CN105618005A - Preparation method of magnetic chitosan - Google Patents
Preparation method of magnetic chitosan Download PDFInfo
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- CN105618005A CN105618005A CN201610186178.9A CN201610186178A CN105618005A CN 105618005 A CN105618005 A CN 105618005A CN 201610186178 A CN201610186178 A CN 201610186178A CN 105618005 A CN105618005 A CN 105618005A
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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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- Environmental & Geological Engineering (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a preparation method of magnetic chitosan. The preparation method comprises the following steps: 1) adding 0.45 to 1.8 g of solid FeCl3.6H2O into 25 ml of ethylene-glycol, putting a beaker into an ultrasound instrument, stirring slowly with a glass rod, adding 0.54 to 2.15g of chitosan powder, and stirring constantly till straw yellow viscous liquid is obtained; 2) adding 2 ml of a hexamethylene diamine solution (1.8646 mol/L) into the straw yellow viscous liquid, and stirring constantly; 3) transferring the liquid treated in the step 2) into a reaction kettle, and carrying out a reaction at 160 to 220 DEG C; 4) after the reaction is finished, cleaning an obtained black mixed solution with secondary water for 2 to 3 times, and cleaning with anhydrous ethyl alcohol for 2 to 3 times, carrying out magnetic hysteresis separation, and drying to obtain a black product MFe3O4/CS NPs. The preparation method is simple to operate; synthesis is realized in one step; the prepared magnetic chitosan is used for adsorb treatment of dye wastewater, and has the advantages of high in separation possibility and recyclability, free of secondary pollution and low in cost.
Description
Technical field
The present invention relates to sewage treating material, specifically belong to the preparation method of a kind of chitosan magnetic sorbent material, and the application of chitosan magnetic in dye wastewater treatment.
Background technology
Developing rapidly of modern industry creates a large amount of waste water containing dyestuff, because of its pollutent non-degradable and easily by food chain enrichment in organism, environment and human lives is constituted very big threat. In the treatment process of current waste water from dyestuff, biosorption process widespread use because of simple to operate, processing efficiency height. Wherein the advantage such as chitosan resource is abundant, environmental friendliness, adsorptive power height, diffusion are good owing to having, selective adsorption, easily activity recovery, is subject to extensive concern.
Chitosan (Chitosan) is the de-acetyl product of the biomass resource chitin that in nature, reserves are second largest. It, as a kind of line style natural polymer, has good biocompatibility and degradability, containing a large amount of hydroxyls, amino on its macromolecular chain, dyestuff has certain adsorption, can be used as the dyestuff in a kind of sorbent treatment waste water. Chitosan being carried out chemical modification, it is possible to generate corresponding derivative, the process aspect for waste water from dyestuff has a good application prospect.
Recently, magnetic separation technique is subject to the extensive concern of researcher, wherein magneticsubstance Fe3O4The most common. People are for Fe3O4Research experienced by from micron to nanometer change procedure. Find to work as Fe3O4When microballoon is in nano-scale, its structure being different from solid matter and also there is very big difference with single atom, this kind of unique structure makes Fe just3O4Microballoon has novelty, efficient, unique physics and chemistry character such as superparamagnetism etc. Exactly because this kind of unique character makes Fe3O4Microballoon has potential using value in numerous fields such as dyestuff, magnetic recording, biomedicine, Magnetic Sensor, catalyzer so that it becomes emphasis and the focus of scientific researcher research.
At present, chitosan magnetic absorption method dye wastewater treatment is applied. But, synthetic method complexity, the cost height of existing chitosan magnetic, adsorption efficiency is low, repeating utilization factor is low, therefore, study that a kind of easy synthesis, cost are low, adsorption efficiency height, the chitosan magnetic that can reuse seem particularly important.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of a kind of chitosan magnetic, and the method is simple to operate, one-step synthesis; When prepared chitosan magnetic is disposed of sewage easily separated, can reuse, non-secondary pollution, cost low.
The preparation method of a kind of chitosan magnetic provided by the invention, step is:
1) in 25mL ethylene glycol, add the FeCl of 0.45-1.8g3��6H2O solid, puts into ultrasonic apparatus by beaker and slowly stirs with glass stick, adds the Chitosan powder of 0.54-2.15g subsequently and constantly stirs, to forming light yellow viscous liquid;
2) in above-mentioned thick liquid, add 2mL (1.8646mol/L) hexanediamine solution and constantly stir;
3) by step 2) divert away that processes in reactor, 160 DEG C-220 DEG C reaction 6h-10h;
4) after having reacted, obtain black mixed solution, respectively with two water, washes of absolute alcohol 2-3 time, carry out magnetic hysteresis separation, obtain black product;
5) black product is put into the dry 24h of vacuum drying oven, and the black powder obtained is final product MFe3O4/CSNPs��
Preferred steps 1) in FeCl3��6H2The add-on of O solid is 1.5g. Chitosan powder add-on is 1.79g.
Preferred steps 3) in temperature of reaction be 220 DEG C, reaction times 8h.
Above-mentioned prepared chitosan magnetic can be applied in dye wastewater treatment. Particularly application in process amino black 10B waste water from dyestuff.
Compared with prior art, the advantage of the present invention: chitosan magnetic synthetic method is one step hydro thermal method, preparation method is simple, and reaction conditions is gentle; The required medicine number of synthesis reduces in reporting than other documents to some extent, saves medicine, reduces costs. Products therefrom has good dispersion and stability, and gets final product separated and collected under the existence of external magnetic field, easily reclaims, and takes off attached recycling, saves Financial cost, easily realizes mass-producing application.
Accompanying drawing explanation
Fig. 1 is MFe prepared by embodiment 33O4The transmission electron microscope picture of/CSNPs.
Fig. 2 is MFe prepared by embodiment 33O4The scanning electron microscope (SEM) photograph of/CSNPs.
Fig. 3 is MFe prepared by embodiment 33O4The FTIR spectrum figure of/CSNPs.
Fig. 4 is MFe prepared by embodiment 33O4The susceptibility curve of/CSNPs.
Fig. 5 is MFe prepared by embodiment 33O4/ CSNPs adsorbs the adsorption isothermal curve of amino black 10B.
Fig. 6 is MFe prepared by embodiment 33O4/ CSNPs adsorbs the curve of adsorption kinetics of amino black 10B.
Fig. 7 is MFe prepared by embodiment 33O4When/CSNPs adsorbs amino black 10B, pH is to the effect diagram of adsorptive capacity.
Embodiment
The following is and in conjunction with the accompanying drawings and embodiments the present invention is described in further details.
Embodiment 1
1. the preparation of chitosan magnetic
1) in 25mL ethylene glycol, add the FeCl of 1.5g3��6H2O solid, puts into ultrasonic apparatus by beaker and slowly stirs with glass stick, adds the Chitosan powder of 1.79g subsequently and constantly stirs;
2) in above-mentioned solution, move into 2mL (1.8646mol/L) hexanediamine solution with shifting liquid rifle and constantly stir;
3) above-mentioned solution is transferred in 50ml inner liner of reaction kettle, after assembling reactor, puts it in the air dry oven of 160 DEG C and react 6h;
4) after having reacted, take out reactor, obtain black mixed solution, respectively with two water, washes of absolute alcohol 2-3 time, carry out magnetic hysteresis separation, obtain black product;
5) this product is put into the dry 24h of vacuum drying oven, and the black powder obtained is final product MFe3O4/CSNPs��
2. the adsorption experiment of amino black 10B
1) MFe of 0.001g is got3O4/ CSNPs adds in certain volume 2mg/mL amino black 10B solution;
2) above-mentioned for mixing mixing liquid is placed shaking table and shake 1h;
3) MFe is surveyed respectively at amino black 10B maximum absorption wavelength 618nm place3O4/ CSNPs adsorbs the absorbancy of solution before and after amino black 10B, thus calculates MFe3O4/ CSNPs, to the maximal absorptive capacity of amino black 10B, is 13.81mg/g.
Embodiment 2
1. the preparation of chitosan magnetic
1) in 25mL ethylene glycol, add the FeCl of 1.5g3��6H2O solid, puts into ultrasonic apparatus by beaker and slowly stirs with glass stick, adds the Chitosan powder of 1.79g subsequently and constantly stirs;
2) in above-mentioned solution, move into 2mL (1.8646mol/L) hexanediamine solution with shifting liquid rifle and constantly stir;
3) above-mentioned solution is transferred in 50ml inner liner of reaction kettle, after assembling reactor, puts it in the air dry oven of 180 DEG C and react 8h;
4) after having reacted, take out reactor, obtain black mixed solution, respectively with two water, washes of absolute alcohol 2-3 time, carry out magnetic hysteresis separation, obtain black product;
5) this product is put into the dry 24h of vacuum drying oven, and the black powder obtained is final product MFe3O4/CSNPs��
2. the adsorption experiment of amino black 10B
1) MFe of 0.001g is got3O4/ CSNPs adds in certain volume 2mg/mL amino black 10B solution;
2) above-mentioned for mixing mixing liquid is placed shaking table and shake 1h;
3) MFe is surveyed respectively at amino black 10B maximum absorption wavelength 618nm place3O4/ CSNPs adsorbs the absorbancy of solution before and after amino black 10B, thus calculates MFe3O4/ CSNPs, to the maximal absorptive capacity of amino black 10B, is 30.13mg/g.
Embodiment 3
1. the preparation of chitosan magnetic
1) in 25mL ethylene glycol, add the FeCl of 1.5g3��6H2O solid, puts into ultrasonic apparatus by beaker and slowly stirs with glass stick, adds the Chitosan powder of 1.79g subsequently and constantly stirs;
2) in above-mentioned solution, move into 2mL (1.8646mol/L) hexanediamine solution with shifting liquid rifle and constantly stir;
3) above-mentioned solution is transferred in 50ml inner liner of reaction kettle, after assembling reactor, puts it in the air dry oven of 220 DEG C and react 8h;
4) after having reacted, take out reactor, obtain black mixed solution, respectively with two water, washes of absolute alcohol 2-3 time, carry out magnetic hysteresis separation, obtain black product;
5) this product is put into the dry 24h of vacuum drying oven, and the black powder obtained is final product MFe3O4/CSNPs��
2. the adsorption experiment of amino black 10B
1) MFe of 0.001g is got3O4/ CSNPs adds in certain volume 2mg/mL amino black 10B solution;
2) above-mentioned for mixing mixing liquid is placed shaking table and shake 1h;
3) MFe is surveyed respectively at amino black 10B maximum absorption wavelength 618nm place3O4/ CSNPs adsorbs the absorbancy of solution before and after amino black 10B, thus calculates MFe3O4/ CSNPs, to the maximal absorptive capacity of amino black 10B, is 99.94mg/g.
Embodiment 4
1. the preparation method of chitosan magnetic is with embodiment 3
2. the adsorption experiment of methylene blue
1) MFe of 0.001g is got3O4/ CSNPs adds in certain volume 2mg/mL methylene blue solution;
2) above-mentioned for mixing mixing liquid is placed shaking table and shake 1h;
3) MFe is surveyed respectively at methylene blue maximum absorption wavelength 665nm place3O4/ CSNPs adsorbs the absorbancy of solution before and after methylene blue, thus calculates MFe3O4/ CSNPs, to the maximal absorptive capacity of methylene blue, is 54.42mg/g.
Embodiment 5
1. the preparation method of chitosan magnetic is with embodiment 3
2. the adsorption experiment of acid red G
1) MFe of 0.001g is got3O4/ CSNPs adds in certain volume 2mg/mL acid red G solution;
2) above-mentioned for mixing mixing liquid is placed shaking table and shake 1h;
3) MFe is surveyed respectively at acid red G maximum absorption wavelength 504nm place3O4The absorbancy of solution before and after the bright red G of/CSNPs adsorb acidic, thus calculate MFe3O4/ CSNPs, to the maximal absorptive capacity of acid red G, is 46.21mg/g.
Claims (7)
1. the preparation method of a chitosan magnetic, it is characterised in that, step is:
1) in 25mL ethylene glycol, add the FeCl of 0.45-1.8g3��6H2O solid, puts into ultrasonic apparatus by beaker and slowly stirs with glass stick, adds the Chitosan powder of 0.54-2.15g subsequently and constantly stirs, to forming light yellow viscous liquid;
2) in above-mentioned thick liquid, add hexanediamine solution that 2mL concentration is 1.8646mol/L and constantly stir;
3) by step 2) divert away that processes in reactor, 160 DEG C-220 DEG C reaction 6h-10h;
4) after having reacted, obtain black mixed solution, respectively with two water, washes of absolute alcohol 2-3 time, carry out magnetic hysteresis separation, obtain black product;
5) black product is put into the dry 24h of vacuum drying oven, and the black powder obtained is final product MFe3O4/CSNPs��
2. the preparation method of chitosan magnetic as claimed in claim 1, it is characterised in that, described step 1) in FeCl3��6H2The add-on of O solid is 1.5g.
3. the preparation method of chitosan magnetic as claimed in claim 1, it is characterised in that, described step 1) in Chitosan powder add-on be 1.79g.
4. the preparation method of chitosan magnetic as claimed in claim 1, it is characterised in that, described step 3) in temperature of reaction be 220 DEG C.
5. the preparation method of chitosan magnetic as claimed in claim 1, it is characterised in that, described step 3) in the reaction times be 8h.
6. the application of the chitosan magnetic that as claimed in claim 1 prepared by method in dye wastewater treatment.
7. the application of the chitosan magnetic that as claimed in claim 1 prepared by method in process amino black 10B waste water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106215880A (en) * | 2016-08-31 | 2016-12-14 | 南京大学 | The preparation method of chitosan magnetic bead |
| CN107262033A (en) * | 2017-06-30 | 2017-10-20 | 安徽工业大学 | The preparation and application of a kind of attapulgite/Fe3O4/ carbon composites |
| CN109126728A (en) * | 2018-08-27 | 2019-01-04 | 成都信息工程大学 | A kind of Fe3O4The preparation method and applications of chitosan |
| CN110064378A (en) * | 2019-05-08 | 2019-07-30 | 广州大学 | A kind of high absorption property chitosan magnetic carbon ball and its preparation method and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106215880A (en) * | 2016-08-31 | 2016-12-14 | 南京大学 | The preparation method of chitosan magnetic bead |
| CN107262033A (en) * | 2017-06-30 | 2017-10-20 | 安徽工业大学 | The preparation and application of a kind of attapulgite/Fe3O4/ carbon composites |
| CN109126728A (en) * | 2018-08-27 | 2019-01-04 | 成都信息工程大学 | A kind of Fe3O4The preparation method and applications of chitosan |
| CN110064378A (en) * | 2019-05-08 | 2019-07-30 | 广州大学 | A kind of high absorption property chitosan magnetic carbon ball and its preparation method and application |
| CN110064378B (en) * | 2019-05-08 | 2021-10-26 | 广州大学 | Magnetic chitosan carbon sphere with high adsorption performance and preparation method and application thereof |
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