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Method for preparing cellulose microsphere by taking ionic liquid as solvent

A technology of cellulose microspheres and ionic liquids, applied in the fields of microsphere preparation, chemical instruments and methods, microcapsule preparations, etc., can solve the problem of high difficulty, and achieve the effects of less environmental pollution, good thermal stability and good sphericity

Inactive Publication Date: 2009-12-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of cellulose microspheres by ionic liquid dissolution method is quite difficult, and some key process problems have yet to be solved, so there are no relevant literature reports

Method used

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  • Method for preparing cellulose microsphere by taking ionic liquid as solvent
  • Method for preparing cellulose microsphere by taking ionic liquid as solvent

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 500ml flask, add 38.6 g of 1-butyl-3-methyl-imidazolium chloride (BMINCl), add 1.4 g of refined cotton with a molecular weight of 190,000 Daltons, and stir at 105°C for 20 minutes to form a total weight of 40.0 g of cellulose solution. The temperature was lowered to 100°C, kept stirring, 12.0 g of tungsten carbide powder was added, and the mixture was stirred evenly. 200ml of vacuum pump oil and 4g of Tween 80 were added, the temperature was kept at 100°C, the rotational speed was adjusted to 500rpm, and the temperature was lowered after maintaining stirring for 20 minutes. The temperature was lowered to 40° C. within 120 minutes, 100 ml of absolute ethanol was added, the rotational speed was adjusted to 200 rpm, and the stirring was maintained for 20 minutes to solidify to obtain cellulose / tungsten carbide composite microspheres. The microspheres were filtered from the reaction liquid and washed three times with deionized water. Wet sieving, deionized water wash...

Embodiment 2

[0023] In a 500ml flask, add 38.8 g of 1-butyl-3-methyl-imidazolium chloride (BMINCl), add 1.2 g of refined cotton with a molecular weight of 190,000 Daltons, and stir at 110°C for 20 minutes to form a total weight of 40.0 g of cellulose solution. The temperature was lowered to 100°C, kept stirring, 10.0 g of tungsten carbide powder was added, and the mixture was stirred evenly. 200ml of vacuum pump oil and 2g of Tween 80 were added, the temperature was 95°C, the rotational speed was adjusted to 650rpm, and the temperature was started after maintaining stirring for 20 minutes. The temperature was lowered to 35° C. within 120 minutes, 120 ml of absolute ethanol was added, the rotational speed was adjusted to 200 rpm, and the stirring was maintained for 20 minutes to solidify to obtain cellulose / tungsten carbide composite microspheres. The microspheres were filtered from the reaction liquid and washed three times with deionized water. Wet sieving, deionized water washing and s...

Embodiment 3

[0025]Add 38.8 grams of 1-butyl-3-methyl-imidazolium chloride (BMINCl) in a 500ml flask, add 1.2 grams of refined cotton with a molecular weight of 190,000 Daltons, stir at 90°C for 30 minutes, and form a total weight of 40.0 grams of cellulose solution. Keep the temperature at 90°C, keep stirring, add 10.0 grams of tungsten carbide powder, and stir evenly. Add 160ml of vacuum pump oil and 4g of Tween 80, drop the temperature to 85°C, adjust the rotation speed to 700rpm, keep stirring for 20 minutes, and then start to drop the temperature. Reduce the temperature to 30°C within 110 minutes, add 100ml of acetone, adjust the rotation speed to 200rpm, keep stirring for 20 minutes, and solidify to obtain cellulose / tungsten carbide composite microspheres. The microspheres were filtered from the reaction liquid and washed three times with deionized water. Wet sieving, washing and soaking in deionized water, obtained 11.3ml of cellulose microspheres with a particle size of 74-300μm ...

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Abstract

The invention discloses a method for preparing cellulose microspheres by taking ionic liquid as a solvent. The method comprises the steps of: 1) preparing cellulose solution as follows: dissolving the cellulose into the ionic liquid under low-speed stirring and proper temperature; 2) adding inert particles: adding proper amount of inert particles, and stirring evenly; 3) forming spheres by reversed phase suspension: adding oil phase and a surface active agent, leading the cellulose solution to be condensed into spheres by reversed phase suspension and program temperature reduction; 4) curving microspheres: adding a curving agent and curving to form the cellulose microspheres; 5) washing: using deionized water to wash and soak so as to obtain the cellulose microspheres; and 6) screening: screening in a wet state and obtaining the cellulose microspheres with a certain particle size range. The developed preparation process is simple and convenient, the used solvent is safe and non-toxic, the prepared cellulose micrsphere has porous structure and proper particle size, high sphericity and good hydropathy, can adjust density, can be used as substrate of an absorbent and has good biocompatibility.

Description

technical field [0001] The invention relates to a method for preparing cellulose microspheres by using ionic liquid as a solvent. Background technique [0002] Cellulose is the most abundant renewable resource in nature and a natural polysaccharide molecule. Cellulose microspheres have high hydrophilicity, good biocompatibility, suitable porous structure, extremely low non-specific adsorption and high mechanical strength, and are a good adsorbent matrix material, which can be used in bioengineering In the downstream separation and purification process of the product, it can also be used as a carrier material for enzyme immobilization. Due to the strong hydrogen bonding between natural cellulose molecules, a very dense structure is formed, which causes difficulties in the processing of cellulose materials, especially the preparation of cellulose porous microspheres. At present, the vast majority of chromatographic media for biological separation are prepared from agarose or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02B01J20/285B01J20/28B01J20/30
Inventor 林东强施霏姚善泾杜悦娴
Owner ZHEJIANG UNIV
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