dioxide The ratio is 1:4;

[0032] (3) When the pressure reaches 1MPa, close the inlet and outlet valves of the high-pressure reactor, set the speed at 280r / min, the temperature at 60°C, and the reaction time at 8h;

[0033] (4) Use chloroform to dissolve the product obtained after the reaction, add hydrochloric acid methanol solution (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 drying oven, vacuum-dry at room temperature for 12 hours to obtain a terpolymer of sulfur dioxide, carbon dioxide ...

Embodiment 3

[0035] (1) Add 20mL of epoxycyclohexane and 59.3mg of SalenCr into a 50ml autoclave Ⅲ Cl catalyst and 29.7 mgPPNCl;

[0036] (2) Introduce 99.0% nitrogen gas into the sealed autoclave, repeat nitrogen gas three times, and then in turn into the autoclave with 99.0% purity of sulfur dioxide and 99.0% carbon dioxide, the mole of sulfur dioxide and carbon dioxide The ratio is 1:4;

[0037](3) When the pressure reaches 2MPa, close the inlet and outlet valves of the high-pressure reactor, set the speed at 280r / min, the temperature at 70°C, and the reaction time at 10h;

[0038] (4) Use chloroform to dissolve the product obtained after the reaction, add hydrochloric acid methanol solution (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 drying oven, vacuum dry at room temperature for 24 hours to obtain a terpolymer of sulfur dioxide, carbon dioxide...

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Abstract

The invention discloses a preparation method of a sulfur dioxide, carbon dioxide and epoxide copolymer. According to the method, epoxide, SalenCr<III>Cl and PPNCl are sequentially added to a high-pressure reaction kettle, sulfur dioxide and carbon dioxide are introduced and have a reaction at the temperature of 50-100 DEG C for 8-48 h, then, a product is dissolved with chloroform, a hydrochloric acid and methanol solution is used for precipitation, amber precipitates are filtered and repeatedly washed with methanol, the washed product is dried in vacuum at the room temperature, and the sulfur dioxide, carbon dioxide and epoxide terpolymer with higher stereoregularity can be obtained. The sulfur dioxide, carbon dioxide and epoxide terpolymer has structural characteristics of polycarbonate and polysulfone and has a wide application prospect in the fields of packaging, filtration and the like; 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 present invention relates to the preparation technology of thermoplastic and degradable polymer polymer material, specifically a kind of using SalenCr Ⅲ Cl simultaneously catalyzes the method of ternary copolymerization of sulfur dioxide, carbon dioxide and epoxy compound. Background technique [0002] Since 1934, it has been discovered that sulfur dioxide can be copolymerized with olefins under the action of an initiator. Due to the activity of sulfur dioxide itself and the instability of the carbon-carbon double bond of olefins, this reaction is easy to occur, and the polysulfone obtained by this free radical polymerization can have zwitterions at the same time after modification. At present, there are seawater desalination abroad. The factory uses modified polysulfone as scale inhibitor. Sulfur dioxide in such as Et 2 Zn, SnCl 4 or SbCl 5 The copolymerization reaction with epoxy compounds can occur under the catalysis of Lewis acid, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/20C08G64/34C08G64/40
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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