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High-strength polysaccharide aerogel microsphere, and preparation method and application thereof

A technology of gel microspheres and polysaccharides, which is applied in the direction of microsphere preparation, microcapsule preparation, chemical instruments and methods, etc., and can solve problems such as no pressure resistance and low medium flow rate

Active Publication Date: 2014-05-07
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the purposes of the present invention is to provide a polysaccharide gel microsphere, specifically, one of the purposes of the present invention is to provide a high-strength polysaccharide gel microsphere that can be used as a chromatographic separation filler, the Gel microspheres solve the problems of low flow rate and pressure resistance of existing polysaccharide soft gel media

Method used

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  • High-strength polysaccharide aerogel microsphere, and preparation method and application thereof
  • High-strength polysaccharide aerogel microsphere, and preparation method and application thereof
  • High-strength polysaccharide aerogel microsphere, and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0067] Example 1 Blending method to prepare high-strength agarose microspheres with a concentration of 4wt%

[0068] (1) Modification of agarose raw material

[0069] Weigh 4g of agarose powder, add 40mL of water, heat and dissolve to obtain a 10% agarose solution, cool down to about 65°C, slowly add 0.5mL of 40% NaOH solution and bifunctional cross-linking agent allyl glycidyl ether to it 6mL. Among them, the concentration of allyl glycidyl ether in the water phase is 15%, OH - The concentration is 0.21mol / L. After stirring and reacting at 65° C. for 8 h, the reaction was terminated by adjusting the pH value to 7-8 with 60% glacial acetic acid solution, and an allylated agarose solution was obtained. Add 4 times the volume of ethanol to the solution, centrifuge to collect the precipitate, pre-freeze at -70°C for 2 hours, and freeze-dry for 72 hours to obtain the modified agarose raw material.

[0070] (2) Preparation of agarose microspheres modified by cross-linking agent...

Embodiment 2

[0076] Example 2 Blending method to prepare high-strength agarose microspheres with a concentration of 4wt%

[0077] In order to further increase the strength of the agarose gel microspheres, on the basis of the cross-linking process described in Example 1, the traditional method was used to continue cross-linking once. That is, take 20 g of cross-linked agarose microspheres obtained in step (3) of Example 1, disperse them in 40 mL of deionized water, and gradually raise the temperature to 47.5° C. for 2 hours. After that, 1.6 mL of epichlorohydrin and 2.4 mL of 40% NaOH solution (containing 3% NaBH 4 ), and continued to react for 12h in a constant temperature water bath shaker. After the cross-linking was completed, it was washed with water until neutral, and the obtained 4wt% highly cross-linked agarose microspheres had an average particle size of 86.41 μm and a maximum flow rate of 2980 cm / h in the linear range. The pressure flow rate curve is as figure 2 shown.

Embodiment 3

[0087] Example 3 Blending method to prepare high-strength agarose microspheres with a concentration of 6wt%

[0088] (1) Modification of agarose raw material

[0089] Prepare 40 mL of agarose solution with a concentration of 18%, cool down to about 80 °C, and slowly add 3 mL of 40% NaOH solution and 8 mL of cross-linking agent allyl glycidyl ether into it. Among them, the concentration of allyl glycidyl ether in the aqueous phase is 20%, OH - The concentration is 1.25mol / L. After stirring and reacting at 80° C. for 3 h, the reaction was terminated by adjusting the pH value to 7-8 with 60% glacial acetic acid solution, and an allylated agarose solution was obtained. Add 4 times the volume of ethanol to the solution, centrifuge to collect the precipitate, pre-freeze at -70°C for 2 hours, and freeze-dry for 72 hours to obtain the modified agarose raw material.

[0090] (2) Preparation of agarose microspheres modified by cross-linking agent by blending

[0091] Accurately weig...

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Abstract

The invention discloses a high-strength polysaccharide aerogel microsphere, and a preparation method of the high-strength polysaccharide aerogel microsphere, which are mainly used in the field of chromatographic separation. According to the preparation method, firstly a difunctional cross-linking agent is used to modify a polysaccharide material, then the polysaccharide material is mixed with a material not modified, and the mixture is emulsified into a sphere, and activated at the later stage to achieve crosslinking in the microsphere. The modified polysaccharide chain forms a covalent cross-linking bond in an aerogel fiber bundle and between the aerogel fiber bundles, so that the mechanical strength of the aerogel microsphere is greatly improved; the polysaccharide chain not modified contains a large quantity of hydroxide radicals so as to be good for the formation of a hydrogen bond in the gelation process and play a role of skeleton supporting, then a macropore network structure formed through aerogel solidification is kept, and the shrinkage and the deformation of the microsphere are effectively avoided. The aerogel microsphere not only has an excellent property of the natural polysaccharide, but also has a remarkable advantage on the skeleton rigidity and operation flow rate, and is therefore an ideal industrial chromatographic separation filler.

Description

technical field [0001] The invention belongs to the field of chromatographic separation materials, and relates to a high-strength polysaccharide gel microsphere, a preparation method and an application thereof. Background technique [0002] Natural polysaccharides are rich in hydroxyl groups, highly hydrophilic, and have good compatibility with biomacromolecules, occupying a core position in the field of biomacromolecules separation. Especially the gel-type polysaccharide separation medium, which has a macroporous network structure in the swollen state, has special advantages for the separation and purification of biological macromolecules. However, the skeleton structure of polysaccharide gel is mainly maintained by hydrogen bonds. Although it has certain mechanical strength, compared with inorganic microspheres and other organic polymer microspheres, the particles are relatively soft, so it is called "soft matrix". When used as a separation medium, under high pressure, th...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/28B01J20/30B01J13/14B01J13/02C08J3/24C08L5/00
Inventor 马光辉赵希吴颉崔金梅周炜清苏志国
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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