CN111410718A - Manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption and preparation method thereof - Google Patents

Manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption and preparation method thereof Download PDF

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CN111410718A
CN111410718A CN202010333424.5A CN202010333424A CN111410718A CN 111410718 A CN111410718 A CN 111410718A CN 202010333424 A CN202010333424 A CN 202010333424A CN 111410718 A CN111410718 A CN 111410718A
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胡万平
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Abstract

The invention relates to the technical field of sewage treatment, and discloses manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption which comprises the following formula raw materials and components of nano manganese-zinc ferrite grafted cyclodextrin, ammonium persulfate, methacrylic acid and N, N' -methylene bisacrylamide.

Description

Manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption and preparation method thereof
Technical Field
The invention relates to the technical field of sewage treatment, in particular to manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption and a preparation method thereof.
Background
In recent years, the problem of water pollution in China is becoming more severe, water shortage and health problems caused by water pollution are continuously caused, the water pollution is mainly caused by domestic sewage, industrial wastewater, agricultural sewage and the like which are discharged without being treated, and the pollutants mainly comprise heavy metal compounds such as copper, mercury, chromium and the like and ions thereof, and organic pollutants such as organic dyes, halides, organic solvents and the like.
At present, the sewage treatment method mainly comprises a physical adsorption method, a chemical oxidation method, a biodegradation method and the like, the physical adsorption material mainly comprises an activated carbon material, polyacrylamide, a zeolite molecular sieve and the like, the polyacrylic acid hydrogel material is a three-dimensional network structure gel with strong hydrophilicity, contains rich carboxyl groups, can perform a complexing action with heavy metal ions such as chromium and the like, and organic dyes such as rhodamine B and the like, can play a good adsorption role, is a sewage treatment adsorption material with huge potential, and can be added with active adsorption groups such as β -cyclodextrin, sodium alginate and the like and magnetic substances such as ferroferric oxide, manganese zinc ferrite and the like through a physical blending method to enhance the adsorption performance and the magnetic adsorption effect of the polyacrylic acid hydrogel, but the physical blending method can cause that β -cyclodextrin, manganese zinc ferrite and polyacrylic acid hydrogel are not firmly combined, and can cause β -cyclodextrin and manganese zinc ferrite to separate out of the polyacrylic acid hydrogel matrix in a complex and flowing water body environment, thereby reducing the adsorption performance of the material and causing secondary pollution.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption and a preparation method thereof, and solves the problem that β -cyclodextrin, manganese-zinc ferrite and polyacrylic acid hydrogel are not firmly combined and can be separated from a hydrogel matrix.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption material comprises the following raw materials and components: the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 20-50:1-2:100: 5-15.
Preferably, the preparation method of the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel through adsorption comprises the following steps:
(1) adding an ethylene glycol solvent, ferric sulfate, zinc sulfate and manganese sulfate into a reaction bottle, uniformly stirring at 50-70 ℃ for 30-60min, adding sodium hydroxide to adjust the pH value of the solution to 10-11, adding 1, 6-hexanediamine, uniformly stirring, pouring the solution into a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a reaction kettle heater, heating to 150 ℃ and 170 ℃, reacting for 10-15h, filtering the solution to remove the solvent, washing the solid product with deionized water and ethanol, and drying to prepare the aminated nano manganese-zinc ferrite, wherein the molecular formula of the manganese-zinc ferrite is Mn0.6Zn0.4Fe2O4。
(2) Adding a deionized water solvent, amino β -cyclodextrin, aminated nano manganese-zinc ferrite and a cross-linking agent glutaraldehyde into a reaction bottle, ultrasonically dispersing uniformly, then stirring at a constant speed at 40-80 ℃ for reaction for 6-12h, placing the solution into an ice water bath, adding deionized water until a large amount of precipitate is separated out, filtering to remove the solvent, washing with deionized water and ethanol, and drying to prepare the nano manganese-zinc ferrite grafted cyclodextrin.
(3) Introducing nitrogen into a reaction bottle, adding a deionized water solvent and the nano manganese-zinc ferrite grafted cyclodextrin, ultrasonically dispersing uniformly, adding ammonium persulfate at the temperature of 60-70 ℃, stirring and activating at a constant speed for 20-40min, adding methacrylic acid and a crosslinking agent N, N' -methylenebisacrylamide, heating to 75-85 ℃, stirring and reacting at a constant speed for 4-8h, centrifugally separating and washing by using deionized water and ethanol until supernatant is clear, and dialyzing and removing impurities from a solid product to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel for adsorption.
Preferably, the mass ratio of the ferric sulfate, the zinc sulfate, the manganese sulfate and the 1, 6-hexamethylene diamine in the step (1) is 2-2.5:0.4:0.6: 8-12.
Preferably, the reation kettle heater in step (1) includes constant temperature heating ware, the inside below fixedly connected with circulator of reation kettle heater, the inside swing joint of circulator has bearing, bearing and rotation axis swing joint, rotation axis top fixedly connected with base, and the base top is provided with the reaction bulb, base top fixedly connected with bracing piece, bracing piece swing joint have the governing valve, governing valve swing joint have adjust the pole, adjust pole fixedly connected with limiting plate.
Preferably, the mass ratio of the amino β -cyclodextrin to the aminated nano manganese-zinc ferrite to the glutaraldehyde in the step (1) is 100:15-35: 70-120.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the manganese-zinc-ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption is characterized in that a hot solvent method is adopted, the pH value of a solution is adjusted, 1, 6-hexamethylene diamine is used as a surface modifier, aminated nano manganese-zinc ferrite grafted on the surface of 1, 6-hexamethylene diamine is controllably synthesized, the magnetic performance of the nano manganese-zinc ferrite is much higher than that of ferrites such as traditional ferroferric oxide, glutaraldehyde is used as a cross-linking agent, the aminated nano manganese-zinc ferrite and amino β -cyclodextrin are subjected to cross-linking reaction to obtain nano manganese-zinc-ferrite grafted cyclodextrin, ammonium persulfate is used as an initiator to promote β -cyclodextrin to generate active free radicals, methacrylic acid free radical polymerization is initiated in situ, manganese-zinc-ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption is formed under the cross-linking effect of N, N' -methylene bisacrylamide, the nano manganese-zinc-ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption is introduced into a molecular chain of polyacrylic acid through chemical bond covalent modification, the nano manganese-zinc-ferrite and amino β -cyclodextrin are added, the binding capacity of the nano manganese-zinc-ferrite grafted cyclodextrin and the polyacrylic acid hydrogel are hardly separated, the magnetic performance of the nano manganese-zinc-ferrite grafted hydrogel and the amino group-acrylic acid hydrogel is endowed with excellent magnetic performance, and the amino group-hydroxyl group adsorption material is remarkably enhanced.
Drawings
FIG. 1 is a schematic front view of a reactor heater;
FIG. 2 is an enlarged schematic view of the base;
fig. 3 is a limiting plate adjustment schematic.
1-a reactor heater; 2-constant temperature heater; 3-a rotator; 4-a bearing; 5-a rotating shaft; 6-a base; 7-reaction flask; 8-a support bar; 9-adjusting valve; 10-adjusting the rod; 11-limiting plate.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption material comprises the following raw materials and components: the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 20-50:1-2:100: 5-15.
The preparation method of the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption comprises the following steps:
(1) adding glycol solvent, ferric sulfate, zinc sulfate and manganese sulfate into a reaction bottle, uniformly stirring for 30-60min at 50-70 ℃, adding sodium hydroxide to adjust the pH value of the solution to 10-11, and then adding 1, 6-hexanediamine, wherein the mass ratio of the ferric sulfate, the zinc sulfate, the manganese sulfate and the 1, 6-hexanediamine is 2-2.5: 0.6:8-12, uniformly stirring, pouring the solution into a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a reaction kettle heater, wherein the reaction kettle heater comprises a constant temperature heater, a rotator is fixedly connected below the inner part of the reaction kettle heater, a bearing is movably connected inside the rotator and is movably connected with a rotating shaft, a base is fixedly connected above the rotating shaft, the reaction bottle is arranged above the base, a support rod is fixedly connected above the base, an adjusting valve is movably connected with the support rod, an adjusting rod is movably, Adjusting a rod fixedly connected with a limiting plate, heating to 150-0.6Zn0.4Fe2O4。
(2) Adding a deionized water solvent, amino β -cyclodextrin, aminated nano manganese-zinc ferrite and a cross-linking agent glutaraldehyde into a reaction bottle, performing ultrasonic dispersion uniformly, then performing uniform stirring reaction at 40-80 ℃ for 6-12h, placing the solution into an ice water bath, adding deionized water until a large amount of precipitate is separated out, filtering to remove the solvent, washing with deionized water and ethanol, and drying to obtain the nano manganese-zinc ferrite grafted cyclodextrin.
(3) Introducing nitrogen into a reaction bottle, adding a deionized water solvent and the nano manganese-zinc ferrite grafted cyclodextrin, ultrasonically dispersing uniformly, adding ammonium persulfate at the temperature of 60-70 ℃, stirring and activating at a constant speed for 20-40min, adding methacrylic acid and a crosslinking agent N, N' -methylenebisacrylamide, heating to 75-85 ℃, stirring and reacting at a constant speed for 4-8h, centrifugally separating and washing by using deionized water and ethanol until supernatant is clear, and dialyzing and removing impurities from a solid product to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel for adsorption.
Example 1
(1) Adding glycol solvent, ferric sulfate, zinc sulfate and manganese sulfate into a reaction bottle, stirring at 50 ℃ for 30min at constant speed, adding sodium hydroxide to adjust the pH value of the solution to 10, adding 1, 6-hexanediamine, wherein the mass ratio of the ferric sulfate, the zinc sulfate, the manganese sulfate and the 1, 6-hexanediamine is 2:0.4:0.6:8, pouring the solution into a hydrothermal reaction kettle after uniformly stirring, placing the hydrothermal reaction kettle in a reaction kettle heater, wherein the reaction kettle heater comprises a constant temperature heater, a rotator is fixedly connected below the inner part of the reaction kettle heater, a bearing is movably connected inside the rotator and movably connected with a rotating shaft, a base is fixedly connected above the rotating shaft, the reaction bottle is arranged above the base, a supporting rod is fixedly connected above the base, an adjusting valve is movably connected with the supporting rod, and a limiting plate is fixedly connected with the adjusting, heating to 150 ℃, reacting for 10h, filtering the solution to remove the solvent, washing the solid product with deionized water and ethanol, and drying to obtain the aminated nano manganese-zinc ferrite, wherein the molecular formula of the manganese-zinc ferrite is Mn0.6Zn0.4Fe2O4。
(2) Adding a deionized water solvent, amino β -cyclodextrin, aminated nano manganese-zinc ferrite and a cross-linking agent glutaraldehyde into a reaction bottle, uniformly dispersing by ultrasonic, uniformly stirring at a constant speed at 40 ℃ for reaction for 6 hours, placing the solution into an ice water bath, adding deionized water until a large amount of precipitate is separated out, filtering to remove the solvent, washing with deionized water and ethanol, and drying to prepare the nano manganese-zinc ferrite grafted cyclodextrin.
(3) Introducing nitrogen into a reaction bottle, adding a deionized water solvent and the nano manganese-zinc ferrite grafted cyclodextrin, ultrasonically dispersing uniformly, adding ammonium persulfate at 60 ℃, stirring at a constant speed for activation for 20min, adding methacrylic acid and a crosslinking agent N, N '-methylene bisacrylamide, wherein the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 20:1:100:5, heating to 75 ℃, stirring at a constant speed for reaction for 4h, centrifugally separating and washing by using deionized water and ethanol until supernatant liquid is clear, and dialyzing and removing impurities from a solid product to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption 1.
Example 2
(1) Adding glycol solvent, ferric sulfate, zinc sulfate and manganese sulfate into a reaction bottle, stirring at a constant speed of 70 ℃ for 40min, adding sodium hydroxide to adjust the pH value of the solution to 11, adding 1, 6-hexanediamine, wherein the mass ratio of the ferric sulfate, the zinc sulfate, the manganese sulfate and the 1, 6-hexanediamine is 2.1:0.4:0.6:9, pouring the solution into a hydrothermal reaction kettle after uniformly stirring, placing the hydrothermal reaction kettle in a reaction kettle heater, wherein the reaction kettle heater comprises a constant temperature heater, a rotator is fixedly connected below the inner part of the reaction kettle heater, a bearing is movably connected inside the rotator and is movably connected with a rotating shaft, a base is fixedly connected above the rotating shaft, the reaction bottle is arranged above the base, a supporting rod is fixedly connected above the base, an adjusting valve is movably connected with the supporting rod, and a limiting plate is fixedly connected with, heating to 170 ℃, reacting for 15h, filtering the solution to remove the solvent, washing the solid product with deionized water and ethanol, and drying to obtain the aminated nano manganese-zinc ferrite, wherein the molecular formula of the manganese-zinc ferrite is Mn0.6Zn0.4Fe2O4。
(2) Adding a deionized water solvent, amino β -cyclodextrin, aminated nano manganese-zinc ferrite and a cross-linking agent glutaraldehyde into a reaction bottle, uniformly dispersing by ultrasonic, uniformly stirring at a constant speed at 80 ℃ for 8 hours to react, putting the solution into an ice water bath, adding deionized water until a large amount of precipitate is separated out, filtering to remove the solvent, washing with deionized water and ethanol, and drying to prepare the nano manganese-zinc ferrite grafted cyclodextrin.
(3) Introducing nitrogen into a reaction bottle, adding a deionized water solvent and the nano manganese-zinc ferrite grafted cyclodextrin, ultrasonically dispersing uniformly, adding ammonium persulfate at 65 ℃, stirring at a constant speed for activation for 30min, adding methacrylic acid and a crosslinking agent N, N '-methylene bisacrylamide, wherein the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 30:1.4:100:8, heating to 85 ℃, stirring at a constant speed for reaction for 8h, centrifugally separating and washing by using deionized water and ethanol until supernatant is clear, and dialyzing and removing impurities from a solid product to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption 2.
Example 3
(1) Adding glycol solvent, ferric sulfate, zinc sulfate and manganese sulfate into a reaction bottle, stirring at a constant speed of 60 ℃ for 45min, adding sodium hydroxide to adjust the pH value of the solution to 11, adding 1, 6-hexanediamine, wherein the mass ratio of the ferric sulfate, the zinc sulfate, the manganese sulfate and the 1, 6-hexanediamine is 2.3:0.4:0.6:10, pouring the solution into a hydrothermal reaction kettle after uniformly stirring, placing the hydrothermal reaction kettle in a reaction kettle heater, wherein the reaction kettle heater comprises a constant temperature heater, a rotator is fixedly connected below the inner part of the reaction kettle heater, a bearing is movably connected inside the rotator and is movably connected with a rotating shaft, a base is fixedly connected above the rotating shaft, the reaction bottle is arranged above the base, a supporting rod is fixedly connected above the base, an adjusting valve is movably connected with the supporting rod, and a limiting plate is fixedly connected with, heating to 160 ℃, reacting for 13h, filtering the solution to remove the solvent, washing the solid product with deionized water and ethanol, and drying to obtain the aminated nano manganese-zinc ferrite, wherein the molecular formula of the manganese-zinc ferrite is Mn0.6Zn0.4Fe2O4。
(2) Adding a deionized water solvent, amino β -cyclodextrin, aminated nano manganese-zinc ferrite and a cross-linking agent glutaraldehyde into a reaction bottle, uniformly dispersing by ultrasonic, uniformly stirring at a constant speed at 60 ℃ for reaction for 10 hours, placing the solution into an ice water bath, adding deionized water until a large amount of precipitate is separated out, filtering to remove the solvent, washing with deionized water and ethanol, and drying to prepare the nano manganese-zinc ferrite grafted cyclodextrin.
(3) Introducing nitrogen into a reaction bottle, adding a deionized water solvent and the nano manganese-zinc ferrite grafted cyclodextrin, ultrasonically dispersing uniformly, adding ammonium persulfate at 65 ℃, stirring at a constant speed for activation for 30min, adding methacrylic acid and a crosslinking agent N, N '-methylene bisacrylamide, wherein the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 40:1.6:100:12, heating to 80 ℃, stirring at a constant speed for reaction for 6h, centrifugally separating and washing by using deionized water and ethanol until supernatant liquid is clear, and dialyzing and removing impurities from a solid product to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption 3.
Example 4
(1) Adding glycol solvent, ferric sulfate, zinc sulfate and manganese sulfate into a reaction bottle, stirring at a constant speed of 70 ℃ for 60min, adding sodium hydroxide to adjust the pH value of the solution to 11, adding 1, 6-hexanediamine, wherein the mass ratio of the ferric sulfate, the zinc sulfate, the manganese sulfate and the 1, 6-hexanediamine is 2.5:0.4:0.6:12, pouring the solution into a hydrothermal reaction kettle after uniformly stirring, placing the hydrothermal reaction kettle in a reaction kettle heater, wherein the reaction kettle heater comprises a constant temperature heater, a rotator is fixedly connected below the inner part of the reaction kettle heater, a bearing is movably connected inside the rotator and is movably connected with a rotating shaft, a base is fixedly connected above the rotating shaft, the reaction bottle is arranged above the base, a supporting rod is fixedly connected above the base, an adjusting valve is movably connected with the supporting rod, and a limiting plate is fixedly connected with, heating to 170 ℃, reacting for 15h, filtering the solution to remove the solvent, washing the solid product with deionized water and ethanol, and drying to obtain the aminated nano manganese-zinc ferrite, wherein the molecular formula of the manganese-zinc ferrite is Mn0.6Zn0.4Fe2O4。
(2) Adding a deionized water solvent, amino β -cyclodextrin, aminated nano manganese-zinc ferrite and a cross-linking agent glutaraldehyde into a reaction bottle, uniformly dispersing by ultrasonic, uniformly stirring at a constant speed at 80 ℃ for reaction for 12 hours, putting the solution into an ice water bath, adding deionized water until a large amount of precipitate is separated out, filtering to remove the solvent, washing with deionized water and ethanol, and drying to prepare the nano manganese-zinc ferrite grafted cyclodextrin.
(3) Introducing nitrogen into a reaction bottle, adding a deionized water solvent and the nano manganese-zinc ferrite grafted cyclodextrin, ultrasonically dispersing uniformly, adding ammonium persulfate at 70 ℃, stirring at a constant speed for activation for 40min, adding methacrylic acid and a crosslinking agent N, N '-methylene bisacrylamide, wherein the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 50:2:100:15, heating to 85 ℃, stirring at a constant speed for reaction for 8h, centrifugally separating and washing by using deionized water and ethanol until supernatant liquid is clear, and dialyzing and removing impurities from a solid product to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption 4.
Comparative example 1
(1) Adding glycol solvent, ferric sulfate, zinc sulfate and manganese sulfate into a reaction bottle, stirring at a constant speed of 70 ℃ for 50min, adding sodium hydroxide to adjust the pH value of the solution to 11, adding 1, 6-hexanediamine, wherein the mass ratio of the ferric sulfate, the zinc sulfate, the manganese sulfate and the 1, 6-hexanediamine is 1.8:0.4:0.6:6, pouring the solution into a hydrothermal reaction kettle after uniformly stirring, placing the hydrothermal reaction kettle in a reaction kettle heater, wherein the reaction kettle heater comprises a constant temperature heater, a rotator is fixedly connected below the inner part of the reaction kettle heater, a bearing is movably connected inside the rotator and is movably connected with a rotating shaft, a base is fixedly connected above the rotating shaft, the reaction bottle is arranged above the base, a supporting rod is fixedly connected above the base, an adjusting valve is movably connected with the supporting rod, and a limiting plate is fixedly connected with, heating to 170 ℃, reacting for 10h, filtering the solution to remove the solvent, washing the solid product with deionized water and ethanol, and drying to obtain the aminated nano manganese-zinc ferrite, wherein the molecular formula of the manganese-zinc ferrite is Mn0.6Zn0.4Fe2O4。
(2) Adding a deionized water solvent, amino β -cyclodextrin, aminated nano manganese-zinc ferrite and a cross-linking agent glutaraldehyde into a reaction bottle, uniformly dispersing by ultrasonic, uniformly stirring at a constant speed at 50 ℃ for reaction for 12 hours, placing the solution into an ice water bath, adding deionized water until a large amount of precipitate is separated out, filtering to remove the solvent, washing with deionized water and ethanol, and drying to prepare the nano manganese-zinc ferrite grafted cyclodextrin.
(3) Introducing nitrogen into a reaction bottle, adding a deionized water solvent and the nano manganese-zinc ferrite grafted cyclodextrin, ultrasonically dispersing uniformly, adding ammonium persulfate at 70 ℃, stirring at a constant speed for activation for 20min, adding methacrylic acid and a crosslinking agent N, N '-methylene bisacrylamide, wherein the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 60:0.6:100:20, heating to 85 ℃, stirring at a constant speed for reaction for 4h, centrifugally separating and washing by using deionized water and ethanol until supernatant is clear, and dialyzing and removing impurities from a solid product to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption comparison material 1.
Respectively adding 2% of Cr3+Adding the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel in the examples and the comparative examples into the solution for adsorption, wherein the mass fraction is 5%, uniformly stirring for 12h for carrying out the adsorption process, and testing Cr by using a TU-1810PC ultraviolet-visible spectrophotometer3+And calculating the adsorption rate, wherein the test standard is GB/T10533-2014.
Figure BDA0002465766810000091
Figure BDA0002465766810000101

Claims (5)

1. The manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption material comprises the following raw materials and components, and is characterized in that: the mass ratio of the nano manganese-zinc ferrite grafted cyclodextrin to the ammonium persulfate to the methacrylic acid to the N, N' -methylene bisacrylamide is 20-50:1-2:100: 5-15.
2. The manganese zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorbent of claim 1, wherein: the preparation method of the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption comprises the following steps:
(1) adding ferric sulfate, zinc sulfate and manganese sulfate into an ethylene glycol solvent, stirring for 30-60min at 50-70 ℃, adding sodium hydroxide to adjust the pH value of the solution to 10-11, adding 1, 6-hexanediamine, stirring uniformly, pouring the solution into a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a reaction kettle heater, heating to 150 ℃ and 170 ℃, reacting for 10-15h, filtering, washing and drying to prepare the aminated nano manganese-zinc ferrite, wherein the molecular formula of the manganese-zinc ferrite is Mn0.6Zn0.4Fe2O4；
(2) Adding amino β -cyclodextrin, aminated nano manganese-zinc ferrite and cross-linking agent glutaraldehyde into deionized water solvent, reacting for 6-12h at 40-80 ℃ after uniform ultrasonic dispersion, cooling, precipitating, filtering, washing and drying to prepare nano manganese-zinc ferrite grafted cyclodextrin;
(3) adding the nano manganese-zinc ferrite grafted cyclodextrin into a deionized water solvent in a nitrogen atmosphere, uniformly dispersing by ultrasonic, adding ammonium persulfate at the temperature of 60-70 ℃, stirring and activating for 20-40min, adding methacrylic acid and a crosslinking agent N, N' -methylene bisacrylamide, heating to 75-85 ℃, reacting for 4-8h, centrifugally separating, washing, dialyzing and removing impurities to prepare the manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel for adsorption.
3. The manganese zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption device according to claim 2, wherein: the mass ratio of ferric sulfate, zinc sulfate, manganese sulfate and 1, 6-hexamethylene diamine in the step (1) is 2-2.5:0.4:0.6: 8-12.
4. The manganese zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption device according to claim 2, wherein: the reaction kettle heater in the step (1) comprises a constant temperature heater, a rotator fixedly connected with the lower portion inside the reaction kettle heater, a bearing movably connected with the inside of the rotator, a bearing movably connected with a rotating shaft, a base fixedly connected with the upper portion of the rotating shaft, a reaction bottle arranged above the base, a supporting rod fixedly connected with the upper portion of the base, a regulating valve movably connected with the supporting rod, a regulating rod movably connected with the regulating valve, and a limiting plate fixedly connected with the regulating rod.
5. The manganese-zinc-ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption method according to claim 2, wherein the mass ratio of amino β -cyclodextrin, aminated nano manganese-zinc-ferrite and glutaraldehyde in step (1) is 100:15-35: 70-120.
CN202010333424.5A 2020-04-24 2020-04-24 Manganese-zinc ferrite grafted cyclodextrin-acrylic acid hydrogel adsorption and preparation method thereof Withdrawn CN111410718A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114702682A (en) * 2022-04-24 2022-07-05 齐鲁工业大学 Preparation method of bifunctional dextrin with high embedding rate and fast absorption

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114702682A (en) * 2022-04-24 2022-07-05 齐鲁工业大学 Preparation method of bifunctional dextrin with high embedding rate and fast absorption
CN114702682B (en) * 2022-04-24 2023-03-14 齐鲁工业大学 Preparation method of bifunctional dextrin with high embedding rate and fast absorption

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Application publication date: 20200714