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Natural polysaccharide-grafted polycaprolactone in ionic liquid as well as preparation method and application thereof

A technology of natural polysaccharides and ionic liquids, applied in the field of biodegradable materials, can solve the problems of less research on the dissolution of konjac glucomannan and polysaccharide nanocrystals, and no research on the chemical modification of polysaccharide nanocrystals, so as to improve humidity Very sensitive, easy to degrade mechanical properties, good film-forming effect

Inactive Publication Date: 2013-04-24
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, the research on ionic liquids has developed rapidly. The research on the use of room temperature ionic liquids as green reaction solvents in the field of polymers is a research hotspot at home and abroad. However, for konjac glucomannan and polysaccharide nanocrystals There are still relatively few studies on dissolution in liquids, especially for the chemical modification of polysaccharide nanocrystals in ionic liquids.

Method used

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  • Natural polysaccharide-grafted polycaprolactone in ionic liquid as well as preparation method and application thereof
  • Natural polysaccharide-grafted polycaprolactone in ionic liquid as well as preparation method and application thereof
  • Natural polysaccharide-grafted polycaprolactone in ionic liquid as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Can be used in the preparation method of konjac glucomannan grafted polycaprolactone in ionic liquid chlorinated 1-butyl-3-methylimidazole [BMIM]Cl, it comprises the following steps:

[0031] 1) Pretreatment of raw materials: konjac glucomannan, vacuum-dried at 40°C for 12 h; caprolactone monomer (ε-CL), distilled under reduced pressure to remove water;

[0032] 2) Dissolution of konjac glucomannan: under nitrogen atmosphere, first melt the ionic liquid at 70 °C, and then add konjac glucomannan according to the mass ratio of konjac glucomannan and ionic liquid [BMIM]Cl at 1:15 For polysaccharides, magnetically stir for 3-5 hours;

[0033] 3) Konjac glucomannan grafted polycaprolactone in ionic liquid: under nitrogen atmosphere, slowly add caprolactone monomer dropwise at a mass ratio of konjac glucomannan to caprolactone monomer of 1:5 At the same time, the catalyst stannous octoate [Sn(Oct) 2 ], magnetically stirred, and reacted for 12 hours under temperature control...

Embodiment 2

[0036] Can be used in the preparation method of konjac glucomannan graft polycaprolactone in ionic liquid [BMIM]Cl, it comprises the following steps:

[0037] 1) Pretreatment of raw materials: konjac glucomannan, vacuum-dried at 40°C for 12 h; caprolactone monomer (ε-CL), distilled under reduced pressure to remove water;

[0038] 2) Dissolution of konjac glucomannan: under nitrogen atmosphere, first melt the ionic liquid at 70 °C, and then add konjac glucomannan according to the mass ratio of konjac glucomannan and ionic liquid [BMIM]Cl at 1:15 For polysaccharides, magnetically stir for 3-5 hours;

[0039]3) Konjac glucomannan grafted polycaprolactone in ionic liquid: under nitrogen atmosphere, slowly add caprolactone monomer dropwise at a mass ratio of konjac glucomannan to caprolactone monomer of 1:20 At the same time, the catalyst stannous octoate [Sn(Oct) 2 ], magnetically stirred, and reacted for 18 hours under temperature control at 80°C;

[0040] 4) Purification of t...

Embodiment 3

[0042] Can be used in the preparation method of konjac glucomannan graft polycaprolactone in ionic liquid [BMIM]Cl, it comprises the following steps:

[0043] 1) Pretreatment of raw materials: konjac glucomannan, vacuum-dried at 40°C for 12 h; caprolactone monomer (ε-CL), distilled under reduced pressure to remove water;

[0044] 2) Dissolution of konjac glucomannan: under a nitrogen atmosphere, first melt the ionic liquid at 70 °C, and then add konjac glucomannan according to the mass ratio of konjac glucomannan and ionic liquid [BMIM]Cl at 1:30 For polysaccharides, magnetically stir for 3-5 hours;

[0045] 3) Konjac glucomannan grafted polycaprolactone in ionic liquid: under nitrogen atmosphere, slowly add caprolactone monomer dropwise at a mass ratio of konjac glucomannan to caprolactone monomer of 1:30 At the same time, the catalyst stannous octoate [Sn(Oct) 2 ], magnetically stirred, and reacted for 24 hours under temperature control at 115°C;

[0046] 4) Purification ...

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Abstract

The invention relates to a preparation method of natural polysaccharide-grafted polycaprolactone in ionic liquid. The preparation method comprises the following steps of: (1) carrying out pretreatment on a raw material; (2) dissolving natural polysaccharide in ionic liquid; (3) grafting the natural polysaccharide in the ionic liquid with polycaprolactone: in a nitrogen atmosphere, slowly dropping a caprolactone monomer and rapidly adding a catalyst, magnetically stirring, controlling temperature at 70-115 DEG C and reacting for 12-24hours; and (4) precipitating by ethanol to obtain a crude product, adding methylene dichloride, magnetically stirring for 72hours, filtering, washing and drying to obtain the final product: natural polysaccharide-grafted polycaprolactone. The preparation method disclosed by the invention is green and environment-friendly, low in cost, and simple and efficient in process; and the obtained material can be completely biodegraded and directly processed and shaped or used as a cosolvent of other blending materials.

Description

technical field [0001] The invention relates to a natural polysaccharide grafted polycaprolactone in an ionic liquid and a preparation method and application thereof, belonging to the field of biodegradable materials. Background technique [0002] Konjac glucomannan, a characteristic resource in my country, has a wide range of sources and low cost. It has excellent hydrophilicity, gelling, thickening, viscosity, stability, reversible suspension, film-forming and flavoring properties, etc. A variety of unique physical and chemical properties, and specific biological activities, have a wide range of application and development value, especially its excellent film-forming properties have attracted attention at home and abroad. Cellulose, as the most abundant natural polymer in the world, has been widely used in people's daily life and has great research significance and value. This kind of natural polysaccharide is a renewable resource, which has the advantages of biodegradabil...

Claims

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Application Information

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IPC IPC(8): C08G63/664C08L67/04
Inventor 黄进黄清车圆圆周琪张荣贵阿兰·迪夫雷纳高山俊
Owner WUHAN UNIV OF TECH
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