CN112495352A - Preparation method of chitosan-beta cyclodextrin adsorbent - Google Patents
Preparation method of chitosan-beta cyclodextrin adsorbent Download PDFInfo
- Publication number
- CN112495352A CN112495352A CN201910873410.XA CN201910873410A CN112495352A CN 112495352 A CN112495352 A CN 112495352A CN 201910873410 A CN201910873410 A CN 201910873410A CN 112495352 A CN112495352 A CN 112495352A
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- CN
- China
- Prior art keywords
- chitosan
- beta
- cyclodextrin
- beta cyclodextrin
- acetic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a preparation method of a chitosan-beta cyclodextrin adsorbent, which comprises the following raw materials: acetic acid; chitosan; beta-cyclodextrin; glutaraldehyde; deionized water. The invention firstly mixes chitosan and beta cyclodextrin evenly in acetic acid solution with certain concentration, then adds cross-linking agent to prepare chitosan-beta cyclodextrin composite material, and then carries out pore-forming on the composite material by a freeze-induced drying method. Three chitosan-beta cyclodextrin adsorbents with different addition ratios are prepared.
Description
Technical Field
The invention relates to a preparation method of a chitosan-beta cyclodextrin adsorbent.
Technical Field
Chitosan is a homopolymer formed by connecting 2-amino-2-deoxy-D-glucose monomers by beta (1 → 4) glycosidic bonds. Due to excellent biocompatibility, biodegradability, antibacterial property and immunogenicity, and good adsorbability, film-forming property, biocompatibility and degradability of chitosan, the chitosan has good application value in the fields of medicine, wastewater treatment, fresh keeping and the like.
Beta-cyclodextrin (beta-CD) is a clathrate compound formed by cyclic oligosaccharide (7 glucopyranose units) connected by alpha-1, 4-type glycosidic bonds, has a molecular shape of a slightly hollow round table, has a special molecular structure of 'inner hydrophobicity and outer hydrophilicity', and can be used as a host model to form a clathrate compound with a series of object molecules including inorganic, organic compounds, neutral and ionic compounds and rare gases through host-object recognition (hydrophobicity, hydrogen bonds and Van der Waals force). Because it contains rich O-H bond, C-O bond and C-C bond, it can form many kinds of derivatives with different properties. The beta-cyclodextrin polymer is a high molecular compound and has a chain shape, so that the beta-cyclodextrin polymer has high solubility and adsorbability.
The presence of dyes makes our world more colorful but also results in the discharge of large amounts of organic dye waste water. The dye wastewater which is generated in the printing and dyeing process (pretreatment, dyeing, printing and finishing) has high chroma, strong toxicity, great harm and difficult degradation and has serious harm. The discharge amount of the printing and dyeing wastewater in China is considerable (more than 17 hundred million m3), which accounts for 35 percent of the total amount of the industrial wastewater, the treatment rate is only 30 percent, and the discharge amount which can reach the standard after treatment only accounts for 60 percent of the treatment amount. Therefore, it is very important to develop an effective adsorbent to improve the adsorption rate of the organic dye.
Disclosure of Invention
The invention aims to utilize cyclodextrin and chitosan to carry out crosslinking, exert the synergistic effect of chitosan and cyclodextrin and enhance the adsorption capacity of chitosan. A process for preparing the composite chitosan-beta-cyclodextrin material includes such steps as dissolving chitosan and beta-cyclodextrin in acetic acid solution, stirring, and cross-linking by adding glutaraldehyde at 60 deg.C.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the chitosan-gelatin composite material mainly comprises the following steps:
the first step is as follows: weighing a certain amount of chitosan and a certain amount of beta-cyclodextrin, dissolving in 1% acetic acid solution, and mechanically stirring until the chitosan and the beta-cyclodextrin are completely dissolved and uniformly mixed.
The second step is that: and (3) adding 5% glutaraldehyde into the solution obtained in the first step at 60 ℃ under mechanical stirring, and reacting for a certain time.
The third step: and pre-freezing the product obtained in the second step in a refrigerator for 12 hours, and then drying in a vacuum drying oven for 24 hours. And repeatedly washing the dried sample by using a sodium hydroxide solution and deionized water to wash off acetic acid, and drying to obtain a final product.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts chitosan, has good adsorption capacity and has chelation effect on heavy metal ions and dye ions in sewage.
(2) And a freeze-drying method is adopted to carry out pore-forming on the material, so that the physical adsorption effect is enhanced.
(3) The chitosan and the beta-cyclodextrin have a synergistic effect, and the adsorption capacity of the material is further enhanced.
Detailed Description
The present invention is described in further detail below with reference to examples, but the embodiments of the present invention are not limited thereto. In the following examples of embodiments; the materials and methods mentioned in the examples are those commonly used in the art unless otherwise specified.
Example 1
Weighing a certain amount of chitosan and a certain amount of beta-cyclodextrin according to the ratio of the beta-cyclodextrin to the chitosan being 2: 1, dissolving the mixture in a 1% acetic acid solution, and mechanically stirring the mixture until the chitosan and the beta-cyclodextrin are completely dissolved and uniformly mixed. Adding cross-linking agent glutaraldehyde under stirring, and reacting at 60 deg.C for 2 h. After the reaction is finished, putting the obtained product into a refrigerator for pre-freezing for 12h, and finally putting the product into a vacuum freeze dryer for drying. And repeatedly washing the dried product by using sodium hydroxide and deionized water to remove acetic acid, and drying to obtain the final product.
Example 2
Weighing a certain amount of chitosan and a certain amount of beta-cyclodextrin according to the ratio of the beta-cyclodextrin to the chitosan being 1: 1, dissolving in a 1% acetic acid solution, and mechanically stirring until the chitosan and the beta-cyclodextrin are completely dissolved and uniformly mixed. Adding cross-linking agent glutaraldehyde under stirring, and reacting at 60 deg.C for 2 h. After the reaction is finished, putting the obtained product into a refrigerator for pre-freezing for 12h, and finally putting the product into a vacuum freeze dryer for drying. And repeatedly washing the dried product by using sodium hydroxide and deionized water to remove acetic acid, and drying to obtain the final product.
Example 3
Weighing a certain amount of chitosan and a certain amount of beta-cyclodextrin according to the ratio of the beta-cyclodextrin to the chitosan being 1: 2, dissolving in a 1% acetic acid solution, and mechanically stirring until the chitosan and the beta-cyclodextrin are completely dissolved and uniformly mixed. Adding cross-linking agent glutaraldehyde under stirring, and reacting at 60 deg.C for 2 h. After the reaction is finished, putting the obtained product into a refrigerator for pre-freezing for 12h, and finally putting the product into a vacuum freeze dryer for drying. And repeatedly washing the dried product by using sodium hydroxide and deionized water to remove acetic acid, and drying to obtain the final product.
Claims (2)
1. A preparation method of chitosan-beta cyclodextrin is characterized in that the chitosan-beta cyclodextrin is composed of the following raw materials: the preparation method of the chitosan-beta cyclodextrin comprises the steps of firstly, uniformly mixing chitosan and beta cyclodextrin in an acetic acid solution with a certain concentration, then adding glutaraldehyde to the mixture for crosslinking at 60 ℃, and finally, performing hole forming on the composite material by a freeze-induced drying method.
2. The method for preparing the chitosan-beta cyclodextrin adsorbent according to claim 1, wherein the chitosan-beta cyclodextrin adsorbent comprises the following main steps:
the first step is as follows: chitosan and beta-cyclodextrin are mixed evenly in 1% acetic acid solution.
The second step is that: the two solutions obtained in the first step are crosslinked by adding glutaraldehyde under mechanical stirring at 60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910873410.XA CN112495352A (en) | 2019-09-16 | 2019-09-16 | Preparation method of chitosan-beta cyclodextrin adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910873410.XA CN112495352A (en) | 2019-09-16 | 2019-09-16 | Preparation method of chitosan-beta cyclodextrin adsorbent |
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| Publication Number | Publication Date |
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| CN112495352A true CN112495352A (en) | 2021-03-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910873410.XA Pending CN112495352A (en) | 2019-09-16 | 2019-09-16 | Preparation method of chitosan-beta cyclodextrin adsorbent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114208848A (en) * | 2022-01-20 | 2022-03-22 | 安徽科技学院 | Corn growth regulator containing chitosan and preparation and use methods thereof |
| CN115337914A (en) * | 2022-08-29 | 2022-11-15 | 东华大学 | Nano cyclodextrin crystal adsorbing material with broad-spectrum adsorbability and preparation method thereof |
-
2019
- 2019-09-16 CN CN201910873410.XA patent/CN112495352A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114208848A (en) * | 2022-01-20 | 2022-03-22 | 安徽科技学院 | Corn growth regulator containing chitosan and preparation and use methods thereof |
| CN114208848B (en) * | 2022-01-20 | 2023-02-28 | 安徽科技学院 | Corn growth regulator containing chitosan and preparation and use methods thereof |
| CN115337914A (en) * | 2022-08-29 | 2022-11-15 | 东华大学 | Nano cyclodextrin crystal adsorbing material with broad-spectrum adsorbability and preparation method thereof |
| CN115337914B (en) * | 2022-08-29 | 2023-07-14 | 东华大学 | Nano cyclodextrin crystal adsorption material with broad-spectrum adsorptivity and preparation method thereof |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210316 |
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| WD01 | Invention patent application deemed withdrawn after publication |