CN112169773B - Enhanced magnetic adsorbent - Google Patents
Enhanced magnetic adsorbent Download PDFInfo
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- CN112169773B CN112169773B CN202011104309.7A CN202011104309A CN112169773B CN 112169773 B CN112169773 B CN 112169773B CN 202011104309 A CN202011104309 A CN 202011104309A CN 112169773 B CN112169773 B CN 112169773B
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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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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- 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
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
Abstract
The invention discloses an enhanced magnetic adsorbent, which is prepared by the following steps: s1, mixing Fe 3 O 4 Adding magnetic nanoparticles into ethanol solution, adding ammonia water solution and distilled water after ultrasonic dispersion, dropwise adding TEOS after ultrasonic dispersion to obtain Fe 3 O 4 @SiO 2 (ii) a S2, dissolving chitosan in acetic acid to obtain chitosan solution, adding Fe 3 O 4 @SiO 2 Stirring the nano particles to obtain a suspension, dispersing the suspension in a mixed solution of cyclohexane and span80, and dripping a glutaraldehyde solution to obtain a magnetic chitosan microsphere solution; s3, adding an initiator VA-044, mixing uniformly, adding a cationic monomer, sealing, and initiating copolymerization under ultraviolet light to obtain the enhanced magnetic adsorbent. The invention can improve the adsorption performance of the chitosan magnetic microsphere, can be repeatedly utilized and reduces the adsorption cost.
Description
Technical Field
The invention relates to the field of dye wastewater treatment, in particular to an enhanced magnetic adsorbent.
Background
The dye is widely applied to industries of food, clothing, decoration and the like, and because of toxicity and mutagenicity, the dye seriously pollutes water environment and an ecological system, particularly, azo dye can convert various carcinogenic substances under certain conditions and is harmful to human health. The treatment of dye wastewater is a problem to be solved urgently, and the adsorption method is the most popular and common method for removing various dyes, metals and medicines and has the advantages of simple operation and low energy consumption. Therefore, in recent years, the development of novel dye decolorization adsorbents has been the focus of much research. Common adsorbents include activated carbon, resins, silicon, graphene, zeolites. However, these adsorbents are limited in that they have low adsorption efficiency and poor recyclability.
Chitosan is a chitin deacetylation product, has active hydroxyl and amino groups with chemical reaction characteristics, and has good adsorption performance on dyes when used as an environment-friendly adsorbent. But its adsorption depends mainly on-NH 2 When sewage is treated, the influence of pH is large, amino groups and hydroxyl groups on molecular chains of chitosan can be used as functional groups for adsorbing pollutants, but the number of the functional groups is limited, the adsorption effect on certain target pollutants is limited, and after the chitosan adsorbs the pollutants, the chitosan is difficult to separate and recover from water, so that the chitosan is prevented from being directly used as an adsorbent.
In recent years, magnetic adsorbents have received much attention. Usually magnetite (Fe) 3 O 4 ) It is widely used as a magnetic substrate due to its low toxicity, superparamagnetism and biocompatibility. To increase Fe 3 O 4 The nanoparticles are often inorganically coated for their oxidation and acid resistance. SiO 2 2 Is coated with Fe 3 O 4 Ideal material for nano-particles because of SiO 2 Has good chemical stability, biocompatibility and hydrophilicity, and SiO 2 Can block Fe 3 O 4 Aggregation of the nanoparticles. In order to facilitate the recycling of chitosan, the chitosan is coated with SiO 2 Fe (b) of 3 O 4 And (3) crosslinking the nano particles to prepare the magnetic chitosan adsorbent. However, chitosan was coated with SiO 2 Fe (b) of 3 O 4 The amount of chitosan is greatly reduced after the nanoparticles are crosslinked, so that the adsorption performance to the dye is reduced.
Therefore, how to prepare an enhanced magnetic adsorbent to treat increasingly complex industrial wastewater is crucial.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the problems of small quantity of crosslinked chitosan and poor adsorption performance to dyes in the existing magnetic chitosan adsorbent, and provides an enhanced magnetic adsorbent.
In order to solve the technical problems, the invention adopts the following technical scheme:
the enhanced magnetic adsorbent is prepared by the following steps:
s1, mixing Fe 3 O 4 Adding magnetic nanoparticles into ethanol solution, adding ammonia water solution and distilled water after ultrasonic dispersion, dropwise adding TEOS after ultrasonic dispersion, and obtaining SiO after reaction 2 Coated Fe 3 O 4 Magnetic nanoparticles of Fe 3 O 4 @SiO 2 ；
S2, dissolving chitosan in acetic acid with the mass fraction of 1% to obtain a chitosan solution, and adding Fe 3 O 4 @SiO 2 Stirring the nano particles to obtain a suspension, dispersing the suspension in a mixed solution of cyclohexane and span80 to obtain an oil-water suspension, and finally dripping a glutaraldehyde solution with the mass fraction of 50% to obtain a magnetic chitosan microsphere solution;
s3, filling N into the magnetic chitosan microsphere dispersion liquid 2 Then adding initiator VA-044, mixing, and charging N 2 Adding cationic monomer, and filling N 2 And sealing and placing under ultraviolet light to initiate copolymerization, and obtaining the enhanced magnetic adsorbent after the reaction is finished.
Wherein, in the step S1, Fe 3 O 4 The mass-volume ratio of the ammonia water to the TEOS is 1 g: 10-12 mL: 4.5-5.5 mL.
In step S2, chitosan and Fe 3 O 4 @SiO 2 The mass ratio of (1): 0.45 to 0.5; the mass volume ratio of chitosan to cyclohexane, span80 and glutaraldehyde is 1 g: 75-80 mL: 0.5-0.6 mL: 0.25-0.3 mL. The concentration of the chitosan solution was 3.75%.
In the step S3, the mass ratio of the initiator VA-044 to the magnetic chitosan microspheres is 0.055-0.135: 1; the mass-to-volume ratio of the magnetic chitosan microspheres to the cationic monomers is 1: 10 to 30. The cationic monomer is acryloyloxyethyl dimethyl benzyl ammonium chloride. The time for photocatalytic initiation of the mixture by ultraviolet irradiation is 1-3 h, and the irradiation intensity is 1000 mu m cm -2 The reaction vessel was placed on a rotating platform at 8 rpm, and the mixture was periodically subjected to ultraviolet light.
Compared with the prior art, the invention has the following advantages:
1. the enhanced magnetic adsorbent provided by the invention is synthesized by introducing acryloyloxyethyl dimethyl benzyl ammonium chloride (AO) with hydrophilic functional groups (quaternary ammonium) and hydrophobic functional groups (benzyl) by adopting an ultraviolet irradiation method, and has good adsorption effect on anionic azo dyes and greatly improved adsorption performance of chitosan magnetic microspheres due to the fact that a large number of quaternary ammonium salt groups of cationic functional groups and benzyl groups with large pi bonds have electrostatic adsorption and pi-pi stacking effects.
2. After adsorbing the anionic azo dye, the enhanced magnetic adsorbent provided by the invention can be rapidly separated and enriched by a magnetic separation technology, can be desorbed by NaOH solution after separation, and then can be regenerated by HCl solution, so that the adsorbent can be recycled, high adsorption capacity can be still reserved after regeneration, and the adsorption cost is greatly reduced.
3. The preparation method provided by the invention adopts ultraviolet light to initiate copolymerization in the preparation process, has high grafting efficiency, is prepared at low temperature, is simple to operate, has no side reaction, and is environment-friendly. The preparation cost is low, and the method is suitable for being widely used for treating dye wastewater.
Drawings
FIG. 1 is a scanning electron micrograph of the enhanced magnetic adsorbent (PFSC) provided in example 1.
FIG. 2 shows Fe provided in example 1 3 O 4 、Fe 3 O 4 @ SiO 2 (FS), magnetic chitosan microspheres (FSC), and enhanced magnetic adsorbents (PFSC).
FIG. 3 is a graph showing the adsorption efficiency of 4 adsorbents (FSC, PFSC1, PFSC 3) to 3 anionic azo dyes of orange II, acid Red 88 or amaranth at different dosages.
FIG. 4 is a graph of the adsorption efficiency of adsorbents FSC and PFSC at different pH's for 3 anionic azo dyes of orange II, acid Red 88 or amaranth.
Fig. 5 is a graph of the recycling of the enhanced magnetic adsorbent (PFSC) provided in example 1.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments.
Firstly, preparing an enhanced magnetic adsorbent.
Example 1
The enhanced magnetic adsorbent is prepared by the following steps:
s1 preparation of Fe 3 O 4 @SiO 2 Nanoparticles (FS): 1.2 g of Fe 3 O 4 Adding the magnetic nanoparticles into a 1000 mL glass beaker containing 600 mL of ethanol, performing ultrasonic dispersion for 10-15 min, then adding 13 mL of ammonia water solution and 200 mL of distilled water, performing ultrasonic dispersion for 40 min, then dropwise adding 6 mL of TEOS, and stirring at room temperature for 8 h; after the reaction is finished, washing the reaction product for 3 times by using ethanol and distilled water, pouring the reaction product into an evaporating dish, and drying the reaction product for 4 hours in vacuum to obtain SiO 2 Coated Fe 3 O 4 Magnetic nanoparticles.
S2, preparing magnetic chitosan microspheres (FSC): firstly, 7.5 g of chitosan is dissolved in 200 mL of acetic acid solution with the mass fraction of 1 percent to prepare chitosan solution with the mass fraction of 3.75 percent, the chitosan solution is stirred for 1 hour, and 3.5 g of Fe obtained in the step S1 is added into the chitosan solution 3 O 4 @SiO 2 And (3) stirring the nanoparticles to obtain a suspension, dispersing the suspension in a mixed solution of 600 mL of cyclohexane and 4.0 mL of span80, and stirring at room temperature for 1 h to obtain an aqueous-oil suspension. Finally, 2.2 mL of a 50% by mass glutaraldehyde solution were added dropwise to the aqueous-oil suspension and the reaction was stirred at 50 ℃ for 3 h. After the reaction is finished, separating the black microspheres by using a magnet, repeatedly washing the black microspheres by using ethanol and water, and drying the black microspheres in vacuum at 50 ℃ until the weight of the black microspheres is constant to obtain the magnetic chitosan microspheres, wherein the magnetic chitosan microspheres are marked as FSC.
S3, preparing a reinforced magnetic adsorbent (PFSC): 0.5 g of the magnetic chitosan microspheres obtained in step S2 was dispersed in 100 mL of distilled water, and the mixture was added to the above solutionFilling N into the dispersion 2 After 3 min, 0.0525 g of initiator VA-044 is added, mixed evenly and N is charged 2 After 5 min, 10 mL of AO monomer was added and N was added 2 Sealing and placing under ultraviolet light after 5 min, irradiating for 2h under stirring, separating black microspheres with magnet after copolymerization reaction is completed, repeatedly washing with ethanol and water, and freeze-drying at 50 ℃ to constant weight to obtain the enhanced magnetic adsorbent, which is marked as PFSC.
The scanning electron microscope image of the PFSC is shown in fig. 1, and has a spherical shape, and the surface is rough and uneven, which contributes to the collision probability between the adsorbing material and the pollutant. Fe 3 O 4 、Fe 3 O 4 @ SiO 2 The hysteresis loops of (FS), magnetic chitosan beads (FSC) and enhanced magnetic adsorbents (PFSC) are shown in FIG. 2. The hysteresis loop in FIG. 2 shows that Fe 3 O 4 Nanoparticles, Fe 3 O 4 @ SiO 2 The saturation magnetizations of (FS), magnetic chitosan microspheres (FSC) and enhanced magnetic adsorbents (PFSC) were 84.11 meu/g, 73.46 meu/g, 15.92 emu/g and 12.03 emu/g. Although the saturation magnetization decreases with the introduction of chitosan and AO monomers, the relatively high saturation magnetization has enabled the separation and regeneration of the magnetic adsorbent.
Example 2
The difference between the preparation method in this example and example 1 is: the mass of initiator VA-044 in step S3 was 0.0275 g, and the volume of AO monomer was 5 mL. The resulting enhanced magnetic adsorbent was designated PFSC 1.
Example 3
The difference between the preparation method in this example and example 1 is: the initiator VA-044 in step S3 had a mass of 0.0775 g and a volume of AO of 15 mL. The resulting enhanced magnetic adsorbent was designated PFSC 3.
And secondly, testing the adsorption performance.
1. The effect of the amount added on the removal of the dye.
Preparing 1000mg/L orange II (OG), 1000mg/L acid red 88 (AE) and 800mg/L amaranth (RM) solution, and adjusting the pH value of the solution to 7.0. Taking 25 mL of each solution in an erlenmeyer flask, carrying out parallel experiments on three groups, adding PFSC adsorbing material in one group, PFSC1 adsorbing material in the other group, and PFSC3 adsorbing material in the third group, wherein the adding amount of the adsorbing agent is respectively 0.25 g/L, 0.5 g/L, 0.75 g/L, 1.0 g/L, 1.25 g/L and 1.5 g/L, placing the erlenmeyer flask in a constant-temperature water bath shaking box at 25 ℃, measuring the concentration of the solution in the erlenmeyer flask after 24 hours, and calculating the removal rate.
The adsorption data are shown in FIG. 3 (a), (b), and (c). As can be seen from the figure, the adsorption performance of PFSC, PFSC1 and PFSC3 on three anionic azo dyes is obviously superior to that of the unmodified chitosan-based magnetic adsorbent FSC, and the PFSC has the best adsorption effect. When the adding amount is 1 g/L, the PFSC adsorption effect is best, and the removal rates of OG, AE and RM reach 98.62%, 99.51% and 61.25% respectively.
2. The effect of pH on dye removal.
Preparing 1200mg/L orange II (OG), 1200mg/L acid red 88 (AE) and 1000mg/L amaranth (RM) solutions, taking 25 mL of each solution in an erlenmeyer flask, carrying out parallel experiments on two groups, adding 25mg of FSC adsorbing material into one group and 25mg of PFSC adsorbing material into the other group, adjusting the pH value of each group of solutions to be 3, 4, 5, 6, 7, 8, 9 and 11, placing the erlenmeyer flask in a constant-temperature water bath shaking box at 25 ℃, measuring the concentration of the solution in the erlenmeyer flask after 24 hours, and calculating the removal rate. The adsorption data are shown in fig. 4 (a), (b), and (c). As can be seen from the figure, the removal rates of the FSC and PFSC for the three dyes are continuously reduced as the pH value is increased from 3.0 to 11.0, the adsorption performance of the PFSC for the three dyes is obviously better than that of the unmodified chitosan-based magnetic adsorbent FSC, and the maximum removal efficiency of the PFSC for OG, AE and RM is 83.54%, 97.66% and 50.00% respectively at the pH value of 3.0.
3. Reuse test of PFSC.
Preparing 1000mg/L orange II (OG), 1000mg/L acid red 88 (AE) and 800mg/L amaranth (RM) solution, and adjusting the pH value of the solution to 7.0. Taking 25 mL of each solution, adding 25mg of PFSC adsorbing material into an erlenmeyer flask, adjusting the pH value of the solution to 3.0, placing the erlenmeyer flask into a constant-temperature water bath shaking box at 25 ℃, measuring the concentration of the solution in the erlenmeyer flask after 24 hours, and calculating the removal rate. The adsorbent was then separated using a magnet, mixed with 25 ml of NaOH (0.10mol/L) and shaken at 150 rpm for 12h to complete the regeneration process. Thereafter, PFSC was isolated and washed with ultrapure water until pH =7.0 for subsequent reabsorption experiments. The adsorption-desorption cycle was repeated 4 times. Repeated adsorption data as shown in figure 5, the adsorption capacity of PFSC decreased slightly with increasing number of repeated uses. After four cycles, the removal rates of OG, AE and RM are respectively reduced from 83.54%, 97.66% and 40.05% to 80.10%, 91.85% and 28.52%. The reduction in removal rate may be due to incomplete washing of the dye during the previous adsorption stage. It can be seen that the PFSC is renewable after simple acid-base treatment and has excellent recyclability.
It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that the technical solutions of the present invention can be modified or substituted with equivalent solutions without departing from the spirit and scope of the technical solutions, and all should be covered in the claims of the present invention.
Claims (6)
1. The enhanced magnetic adsorbent is characterized by being prepared by the following steps:
s1, mixing Fe 3 O 4 Adding magnetic nanoparticles into ethanol solution, adding ammonia water solution and distilled water after ultrasonic dispersion, adding TEOS (tetraethyl orthosilicate) dropwise after ultrasonic dispersion, and obtaining SiO after reaction 2 Coated Fe 3 O 4 Magnetic nanoparticles of Fe 3 O 4 @SiO 2 ；
S2, dissolving chitosan in acetic acid with the mass fraction of 1% to obtain a chitosan solution, and adding Fe 3 O 4 @SiO 2 Stirring the nano particles to obtain a suspension, dispersing the suspension in a mixed solution of cyclohexane and span80 to obtain an oil-water suspension, and finally dripping a glutaraldehyde solution with the mass fraction of 50% to obtain a magnetic chitosan microsphere solution;
s3, filling N into the magnetic chitosan microsphere dispersion liquid 2 Then adding initiator VA-044 and mixing uniformlyHomogenizing and refilling N 2 Adding cationic monomer, and finally filling N 2 Sealing and placing under ultraviolet light to initiate copolymerization, and obtaining the enhanced magnetic adsorbent after the reaction is finished;
the cationic monomer is acryloyloxyethyl dimethyl benzyl ammonium chloride.
2. The enhanced magnetic adsorbent of claim 1, wherein in step S1, Fe 3 O 4 The mass-volume ratio of the ammonia water to the TEOS is 1 g: 10-12 mL: 4.5-5.5 mL.
3. The enhanced magnetic adsorbent of claim 1, wherein in step S2, chitosan and Fe 3 O 4 @SiO 2 The mass ratio of (1): 0.45 to 0.5; the mass-volume ratio of the chitosan to the cyclohexane, the span80 and the glutaraldehyde is 1 g: 75-80 mL: 0.5-0.6 mL: 0.25-0.3 mL.
4. The enhanced magnetic adsorbent of claim 1, wherein in step S2, the chitosan solution has a mass concentration of 3.75%.
5. The enhanced magnetic adsorbent according to claim 1, wherein in the step S3, the mass ratio of the initiator VA-044 to the magnetic chitosan microspheres is 0.055-0.135: 1; the mass-to-volume ratio of the magnetic chitosan microspheres to the cationic monomers is 1 g: 10-30 mL.
6. The enhanced magnetic adsorbent of claim 1, wherein the irradiation of ultraviolet light in S3 is performed for 1-3 h, and the reaction vessel is placed on a rotating platform with a rotation speed of 8 rpm, so that the mixture receives ultraviolet light periodically.
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| CN113233563A (en) * | 2021-03-17 | 2021-08-10 | 重庆大学 | Preparation method and application of cationic chitosan-based magnetic flocculant initiated by low-pressure ultraviolet light |
| CN113121840B (en) * | 2021-04-16 | 2022-04-22 | 安徽工业大学 | Magnetic covalent bond type chitosan-based modified flocculant and preparation method and application thereof |
| CN114231519B (en) * | 2021-11-28 | 2023-12-15 | 中国人民解放军军事科学院军事医学研究院 | Enrichment method of viscous substance holdfast based on magnetic microsphere co-culture |
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| CN104671383A (en) * | 2015-02-10 | 2015-06-03 | 徐州工程学院 | Dicyandiamide-glyoxal-cationic etherified starch composite flocculant and preparation method of composite flocculant |
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