CN115245812A - Preparation method of chitosan/sodium alginate/acrylamide composite hydrogel - Google Patents
Preparation method of chitosan/sodium alginate/acrylamide composite hydrogel Download PDFInfo
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- CN115245812A CN115245812A CN202210000075.4A CN202210000075A CN115245812A CN 115245812 A CN115245812 A CN 115245812A CN 202210000075 A CN202210000075 A CN 202210000075A CN 115245812 A CN115245812 A CN 115245812A
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- chitosan
- sodium alginate
- acrylamide
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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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
Abstract
The invention relates to the technical field of hydrogel adsorption materials, and discloses a preparation method of chitosan/sodium alginate/acrylamide composite hydrogel. Firstly, dissolving sodium alginate in deionized water, secondly, dissolving chitosan in an acidic aqueous solution, thirdly, uniformly mixing the solutions in the first two steps, adding an acrylamide monomer, a cross-linking agent, an initiator and the like, stirring at normal temperature to generate free radicals on hydroxyl groups of the sodium alginate, polymerizing the free radicals with acrylamide to form a polymerized macromolecular substance, and drying to obtain the chitosan/sodium alginate/acrylamide hydrogel material. The method has the advantages of simple synthesis steps, environmental friendliness and no pollution, and the prepared hydrogel material has excellent mechanical properties and has a good adsorption effect on cationic dyes in wastewater. The hydrogel can be used in the fields of textile printing and dyeing wastewater treatment, dye adsorption and the like.
Description
Technical Field
The invention belongs to the technical field of hydrogel adsorbing materials, and particularly relates to a preparation method of a chitosan/sodium alginate/acrylamide hydrogel adsorbing material.
Background
Water is the source of our lives and is one of the basic conditions under which all organisms live. Only with the existence of water, the blue and beautiful star can survive human beings, animals and plants, etc. However, with the rapid development of cities, the pollution of water resources is increased more and more by industrial pollution sources, agricultural pollution sources, domestic pollution sources and the like, and the most representative of the pollution is wastewater in the textile printing and dyeing industry. If untreated wastewater is directly discharged, it may cause serious damage to human health, and may contaminate organisms in water and cause quality reduction of crops, etc., thereby destroying the ecosystem. Therefore, the problem of simply, efficiently and correctly treating water pollution is urgent.
At present, the methods for treating water pollution mainly comprise a chemical precipitation method, an oxidation-reduction method, a material adsorption method and the like. The adsorption method has the advantages of low cost, environmental friendliness, good treatment effect and the like, and has great potential for treating wastewater. However, most of the conventional adsorbents such as activated carbon, activated carbon fiber, zeolite, bentonite, etc. have disadvantages of insignificant effects, high cost, low recyclability, etc., thereby limiting the application range thereof. Therefore, researchers have tried to replace conventional adsorbents with some environmentally friendly natural biomass adsorbent materials that are recyclable and biodegradable.
Hydrogels have an extremely hydrophilic three-dimensional network gel structure, can swell rapidly in water and can hold a large volume of water in the swollen state without dissolving, and the water content in the hydrogel can be as low as a few percent, or as high as 99%.
Chitosan (chitosan) is a chitin N-deacetylated product, and the amino group in the molecular structure of chitosan has strong reactivity, so that the polysaccharide has excellent biological functions and can be subjected to chemical modification reaction. Chitosan has good biocompatibility and is considered as a functional biological material with great application potential. However, due to the disadvantages of low mechanical properties, poor stability in acidic solutions, etc., structural and chemical modifications are still required. Sodium alginate is hygroscopic and readily disperses in water to form a transparent colloidal solution. Sodium alginate and chitosan are introduced as functional monomers, so that the stability of chitosan in an acidic medium can be improved, and the mechanical strength of the chitosan can be improved. The acrylamide hydrogel contains a large amount of functional groups such as carbonyl, amino and amido, has good adsorption effect on cationic dyes such as methylene blue, and has the effect of sewage purification.
For the above reasons, the present application is proposed.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a preparation method of chitosan/sodium alginate/acrylamide hydrogel.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of chitosan/sodium alginate/acrylamide hydrogel comprises the following steps:
(1) Dissolving chitosan in an acidic aqueous solution, and magnetically stirring at normal temperature to completely dissolve the chitosan;
(2) Dissolving sodium alginate in deionized water, and magnetically stirring at normal temperature to dissolve completely;
(3) And (3) uniformly mixing the solutions in the steps (1) and (2) at normal temperature, adding acrylamide, N-methylene bisacrylamide and ammonium persulfate after 10min, continuously performing magnetic stirring for 1h, taking out, and putting into a vacuum drying oven for 24h to obtain the chitosan/sodium alginate/acrylamide composite hydrogel.
Preferably, in step (1), the acidic aqueous solution is glacial acetic acid aqueous solution, formic acid aqueous solution or nitric acid aqueous solution.
Preferably, in step (1), the acidic aqueous solution is glacial acetic acid aqueous solution.
As a preferable scheme, in the step (1), the volume concentration of the acidic aqueous solution is 0.01-1%.
As a preferable scheme, in the step (1), the volume concentration of the acidic aqueous solution is 0.1%.
As a preferable mode, in the step (3), the temperature in the vacuum drying oven is 70 ℃.
The invention has the beneficial effects that: the chitosan/sodium alginate/acrylamide three-dimensional network crosslinked hydrogel prepared by the invention has good adsorption effect on cationic dyes in wastewater, particularly methylene blue dyes, such as large adsorption capacity, good stability, good reusability and the like, and has good mechanical properties.
Detailed Description
The present invention is further illustrated by the following specific examples, which are provided for the purpose of illustration only and are not to be construed as limiting the invention.
Example 1: preparing chitosan/sodium alginate/acrylamide hydrogel with adsorption function.
(1) 0.75g of chitosan was dissolved in 30ml of 0.1% acetic acid solution, and the solution was dissolved completely by magnetic stirring.
(2) 2.25g of sodium alginate is dissolved in 90ml of deionized water, and the mixture is magnetically stirred at normal temperature until the sodium alginate is completely dissolved.
(3) And (3) slowly and uniformly mixing the two dissolved solutions at normal temperature, transferring the two solutions into a beaker, adding 30g of acrylamide, 0.3g of MBA (N, N-methylene bisacrylamide) and 0.3g of APS (ammonium persulfate), continuously magnetically stirring for 1 hour, taking out, and putting into a vacuum drying oven for 24 hours to obtain the chitosan/sodium alginate/acrylamide crosslinked hydrogel.
(4) The hydrogel obtained in (3) was cut into soybean-sized small pieces with a small knife. And putting the mixture into a vacuum drying oven for 48 hours, taking out the mixture, grinding the mixture into small particles, weighing 0.05g of dry gel in parts, and filling the dry gel into a non-woven fabric tea bag for later use.
Examples 1 to 1
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 1 hour, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 36mg/g.
Examples 1 to 2
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 2 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 44mg/g.
Examples 1 to 3
Will be adornedNonwoven tea bags containing 0.05g of xerogel particles were filled to 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 8 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 47mg/g.
Examples 1 to 4
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 10 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, which was 52mg/g.
Examples 1 to 5
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 27 hours, and the amount of methylene blue adsorbed was measured by shaking at 25 ℃ for 12 hours, and the amount of methylene blue adsorbed was 58mg/g.
Examples 1 to 6
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 38 hours, and the amount of methylene blue adsorbed was measured by shaking at 25 ℃ for 12 hours, and the amount of methylene blue adsorbed was 61mg/g.
Example 2: preparing chitosan/sodium alginate/acrylamide hydrogel with adsorption function.
(1) 0.7g of chitosan was dissolved in 30ml of 0.1% acetic acid solution, and the solution was stirred by magnetic force to dissolve completely.
(2) 2.0g of sodium alginate was dissolved in 90ml of deionized water and stirred magnetically at 30 ℃ until it was completely dissolved.
(3) And (3) slowly and uniformly mixing the two dissolved solutions at normal temperature, transferring the two solutions into a beaker, adding 30g of acrylamide, 0.3g of MBA (N, N-methylene bisacrylamide) and 0.3g of APS (ammonium persulfate), continuously magnetically stirring for 1 hour, taking out the solution, and putting the solution into a vacuum drying oven for 24 hours to obtain the chitosan/sodium alginate/acrylamide three-dimensional network crosslinked gel.
(4) The hydrogel obtained in (3) was cut into soybean-sized small pieces with a small knife. Putting into a vacuum drying oven for 48h, taking out, grinding into small particles, respectively weighing 0.05g, and filling into a non-woven fabric tea bag filter bag for later use.
Example 2-1
The non-woven tea bag containing 0.05g of xerogel particles is put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 1 hour, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 32mg/g.
Examples 2 to 2
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 2 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 40mg/g.
Examples 2 to 3
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 8 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 43mg/g.
Examples 2 to 4
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 10 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 45mg/g.
Examples 2 to 5
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution (2) was adsorbed at room temperature for 27 hours, and then shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 49mg/g.
Examples 2 to 6
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 38 hours, and the amount of methylene blue adsorbed was measured by shaking at 25 ℃ for 12 hours, whereby the amount of methylene blue adsorbed was 51mg/g.
Example 3: preparing chitosan/sodium alginate/acrylamide hydrogel with adsorption function.
(1) 0.5g of chitosan was dissolved in 30ml of 0.1% acetic acid solution, and the solution was dissolved completely by magnetic stirring.
(2) 1.5g of sodium alginate was dissolved in 90ml of deionized water and stirred magnetically at 30 ℃ until it was completely dissolved.
(3) And slowly and uniformly mixing the two dissolved solutions at normal temperature, transferring the two solutions into a beaker, adding 30g of acrylamide, 0.3g of MBA (N, N-methylene bisacrylamide) and 0.3g of APS (ammonium persulfate), continuously magnetically stirring for 1 hour, taking out the solution, and putting the solution into a vacuum drying oven for 24 hours to obtain the chitosan/sodium alginate/acrylamide three-dimensional network crosslinked gel.
(4) The hydrogel obtained in (3) was cut into soybean-sized small pieces with a small knife. Putting into a vacuum drying oven for 48h, taking out, grinding into small particles, weighing 0.05g respectively, and packaging into non-woven fabric tea bags for later use.
Example 3-1
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 1 hour, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 30mg/g.
Example 3-2
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 2 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 35mg/g.
Examples 3 to 3
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 8 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the amount of methylene blue adsorbed, and the amount of methylene blue adsorbed was 39mg/g.
Examples 3 to 4
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 In methylene blue solution of (2), adsorbing at room temperature10h, shaking at constant temperature of 25 ℃ for 12h, and measuring the adsorption quantity of methylene blue, wherein the adsorption quantity is 42mg/g.
Examples 3 to 5
The non-woven tea bag containing 0.05g of xerogel particles was put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 27 hours, and the amount of methylene blue adsorbed was measured by shaking at 25 ℃ for 12 hours, and the amount of methylene blue adsorbed was 45mg/g.
Examples 3 to 6
The non-woven tea bag containing 0.05g of xerogel particles is put into 40ml of 25mg L -1 The methylene blue solution was adsorbed at room temperature for 38 hours, and the solution was shaken at a constant temperature of 25 ℃ for 12 hours to measure the adsorption amount of methylene blue, which was 48mg/g.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which are made without departing from the spirit and principle of the present invention should be construed as equivalents and all fall within the protection scope of the present invention.
Claims (4)
1. A preparation method of chitosan/sodium alginate/acrylamide composite hydrogel comprises the following formula raw materials and components, and is characterized in that: 5-10 parts of chitosan, 20-25 parts of sodium alginate, 25-40 parts of acrylamide, 2-6 parts of N, N-methylene bisacrylamide and 2-6 parts of ammonium persulfate.
2. A preparation method of chitosan/sodium alginate/acrylamide composite hydrogel is characterized by comprising the following steps: dissolving chitosan in an acidic aqueous solution, and magnetically stirring at normal temperature to completely dissolve the chitosan, (2) dissolving sodium alginate in deionized water, and magnetically stirring at normal temperature to completely dissolve the sodium alginate, (3) uniformly mixing the solutions obtained in the steps (1) and (2) at normal temperature, adding acrylamide, N-methylene bisacrylamide and ammonium persulfate after 10min, magnetically stirring at normal temperature for 1h, taking out, and putting in a drying oven for 24h to obtain the chitosan/sodium alginate/acrylamide composite hydrogel.
3. The preparation method of claim 2, wherein in the step (1), the acidic aqueous solution is glacial acetic acid aqueous solution, formic acid aqueous solution or nitric acid aqueous solution, and the volume concentration is 0.01% -1%.
4. Furthermore, in the step (1), the acidic aqueous solution is glacial acetic acid aqueous solution, and in the step (1), the volume concentration of the acidic aqueous solution is 0.1%.
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Citations (5)
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| CN105504166A (en) * | 2016-01-20 | 2016-04-20 | 武汉理工大学 | Sodium alginate-acrylamide composite aquagel, and preparation method and application thereof |
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| WO2019062024A1 (en) * | 2017-09-26 | 2019-04-04 | 上海工程技术大学 | Method for preparing soil conditioner |
| CN113230202A (en) * | 2021-05-14 | 2021-08-10 | 大连理工大学 | Preparation method of core-shell structure gastric retention hydrogel capable of realizing sustained release of drug |
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- 2022-01-02 CN CN202210000075.4A patent/CN115245812A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| CN105194740A (en) * | 2015-09-20 | 2015-12-30 | 哈尔滨工业大学 | Postoperation anti-adhesion hydrogel and preparing method thereof |
| CN105504166A (en) * | 2016-01-20 | 2016-04-20 | 武汉理工大学 | Sodium alginate-acrylamide composite aquagel, and preparation method and application thereof |
| WO2019062024A1 (en) * | 2017-09-26 | 2019-04-04 | 上海工程技术大学 | Method for preparing soil conditioner |
| CN109319908A (en) * | 2018-11-07 | 2019-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Modification of chitosan-sodium alginate composite flocculation agent preparation method and products thereof and application |
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| Title |
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| PRIYA ET AL.: "Chemically modified chitosan‑sodium alginate as chemo-sensor adsorbent for the detection of picric acid and removal of biebrich scarlet", 《INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES》, vol. 147, pages 2 * |
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