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A kind of high-strength polysaccharide gel microsphere, preparation method and application thereof

A gel microsphere, high-strength technology, applied in the direction of microsphere preparation, microcapsule preparation, chemical instruments and methods, etc., can solve the problems of low medium flow rate and pressure resistance

Active Publication Date: 2016-07-13
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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  • A kind of high-strength polysaccharide gel microsphere, preparation method and application thereof
  • A kind of high-strength polysaccharide gel microsphere, preparation method and application thereof
  • A kind of high-strength polysaccharide gel microsphere, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0067] Example 1 Preparation of 4wt% high-strength agarose microspheres by blending method

[0068] (1) Modification of agarose raw materials

[0069] Weigh 4g of agarose powder, add 40mL of water, heat to dissolve, get a 10% agarose solution, cool to about 65℃, slowly add 0.5mL of 40% NaOH solution and bifunctional crosslinker 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 hours, the reaction was terminated by adjusting the pH value of 7-8 with 60% glacial acetic acid solution, and an allylated agarose solution was obtained. 4 times the volume of ethanol was added to the solution, the precipitate was collected by centrifugation, pre-frozen at -70°C for 2 hours, and freeze-dried for 72 hours to obtain modified agarose raw material.

[0070] (2) Blending to prepare agarose microspheres modified with crosslinker

[0071] Accurately weigh 1.2...

Embodiment 2

[0076] Example 2 Preparation of 4wt% high-strength agarose microspheres by blending method

[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 is used to continue cross-linking once. That is, take 20 g of cross-linked agarose microspheres obtained in step (3) of Example 1 and disperse in 40 mL of deionized water, and gradually increase the temperature to 47.5° C. for 2 h. Then, slowly add 1.6mL epichlorohydrin and 2.4mL 40% NaOH solution (containing 3% NaBH 4 ), continue to react for 12h in a constant temperature water bath shaker. After the cross-linking is completed, wash with water to neutrality. The average particle size of the 4wt% highly cross-linked agarose microspheres obtained is 86.41μm, and the maximum flow rate in the linear range is 2980cm / h. The pressure flow rate curve is like figure 2 Shown.

Embodiment 3

[0087] Example 3 Preparation of 6wt% high-strength agarose microspheres by blending method

[0088] (1) Modification of agarose raw materials

[0089] Prepare 40 mL agarose solution with a concentration of 18%, cool to about 80°C, and slowly add 3 mL of 40% NaOH solution and 8 mL of crosslinker allyl glycidyl ether to it. Among them, the concentration of allyl glycidyl ether in the water phase is 20%, OH - The concentration is 1.25mol / L. After stirring and reacting at 80℃ for 3h, 60% glacial acetic acid solution was used to adjust the pH value of 7-8 to terminate the reaction, and an allylated agarose solution was obtained. 4 times the volume of ethanol was added to the solution, the precipitate was collected by centrifugation, pre-frozen at -70°C for 2 hours, and freeze-dried for 72 hours to obtain modified agarose raw material.

[0090] (2) Blending to prepare agarose microspheres modified with crosslinker

[0091] Accurately weigh 3.24g of modified agarose raw material (90% of th...

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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 application thereof. Background technique [0002] Natural polysaccharides are rich in hydroxyl groups, have strong hydrophilicity, have good compatibility with biological macromolecules, and occupy a core position in the field of biological macromolecule separation. In particular, the gel-like polysaccharide separation medium has a macroporous network structure in the swollen state, which 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, the particles are relatively soft compared with inorganic microspheres and other organic polymer microspheres, so they are called "soft matrix". When used as a separation medium, this t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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