Surface silanization regenerated cellulose microsphere filling and preparation method and use thereof

A technology of regenerated cellulose and microsphere fillers, which is applied in the fields of chromatography and polymer chemistry, can solve the problems of expensive cellulose solvent system, abnormal chromatographic behavior, complicated preparation process, etc., and achieves high alkali resistance, simple process, low cost effect

Inactive Publication Date: 2006-06-21
WUHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of these methods are that the cellulose solvent system is more expensive or pollutes the environment, or the scope of application is narrow, such as not being able to be used in strong alkaline conditions, or the filler is irregular spherical and the particle size is large so that the filled color The performance of the ordinary column is reduced, or the filler adsorbs the graded polymer, which leads to abnormal chromatographic behavior, etc.
In addition, cellulose derivative gel (J.Chromatogr.A, 919, 29, 2001), cellulose derivative microspheres (J.Chromatogr.A, 552, 389, 1991; Journal of Sichuan University (Engineering Science Edition), 32, 48, 2000), cellulose-coated inorganic fillers (J.Chromatogr.A, 904, 17, 2000; J.Chromatogr.Sci., 40, 315, 2002) are also used in gel permeation chromatography column fillers, However, its preparation process is complex and unstable, which limits its application in separation, fractionation and purification of macromolecular substances

Method used

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  • Surface silanization regenerated cellulose microsphere filling and preparation method and use thereof
  • Surface silanization regenerated cellulose microsphere filling and preparation method and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Mix 3% cellulose and 2% konjac glucomannan NaOH / thiourea aqueous solution according to the ratio of cellulose: konjac glucomannan is 6:4 and defoam, take 40 grams and put it into a 250mL three-port bottle, add 40 mL of 2% Span80 liquid paraffin solution into the system, stir at 200 rpm for 2 hours, and then add 5% CaCl 2 50 mL of aqueous solution was stirred for 1 hour, and then 100 mL of 2% aqueous HCl was added and stirred for half an hour. Stirring was stopped, filtered, and the obtained solid was washed with acetone, absolute ethanol and distilled water, and the product was lyophilized. Take 4 grams of the dried above product and put it into a 100 mL three-necked flask, add 30 mL of N,N dimethylacetamide and 10 mL of pyridine, blow nitrogen at 20°C and stir at a speed of 100 rpm for 1 hour, then add 4 grams of Chlorotrimethylsilane, stirred for 2 hours. The resulting product is filtered with toluene, washed with acetone and absolute ethanol to obtain the desired f...

Embodiment 2

[0017] 4% cellulose and 2% konjac glucomannan NaOH / thiourea aqueous solution are mixed by cellulose: konjac glucomannan is a ratio of 7:3 and defoamed, and 40 grams are put into 250mL three mouthfuls bottle, add 50 mL of 4% Span80 liquid paraffin solution into the system, stir at 200 rpm for 1 hour, and then add 5% CaCl 2 80 mL of aqueous solution was stirred for 1 hour, and then 80 mL of 5% aqueous HCl was added and stirred for half an hour. Stirring was stopped, filtered, and the resulting solid was washed with acetone, absolute ethanol and distilled water, and the product was freeze-dried. Take 4 grams of dried product and put it into a 100mL three-necked flask, add 30mL N, N dimethylacetamide and 10mL pyridine, blow nitrogen at 40C and stir at a speed of 100 rpm for 1 hour, then add 8 grams of triethyl Chlorosilane, stirred for 2 hours. The resulting product is filtered with toluene, acetone and absolute ethanol to wash the desired filler, its particle size is 30 to 50 μ...

Embodiment 3

[0018] Example 3: The surface silanized regenerated cellulose microsphere filler prepared in Example 1 was packed into a glass tube of 550×20 mm to form a gel bed of 500×20 mm, thereby preparing a preparative gel permeation chromatography column. The theoretical pedal number of this preparative gel permeation chromatography column is 2730. The column is used to fractionate the weight average molecular weight M w 8.31×10 4 , a tetrahydrofuran solution of polycaprolactone with a dispersion index d of 1.55, the mobile phase is tetrahydrofuran, and the flow rate is 1.2 mL min-1. This polymkeric substance is divided into 6 fractions, obtains the fraction product of different molecular weight, and its molecular weight is respectively 18.4 * 10 4 , 13.4×10 4 , 11.0×10 4 , 8.48×10 4 , 6.10×10 4 and 1.17×10 4 , and the dispersion index is 1.2. The weight of each fraction accounts for 10-15% of the injection volume, and the total yield reaches 96.2%. It is indicated that the su...

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Abstract

The invention relates to a surface silanized regenerated cellulose microsphere filler, which is composed of 48-90 wt% cellulose, 9-50 wt% konjac glucomannan and 0.5-4 wt% silane. Mix 4-6% cellulose NaOH / thiourea aqueous solution and 2-4% konjac glucomannan NaOH / thiourea aqueous solution evenly and defoam to obtain a mixed solution, then add Span80 liquid paraffin solution to the above mixed solution , stir, and then add 1 to 10 wt% of CaCl 2 Stir the aqueous solution, and finally add HCl aqueous solution, filter, and wash to obtain microspheres. After the obtained microspheres are freeze-dried, use N,N-dimethylacetamide as the medium, add catalyst pyridine, add chlorosilane at 20-100°C and stir After 3-5 hours, filter and wash to obtain regenerated cellulose microsphere filler microspheres with a particle diameter of 30-100 μm. The microsphere filler prepared by the invention has small particle size, high alkali resistance, low adsorption to biomacromolecules, and high efficiency of the filled chromatographic column.

Description

technical field [0001] The invention relates to a surface silanized regenerated cellulose microsphere filler, a preparation method and application thereof. It belongs to the technical field of polymer chemistry and also belongs to the technical field of chromatography. Background technique [0002] Cellulose and konjac glucomannan are rich natural polymers and are environmentally friendly materials; moreover, because they contain rich hydroxyl groups, they can be derivatized to prepare many functional materials; therefore, their research and development are increasingly attractive Attention, especially the development of high value-added products has become a research hotspot in the past ten years. On the other hand, separation, fractionation or purification of biomacromolecules or synthetic polymers using preparative gel permeation chromatography columns is of great importance in both industry and research. However, since the commonly used chromatographic column fillers a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60C08L1/02
Inventor 张俐娜熊晓鹏
Owner WUHAN UNIV
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