Citric acid-modified cyclodextrin crosslinking chitosan porous adsorption material, and preparation and application of same

A technology of porous adsorption material and cross-linked chitosan, which can be used in adsorption water/sewage treatment, other chemical processes, chemical instruments and methods, etc. It can solve the problem of low grafting rate, increase water solubility and reduce crystallinity , the effect of improving chemical stability

Inactive Publication Date: 2017-08-29
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN 103992501 discloses a preparation method of citric acid grafted chitosan hydrogel, reacting citric acid with chitosan ethanol suspensi

Method used

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  • Citric acid-modified cyclodextrin crosslinking chitosan porous adsorption material, and preparation and application of same
  • Citric acid-modified cyclodextrin crosslinking chitosan porous adsorption material, and preparation and application of same
  • Citric acid-modified cyclodextrin crosslinking chitosan porous adsorption material, and preparation and application of same

Examples

Experimental program
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Embodiment 1

[0045] Accurately weigh 12.6g of citric acid, and dissolve 2.52g of sodium hypophosphite in 12mL of deionized water. After complete dissolution, 11.35 g of β-cyclodextrin was added, and the temperature was raised to 80° C., the cyclodextrin was dissolved, and a non-transparent solution was obtained. It was pre-baked at 100°C for 1 hour and then baked at 120°C for 5 hours in a blast-type constant temperature drying oven. After the reaction, add 30-50mL deionized water to dissolve, then slowly add it dropwise into absolute ethanol, precipitate out, and wash repeatedly with absolute ethanol 5-6 times, then dry the precipitate at 55°C to constant weight, To obtain citric acid modified cyclodextrin (such as figure 1 , The IR of the citric acid modified cyclodextrin has an obvious carbonyl absorption peak of the ester bond at 1722cm-1, indicating that the chemical modification is successful).

[0046] Accurately weigh 0.8g of modified cyclodextrin and dissolve it in 20mL of deion...

Embodiment 2

[0048] Accurately weigh 12.6g of citric acid, and dissolve 2.52g of sodium hypophosphite in 12mL of deionized water. After complete dissolution, 11.35 g of β-cyclodextrin was added, and the temperature was raised to 80° C., the cyclodextrin was dissolved, and a non-transparent solution was obtained. It was pre-baked at 100°C for 1 hour and then baked at 120°C for 5 hours in a blast-type constant temperature drying oven. After the reaction, add 30-50mL deionized water to dissolve, then slowly add it dropwise into absolute ethanol, precipitate out, and wash repeatedly with absolute ethanol 5-6 times, then dry the precipitate at 55°C to constant weight, A citric acid modified cyclodextrin was obtained.

[0049] Accurately weigh 1.6g of modified cyclodextrin and dissolve it in 40mL of deionized water, add 2.36g of EDC and 1.41g of NHS and stir for activation at room temperature for 30min. Then add the activation solution into 213.3mL of 3%wt chitosan solution, stir rapidly for 5...

Embodiment 3

[0051] Accurately weigh 12.6g of citric acid, and dissolve 2.52g of sodium hypophosphite in 12mL of deionized water. After complete dissolution, 11.35 g of β-cyclodextrin was added, and the temperature was raised to 80° C., the cyclodextrin was dissolved, and a non-transparent solution was obtained. It was pre-baked at 100°C for 1 hour and then baked at 120°C for 5 hours in a blast-type constant temperature drying oven. After the reaction, add 30-50mL deionized water to dissolve, then slowly add it dropwise into absolute ethanol, precipitate out, and wash repeatedly with absolute ethanol 5-6 times, then dry the precipitate at 55°C to constant weight, A citric acid modified cyclodextrin was obtained.

[0052] Accurately weigh 2.4g of modified cyclodextrin and dissolve in 60mL of deionized water, add 3.54g of EDC and 2.11g of NHS and stir at room temperature for 30min to activate. Then the activation solution was added to 186.7 mL of 3% wt chitosan solution, stirred rapidly fo...

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Abstract

The invention relates to a citric acid-modified cyclodextrin crosslinking chitosan porous adsorption material, and preparation and an application of same. The preparation method includes the steps of: modifying beta-cyclodextrin with citric acid, performing amide crosslinking to a modified beta-cyclodextrin water solution with a chitosan solution under the effect of an EDC/NHS coupling agent, and freeze-drying the product to obtain the modified beta-cyclodextrin crosslinking chitosan porous adsorption material. In the invention, by means of the modified beta-cyclodextrin crosslinking chitosan, the acid resistance of chitosan is improved, and a defect that the chitosan material is liable to dissolve in an acidic solution and is difficult to recycle is overcome. In the invention, hydrogel is freeze-dried, so that chitosan-base porous materials in different shapes can be rapidly produced. The citric acid-modified cyclodextrin crosslinking chitosan porous adsorption material has excellent adsorption capability to anionic dyes; at room temperature, the material can reach 1060.41 mg/g in saturation adsorption quantity to reactive yellow BH-3RS.

Description

technical field [0001] The invention belongs to the field of porous adsorption material and its preparation and application, in particular to a citric acid modified cyclodextrin cross-linked chitosan porous adsorption material and its preparation and application. Background technique [0002] Chitosan is the only amino weakly alkaline polysaccharide in nature, which widely exists in marine crab shells and fungal cell walls. Chitosan has excellent biocompatibility, biodegradability and bioactivity, and is widely used in the fields of drug release carriers, tissue engineering scaffolds, degradable bone implant materials and tissue repair dressings. It is of great significance to further develop and apply it. The chitosan molecular chain is rich in hydroxyl groups, and the amino groups can combine with reactive dyes by hydrogen bonds, van der Waals forces and ionic bonds, and have strong adsorption capacity. However, under weakly acidic conditions, the strength of chitosan ma...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08J3/24C08J3/075C08B37/16C08L5/08C08L5/16B01J20/24C02F1/28C02F101/30
CPCB01J20/24C02F1/286C02F2101/308C08B37/0012C08J3/075C08J3/246C08J9/28C08J2305/08C08J2405/16C08L5/08C08L2205/02C08L5/16
Inventor 王碧佳邹正冬徐小梅
Owner DONGHUA UNIV
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