CN110368916B - Heavy metal composite adsorption material and preparation method and application thereof - Google Patents
Heavy metal composite adsorption material and preparation method and application thereof Download PDFInfo
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- CN110368916B CN110368916B CN201910811216.9A CN201910811216A CN110368916B CN 110368916 B CN110368916 B CN 110368916B CN 201910811216 A CN201910811216 A CN 201910811216A CN 110368916 B CN110368916 B CN 110368916B
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- 239000000463 material Substances 0.000 title claims abstract description 33
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 21
- 239000002905 metal composite material Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 52
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 52
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 52
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 52
- 229960004853 betadex Drugs 0.000 claims abstract description 52
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 42
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010457 zeolite Substances 0.000 claims abstract description 42
- 239000000017 hydrogel Substances 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 239000000178 monomer Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 3
- 239000000945 filler Substances 0.000 claims abstract description 3
- 239000003999 initiator Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 2
- 229920006322 acrylamide copolymer Polymers 0.000 claims 1
- 229910052770 Uranium Inorganic materials 0.000 abstract description 19
- 238000000034 method Methods 0.000 abstract description 10
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 abstract description 6
- 239000010865 sewage Substances 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- -1 uranium ions Chemical class 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- 239000003463 adsorbent Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- WYICGPHECJFCBA-UHFFFAOYSA-N dioxouranium(2+) Chemical compound O=[U+2]=O WYICGPHECJFCBA-UHFFFAOYSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010364 biochemical engineering Methods 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- VBWSWBQVYDBVGA-NAHFVJFTSA-N uranium-234;uranium-235;uranium-238 Chemical compound [234U].[235U].[238U] VBWSWBQVYDBVGA-NAHFVJFTSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
-
- 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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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3028—Granulating, agglomerating or aggregating
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a novel heavy metal composite adsorption material and a preparation method thereof, wherein the heavy metal composite adsorption material is beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel prepared by taking beta-cyclodextrin and acrylic acid monomers as raw materials, artificial zeolite as a filler, N, N' -methylene bisacrylamide as a cross-linking agent and potassium persulfate as an initiator. The composite hydrogel can effectively adsorb heavy metal ions such as uranium and the like so as to achieve the purpose of reasonably treating sewage, and has the advantages of simple synthesis process, low raw material cost, simple adsorption operation steps, wide application prospect and capability of meeting the requirement of rapidly developing sewage treatment.
Description
Technical Field
The invention relates to the field of biochemical engineering, in particular to preparation of beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel and application thereof in heavy metal adsorption.
Background
In recent years, the use of heavy metals has increased with the rapid development of industry, but their unlimited discharge has led to an increase in the metallic substances in the environment. Uranium is currently the primary fuel for most commercial reactors, and the discharge of large amounts of radioactive uranium-containing wastewater into the environment poses a long-term threat to humans and the environment, and therefore, the removal and recovery of uranium from wastewater is an extremely urgent problem.
At present, a plurality of technologies such as ion exchange, solvent extraction, reverse osmosis, membrane filtration and chemical precipitation methods are used for removing uranium from aqueous solution and wastewater. The adsorption method is an important physical and chemical method in the application of heavy metal industrial wastewater treatment, and is widely used due to the advantages of low cost, good effect, high adsorption speed, recyclable adsorbent and the like.
The composite gel material overcomes the defects of natural materials, plays a key role in realizing low-cost and high-efficiency adsorption, and provides a feasible thought and a feasible research direction for preparing novel materials. In addition, multiple groups act together, and the structure of the inorganic material can be used as a physical adsorption binding point, so that the adsorption capacity of the material is greatly improved. Therefore, the method combines natural materials and synthetic polymer materials, and has important research significance and market prospect in developing composite polymer gel materials.
Disclosure of Invention
The invention aims to provide a heavy metal composite adsorption material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a heavy metal composite adsorption material is characterized in that beta-cyclodextrin and acrylic acid monomers are used as raw materials, artificial zeolite is used as a filler, N, N' -methylene bisacrylamide is used as a cross-linking agent, potassium persulfate is used as an initiator, and water-insoluble beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel is rapidly synthesized.
The preparation method of the heavy metal composite adsorption material comprises the steps of dissolving beta-cyclodextrin in 10mol/L sodium hydroxide solution, adding artificial zeolite, stirring for 1 hour, adding a mixed solution containing acrylic acid monomers and N, N' -methylene bisacrylamide, uniformly stirring, reacting in a water bath at 50 ℃ for 1 hour, adding potassium persulfate, uniformly stirring, reacting in a water bath at 50-70 ℃ for 2-3 hours, and freeze-drying a product to obtain the heavy metal composite adsorption material.
The raw materials are as follows by weight percent: 14-18% of beta-cyclodextrin, 10% of sodium hydroxide, 1-20% of artificial zeolite, 60-70% of acrylic monomer, 1.5-3.0% of N, N' -methylene bisacrylamide and 0.1-0.5% of potassium persulfate, wherein the sum of the weight percentages of the raw materials is 100%.
In the polymerization reaction, a C-C single bond can be formed among acrylic monomers, and the hydroxyl of beta-cyclodextrin can form an ester bond with the carboxyl of acrylic acid, so that the obtained heavy metal composite adsorption material contains a large amount of carboxyl and hydroxyl. The existence of carboxyl and hydroxyl active groups can effectively combine heavy metal ions on the active groups through ion exchange or chelation, thereby achieving the effect of well adsorbing the heavy metal ions.
The preparation method of the heavy metal composite adsorption material is simple, the operability is strong, the raw materials are easy to purchase, the price is low, the formed hydrogel has high adsorption activity, and the heavy metals in the sewage can be quickly and effectively removed, so that the requirement of quickly developing sewage treatment can be met.
Drawings
FIG. 1 is an XRD crystal structure analysis chart of different materials, wherein a is beta-cyclodextrin/acrylic acid, b is beta-cyclodextrin/acrylic acid/artificial zeolite, and c is artificial zeolite.
Fig. 2 is a thermogravimetric analysis of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite and b is a beta-cyclodextrin/acrylic acid/artificial zeolite-uranium complex.
Fig. 3 is FTIR spectra of different materials, wherein a is β -cyclodextrin/acrylic acid/artificial zeolite-uranium complex, b is β -cyclodextrin/acrylic acid/artificial zeolite, c is β -cyclodextrin/acrylic acid, and d is artificial zeolite.
Fig. 4 is SEM topography of different materials, where a is beta-cyclodextrin/acrylic acid/artificial zeolite and b is a beta-cyclodextrin/acrylic acid/artificial zeolite-uranium complex.
Fig. 5 is a surface elemental analysis chart of EDX of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is a beta-cyclodextrin/acrylic acid/artificial zeolite-uranium complex.
FIG. 6 is a graph showing the effect of pH on adsorption.
FIG. 7 is a graph of the effect of different materials on adsorption at different initial concentrations, where a is beta-cyclodextrin/acrylic acid/artificial zeolite and b is beta-cyclodextrin/acrylic acid.
FIG. 8 is a graph showing the effect of temperature on adsorption.
Detailed Description
The invention provides a preparation method of a heavy metal composite adsorption material, which is mainly used for synthesizing beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel capable of removing heavy metal ions in sewage, and comprises the following specific preparation steps: dissolving 1.5g of beta-cyclodextrin in 10mol/L solution containing 1.0g of sodium hydroxide, adding 1.0g of artificial zeolite, stirring for 1h, adding a mixed solution containing 6.3g of acrylic acid monomer and 0.18g N, N' -methylene bisacrylamide, uniformly stirring, reacting for 1h in a water bath at 50 ℃, adding 0.02g of potassium persulfate, uniformly stirring, reacting for 2-3h in a water bath at 50-70 ℃, after the polymerization reaction is finished, cutting the hydrogel, drying in a freeze dryer for 24h, and then placing in an oven at 50 ℃ for storage.
The microstructure and chemical composition of the beta-cyclodextrin/acrylic acid/artificial zeolite composite was characterized using fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), energy dispersive X-ray (EDX), and X-ray diffraction (XRD).
FIG. 1 is an XRD crystal structure analysis chart of different materials, wherein a is beta-cyclodextrin/acrylic acid, b is beta-cyclodextrin/acrylic acid/artificial zeolite, and c is artificial zeolite. Comparing the patterns of beta-cyclodextrin/acrylic acid and beta-cyclodextrin/acrylic acid/artificial zeolite, it can be seen that the characteristic diffraction peak of the artificial zeolite appears in the beta-cyclodextrin/acrylic acid/artificial zeolite, which indicates that the hydrogel material is successfully prepared.
FIG. 2 is a thermogravimetric analysis of different materials, wherein a is beta-cyclodextrin/acrylic acid/synthetic zeolite and b is beta-cyclodextrin/acrylic acid. As can be seen from the figure, the thermal stability of the hydrogel adsorption material was significantly improved after the addition of the artificial zeolite.
Fig. 3 is FTIR spectra of different materials, wherein a is β -cyclodextrin/acrylic acid/artificial zeolite-uranium complex, b is β -cyclodextrin/acrylic acid/artificial zeolite, c is β -cyclodextrin/acrylic acid, and d is artificial zeolite. As can be seen, the beta-cyclodextrin/acrylic acid ranges between 1658 and 1254 cm-1Peaks at (a) are C = O and C-O-C bonds of the ester group; after the artificial zeolite was introduced, the resulting beta-cyclodextrin/acrylic acid/artificial zeolite was found to be 1030 cm-1A new peak appears, which may be the (Si, Al) -O asymmetric stretching vibration of the artificial zeolite; after adsorbing the uranium ions, the β -cyclodextrin/acrylic acid/artificial zeolite-uranium complex shows a characteristic peak with O = U = O group.
Fig. 4 is SEM topography of different materials, where a is beta-cyclodextrin/acrylic acid/artificial zeolite and b is a beta-cyclodextrin/acrylic acid/artificial zeolite-uranium complex. As can be seen, the surface of the beta-cyclodextrin/acrylic acid/artificial zeolite is irregularly shaped and fills many pores; after uranium ions are adsorbed, the surface of the uranium ions becomes smooth, and the rough holes are filled with flocculent substances.
Fig. 5 is a surface elemental analysis chart of EDX of different materials, wherein a is beta-cyclodextrin/acrylic acid/artificial zeolite, and b is a beta-cyclodextrin/acrylic acid/artificial zeolite-uranium complex. As can be seen from the figure, the beta-cyclodextrin/acrylic acid/artificial zeolite shows the characteristic elements (Si, Al and Mg) of the artificial zeolite; after adsorbing uranium, the surface of the uranium coated composite material is added with U elements, which shows that uranium ions are adsorbed on the surface of CAP hydrogel, and proves that CAP has a good adsorption effect on the uranium ions.
The present invention is further described below in terms of several specific examples thereof, but the present invention is not limited thereto.
Example 1
And (3) putting 10mg of dried beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel into uranyl ion solutions with different pH values and 500mg/L for adsorption research. The concentration of azoarsine III is measured by an ultraviolet spectrophotometer at the wavelength of 650nm by taking the azoarsine III as a complexing agent.
Wherein q iseRepresents adsorption capacity, ceAnd c0Respectively, the equilibrium and initial concentrations, m represents the mass of the adsorbent material and V represents the volume of the adsorbent solution.
As shown in fig. 6, the pH increased from 2 to 3.5, and the adsorption capacity of the β -cyclodextrin/acrylic acid/artificial zeolite composite hydrogel for uranyl ions gradually increased. When the pH value is increased to 4.5, the adsorption amount of the uranyl ions is almost kept unchanged and reaches an equilibrium, and when the pH value is more than 4.5, the adsorption amount of the uranyl ions is rapidly reduced. The adsorption amount is different under different pH conditions, and the maximum adsorption amount is 730.26 mg/g.
Example 2
The procedure of example 1 was followed to examine the effect of different initial concentrations of 20mL uranyl ion solutions at pH 4.0-4.5 and temperature 25 ℃ on the adsorption process.
As shown in fig. 7, when the initial concentration is greater than 800mg/L, the adsorption capacity of the beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel to uranyl ions can reach a maximum value of 797.37mg/g, which is higher than that of beta-cyclodextrin/acrylic acid, and thus the beta-cyclodextrin/acrylic acid composite hydrogel is proved to be capable of effectively removing the uranyl ions in the solution.
Example 3
The procedure of example 1 was followed using 500mg/L uranyl ion solution at different temperatures and pH 4.0-4.5 to study the effect of temperature on the adsorption process.
As shown in fig. 8, as the temperature increases, the adsorption amount of uranyl ions by the adsorbent increases, and therefore the adsorption process of uranyl ions by the adsorbent is endothermic.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (1)
1. A preparation method of a heavy metal composite adsorption material is characterized by comprising the following steps: the heavy metal composite adsorption material is beta-cyclodextrin/acrylic acid/artificial zeolite composite hydrogel which is quickly synthesized by taking beta-cyclodextrin and acrylic acid monomers as raw materials, artificial zeolite as a filler, N, N' -methylene bisacrylamide as a cross-linking agent and potassium persulfate as an initiator;
dissolving beta-cyclodextrin in 10mol/L sodium hydroxide solution, adding artificial zeolite, stirring for 1h, adding a mixed solution containing an acrylic acid monomer and N, N' -methylene bisacrylamide, uniformly stirring, reacting for 1h in a water bath at 50 ℃, adding potassium persulfate, uniformly stirring, reacting for 2-3h in a water bath at 50-70 ℃, and freeze-drying a product to obtain the beta-cyclodextrin-N-methyl-acrylamide copolymer;
the raw materials are as follows by weight percent: 14-18% of beta-cyclodextrin, 10% of sodium hydroxide, 1-20% of artificial zeolite, 60-70% of acrylic monomer, 1.5-3.0% of N, N' -methylene bisacrylamide and 0.1-0.5% of potassium persulfate, wherein the sum of the weight percentages of the raw materials is 100%.
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