CN113145180B - Preparation method of magnetic ion exchange resin motor, product and application thereof - Google Patents
Preparation method of magnetic ion exchange resin motor, product and application thereof Download PDFInfo
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- CN113145180B CN113145180B CN202110531369.5A CN202110531369A CN113145180B CN 113145180 B CN113145180 B CN 113145180B CN 202110531369 A CN202110531369 A CN 202110531369A CN 113145180 B CN113145180 B CN 113145180B
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- 239000003456 ion exchange resin Substances 0.000 title claims abstract description 117
- 229920003303 ion-exchange polymer Polymers 0.000 title claims abstract description 117
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000001179 sorption measurement Methods 0.000 claims abstract description 71
- 229920000426 Microplastic Polymers 0.000 claims abstract description 46
- 238000012986 modification Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000004048 modification Effects 0.000 claims abstract description 21
- 239000002122 magnetic nanoparticle Substances 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- 239000011521 glass Substances 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 3
- 230000007480 spreading Effects 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 24
- 238000011084 recovery Methods 0.000 abstract description 10
- 230000002269 spontaneous effect Effects 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 description 63
- 239000004033 plastic Substances 0.000 description 63
- 229920000915 polyvinyl chloride Polymers 0.000 description 21
- 239000004800 polyvinyl chloride Substances 0.000 description 21
- 238000000034 method Methods 0.000 description 18
- 239000004793 Polystyrene Substances 0.000 description 15
- 229920002223 polystyrene Polymers 0.000 description 15
- 239000002105 nanoparticle Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 239000004952 Polyamide Substances 0.000 description 9
- 229920002647 polyamide Polymers 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 7
- 238000007885 magnetic separation Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 229920006395 saturated elastomer Polymers 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000005370 electroosmosis Methods 0.000 description 5
- 238000007747 plating Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 241000251468 Actinopterygii Species 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 3
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 240000000146 Agaricus augustus Species 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920006238 degradable plastic Polymers 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000008621 organismal health Effects 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Images
Classifications
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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
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/016—Modification or after-treatment of ion-exchangers
-
- 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
-
- 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
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/014—Ion-exchange processes in general; Apparatus therefor in which the adsorbent properties of the ion-exchanger are involved, e.g. recovery of proteins or other high-molecular compounds
-
- 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
-
- 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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明公开了一种磁性离子交换树脂马达的制备方法及其产品和应用，所述制备方法包括以下步骤：对离子交换树脂进行磁性修饰即得所述磁性离子交换树脂马达；所述磁性修饰为磁性纳米粒子吸附修饰或金属镀膜修饰；本发明制备得到的磁性离子交换树脂马达分散在微塑料的分散液中时，由于非对称吸附会产生自发的运动，对于水体中的微塑料具有良好的吸附效果；通过对离子交换树脂进行磁性修饰，可方便地对离子交换树脂马达进行磁回收；在微塑料吸附量达到饱和后，通过磁控收集之后向磁性离子交换树脂马达中加入盐溶液，可以使微塑料脱落、重新分散，而离子交换树脂马达可以循环利用。
The invention discloses a preparation method of a magnetic ion exchange resin motor, a product and an application thereof. The preparation method comprises the following steps: performing magnetic modification on an ion exchange resin to obtain the magnetic ion exchange resin motor; and the magnetic modification is: Magnetic nanoparticle adsorption modification or metal coating modification; when the magnetic ion exchange resin motor prepared by the present invention is dispersed in the dispersion liquid of microplastics, due to asymmetric adsorption, spontaneous movement will be generated, and it has good adsorption for microplastics in water. Effect; by magnetically modifying the ion exchange resin, the magnetic recovery of the ion exchange resin motor can be conveniently carried out; after the adsorption capacity of the microplastics reaches saturation, adding a salt solution to the magnetic ion exchange resin motor after the magnetic control collection can make The microplastics are shed and re-dispersed, while the ion-exchange resin motor can be recycled.
Description
Technical Field
The invention belongs to the technical field of micro-plastic treatment, and particularly relates to a preparation method of a magnetic ion exchange resin motor, a product and application thereof.
Background
Since 2004, thompson et al, university of princes, british, published a paper on plastic fragments in marine waters and sediments in journal "science", the concept of "micro-plastics" was first proposed, and micro-plastics began to gain widespread worldwide attention. The harm of the micro plastic is mainly reflected in that the particle size is small, the diameter is generally in the micro-nano level, and the harm degree to the environment is deeper compared with other common non-degradable plastics. The sources of micro plastics are very wide, and various plastics existing in daily life, such as polystyrene, polyvinyl chloride, nylon and the like, cannot be completely degraded in natural environment, but are weathered into smaller-particle plastics. The coastal city ecological influence research center of Sydney university discovers more micro-plastics on the coast of densely populated areas, and identifies an important source, namely wastewater discharged by a household washing machine, a certain amount of micro-plastics can be generated when one piece of clothes is washed, and the natural environment is damaged along with the discharge of the wastewater. The micro plastic can also generate biological hazard, and because the micro plastic can not be degraded and digested, the micro plastic can not be completely discharged or digested when entering the organism, and can remain in the organism for a long time to generate serious influence on the health of the organism, for example, the micro plastic exists in fish bodies, and after people eat the fish, the micro plastic can enter the human bodies, and the harm is generated to the human bodies after the people eat the fish for a long time. At present, the global treatment methods for waste plastics include landfill, incineration, regeneration granulation, pyrolysis and the like. The treated plastics are macroscopic, the methods are not available for treating the micro plastics, but the influence of the micro plastics on the human society is increasing, the micro plastics are concerned by countries all over the world, and at present, no reasonable and effective treatment method exists.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a magnetic ion exchange resin motor, a product and an application thereof, and provides a method for adsorbing micro-plastics based on the magnetic ion exchange resin motor aiming at the defects of the existing micro-plastic treatment method in a water body, wherein the surrounding micro-plastics are brought to the vicinity of the ion exchange resin motor by using the electroosmotic flow generated by the exchange action of the magnetic ion exchange resin motor and impurity ions in the water body, and the micro-plastics are effectively collected by electrostatic adsorption; the motor asymmetrically adsorbing the micro-plastics can perform autonomous movement due to the broken symmetry of the peripheral electroosmotic flow, can improve the adsorption speed of the peripheral micro-plastics, can make the micro-plastics fall off and disperse by adding salt (such as sodium sulfate) with a certain concentration after the adsorption amount of the micro-plastics reaches saturation through magnetic separation, and can be recycled after the magnetic ion exchange resin motor is regenerated by corresponding salt.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a magnetic ion exchange resin motor, which comprises the following steps: carrying out magnetic modification on the ion exchange resin to obtain the magnetic ion exchange resin motor;
the magnetic modification is magnetic nanoparticle adsorption modification or metal coating modification.
Further, the magnetic nanoparticle adsorption modification comprises the following steps: dispersing the magnetic nano particles in water, adding ion exchange resin, and adsorbing to obtain the magnetic ion exchange resin motor.
Further, the magnetic nanoparticles are Fe3O4Or NdFeB.
Furthermore, the dosage ratio of the magnetic nanoparticles to water is 1mg to (1-3) mL; the mass ratio of the ion exchange resin to the magnetic nanoparticles is 50: 1-3.
Further, the adsorption time is 5-10 min.
Further, the metal plating film modification comprises the following steps: dispersing ion exchange resin in water, drying the obtained dispersion liquid, and then carrying out metal plating treatment.
Further, the metal is cobalt or nickel.
Further, the thickness of the metal plating film is 20-40 nm.
The invention also provides the magnetic ion exchange resin motor prepared by the preparation method.
The invention also provides an application of the magnetic ion exchange resin motor in adsorbing micro plastic.
Compared with the prior art, the invention has the following beneficial effects:
the invention can conveniently carry out magnetic recovery on the magnetic ion exchange resin motor by carrying out magnetic modification on the ion exchange resin, and after the adsorption capacity of the micro-plastic reaches saturation, the salt solution is added into the magnetic ion exchange resin motor after the micro-plastic is collected by magnetic control, so that the micro-plastic can fall off and be dispersed again, and the ion exchange resin motor can be recycled.
When the magnetic ion exchange resin motor prepared by the invention is used for adsorbing micro-plastics in a water body, the surrounding micro-plastics are brought to the vicinity of the motor by utilizing electroosmotic flow generated by the exchange action of the magnetic ion exchange resin motor and impurity ions in the water body, and the micro-plastics are effectively collected by electrostatic adsorption; due to the non-uniformity of micro plastic particles and the non-uniformity of dispersion, the adsorption of the magnetic ion exchange resin to the micro plastic is asymmetric adsorption, and the resin asymmetrically adsorbing the micro plastic breaks through the symmetry of the peripheral electroosmotic flow, so that the autonomous movement can be realized, and the adsorption efficiency of the peripheral micro plastic is improved.
The magnetic ion exchange resin motor is used for treating the micro-plastic in the water body, and the method is economic and environment-friendly and has good application prospect in the aspect of micro-plastic treatment in the water body.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a microscopic view of the magnetic ion exchange resin motor prepared in example 3;
FIG. 2 is a microscopic morphology of the magnetic ion exchange resin motor prepared in example 5;
FIG. 3 is a graph showing the adsorption effect of the magnetic ion exchange resin motor prepared in example 3 on an electronegative polyvinyl chloride micro-plastic, wherein a is a microscopic picture and b is a scanning electron microscopic picture;
FIG. 4 is a diagram showing the movement of the magnetic ion exchange resin motor prepared in example 5 during the process of adsorbing the electronegative polyvinyl chloride micro-plastic;
FIG. 5 is a graph showing the hysteresis loop and the magnetic separation and recovery effect before and after the magnetic ion exchange resin motor prepared in example 3 adsorbs the negative polyvinyl chloride micro-plastic;
FIG. 6 is a graph showing the effect of the magnetic ion exchange resin motor prepared in example 3 on the redistribution of the negatively charged polyvinyl chloride microplastics after the motor has adsorbed the negatively charged polyvinyl chloride microplastics;
FIG. 7 is a diagram showing the movement of the magnetic ion exchange resin motor prepared in example 5 during the process of adsorbing the electronegative polystyrene micro-plastic;
FIG. 8 is a graph showing the adsorption effect of the magnetic ion exchange resin motor prepared in example 5 on electronegative polystyrene microplastics, wherein a is a microscopic image and b is a scanning electron microscopic image;
fig. 9a is a statistical graph of the adsorption removal rate of the magnetic ion exchange resin motor prepared in example 3 on polyvinyl chloride microplastic, and fig. 9b is a statistical graph of the adsorption removal rate of the magnetic ion exchange resin motor prepared in example 3 on polystyrene microplastic.
FIG. 10 is a graph showing the effect of the magnetic ion exchange resin motor prepared in example 5 on the adsorption of electronegative polyamide microplastics, wherein a is a microscopic image and b is a scanning electron microscopic image.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The ion exchange resin used in the following examples is (OH)-) Anion exchange resin with 400 mesh pore diameter.
The description will not be repeated below.
Example 1
Magnetic Fe3O4Preparing nano particles: 1.622g of FeCl are weighed3·6H 20 and 1.39g FeSO4·7H2Dissolving O in 40mL of water respectively, mixing the solution in a mixed flask, carrying out ultrasonic treatment to uniformly mix the solution, adding 5mL of 28% ammonia water solution into the mixed solution, heating the mixed solution to 90 ℃, adding 4.4g of sodium citrate into the flask, stirring the mixed solution for 30min, and magnetically recovering Fe after the reaction is finished3O4Washing the nano-particles with ethanol, and drying to obtain magnetic Fe3O4And (3) nanoparticles.
Example 2
Modification of glass culture dish:
(1) firstly, ultrasonically cleaning a glass culture dish for 20min by using acetone, ethanol and deionized water respectively;
(2) soaking the glass culture dish cleaned in the step (1) in a mixed solution of concentrated sulfuric acid and hydrogen peroxide in a volume ratio of 3:1 for 30 min;
(3) taking out the glass culture dish after the soaking treatment in the step (2), and sequentially soaking the glass culture dish into two polyelectrolytes of ammonium dialkylene and sodium polystyrene sulfonate for modification: firstly soaking in a mixed solution containing 2mg/mL of ammonium bifenate and 0.5mol/L of sodium chloride for 5min, then washing with deionized water for 1min, then soaking in a mixed solution containing 3mg/mL of sodium polystyrene sulfonate and 0.5mol/L of sodium chloride for 5min, then washing with deionized water for 1min, and repeating for 25 times.
If the last modification is finished by the ammonium dialkylene, the glass culture dish is modified to be electropositive; if the last modification is finished by sodium polystyrene sulfonate, the glass culture dish is modified to be electronegative.
Example 3
The preparation of the magnetic ion exchange resin motor comprises the following steps:
10mg of Fe are weighed3O4Dispersing the nano particles in 30mL of water, and performing ultrasonic dispersion for 30min to enable the magnetic Fe3O4Dispersing the nanoparticles uniformly, adding 500mg of ion exchange resin into the dispersion, stirring and adsorbing for 5min to make Fe3O4And (3) uniformly adsorbing the nano particles on the surface of the ion exchange resin, and drying to obtain the magnetic ion exchange resin motor.
The microscopic morphology of the resulting magnetic ion exchange resin motor was observed, as shown in fig. 1, and it can be seen from fig. 1 that: the surface of the ion exchange resin is adsorbed with magnetic Fe through adsorption modification3O4Nanoparticles, and magnetic Fe added3O4The nanoparticles are fully adsorbed to the resin surface.
Example 4
The preparation of the magnetic ion exchange resin motor comprises the following steps:
30mg of magnetic Fe was weighed3O4Dispersing the nano particles in 30mL of water, and performing ultrasonic dispersion for 30min to enable the magnetic Fe3O4Dispersing the nanoparticles uniformly, adding 500mg of ion exchange resin into the dispersion, stirring and adsorbing for 10min to make Fe3O4The nano particles are uniformly adsorbed on the surface of the ion exchange resin, the magnetic ion exchange resin motor is obtained after drying, and the added magnetic Fe is obtained through detection3O4The nanoparticles are fully adsorbed to the resin surface.
Example 5
The preparation of the magnetic ion exchange resin motor comprises the following steps:
weighing 500mg of ion exchange resin, dispersing in 25mL of deionized water, spreading 5mL of ion exchange resin dispersion on a cleaned glass sheet, evaporating and drying on a heating table to form a single-layer particle film, and plating a layer of nickel with the thickness of 40nm by using micro-nano vacuum equipment.
The microscopic morphology of the resulting magnetic ion exchange resin motor was observed, as shown in fig. 2, and it can be seen from fig. 2 that: through metal coating, half of the surface of the ion exchange resin is coated with a layer of nickel by evaporation, and the effect of magnetic separation can be achieved.
Example 6
The preparation of the magnetic ion exchange resin motor comprises the following steps:
weighing 500mg of ion exchange resin, dispersing in 25mL of deionized water, spreading 5mL of ion exchange resin dispersion on a cleaned glass sheet, evaporating and drying on a heating table to form a single-layer particle film, and plating a layer of nickel with the thickness of 20nm by using micro-nano vacuum equipment.
Effect verification
1. The magnetic ion exchange resin motors prepared in the examples 3-6 are used for adsorbing electronegative polyvinyl chloride micro-plastics, the particle size range of the polyvinyl chloride micro-plastics is 670-2000 nm, the polyvinyl chloride micro-plastics are prepared into suspension with the concentration of 1g/L, a group A-D4 is set in the experiment, the electronegative glass culture dishes prepared in the example 2 are adopted, 50mL of the polyvinyl chloride micro-plastic suspension is added into each group of the culture dishes, then 30mg of the magnetic ion exchange resin motors prepared in the examples 3-6 are respectively added into the group A-D, and after adsorption is saturated, the adsorption effect is observed, wherein the adsorption effect of the group A, namely the magnetic ion exchange resin motor prepared in the example 3 on the polyvinyl chloride micro-plastics is shown in a microscopic picture and a scanning electron microscopic picture; the movement of the magnetic ion exchange resin motor prepared in example 5 in the process of adsorbing polyvinyl chloride micro plastic in group C is shown in fig. 4. As can be seen from fig. 3, the magnetic ion exchange resin motor prepared in example 3 has a significant adsorption effect on the electronegative polyvinyl chloride micro plastic. The adsorption effect of the magnetic ion exchange resin motors in the groups B to D on the polyvinyl chloride micro-plastic is basically the same as that of the group A.
The ion exchange resin after saturated adsorption in each group is separated and recovered by adopting the magnet, and the ion exchange resin motors in the groups A to D can well realize separation and recovery, wherein the hysteresis loops before and after the group A magnetic ion exchange resin motor adsorbs the micro-plastic and the magnetic separation effect are shown in figure 5, so that the magnetic ion exchange resin motor prepared by the invention can recover the micro-plastic by the magnet after adsorbing the micro-plastic.
And adding a sodium sulfate solution with the concentration of 2mol/L into the magnetic ion exchange resin motors obtained by the recovery of the groups A to D, observing that the micro-plastics adsorbed on the magnetic ion exchange resin motors fall off and are dispersed again, wherein an effect diagram of the magnetic ion exchange resin motors obtained by the recovery of the group A on the micro-plastics re-dispersion is shown in figure 6, so that the recycling of the magnetic ion exchange resin motors can be conveniently realized. The magnetic ion exchange resin motors recovered from each group were again placed in the above-mentioned microplastic solution to continue the adsorption, and the above-mentioned magnetic separation and microplastic desorption processes were repeated for 4 cycles in this manner, and then the adsorption removal rate of polyvinyl chloride microplastic in each group of solutions was measured, and the results are shown in table 1.
TABLE 1
| Group of | Group A | Group B | Group C | Group D |
| Adsorption removal rate/%) | 92.4 | 90.1 | 90.7 | 91.8 |
2. The magnetic ion exchange resin motors prepared in examples 3-6 were used for adsorbing electronegative polystyrene micro-plastics with particle size ranging from 1000-2600 nm, prepared into suspensions with concentration of 1G/L, and tested to set up E-H4 groups, using the electronegative glass culture dishes prepared in example 2, 50mL of the above polystyrene micro-plastic suspension was added to the culture dishes of each group, and then 30mg of the magnetic ion exchange resin motors prepared in examples 3-6 were added to the E-H groups, respectively, and during the adsorption process, the movement of the magnetic ion exchange resin and the adsorption of the micro-plastics were observed, wherein the resin movement and the adsorption effect on the micro-plastics during the adsorption process of the magnetic ion exchange resin prepared in group G, namely example 5, to the polystyrene micro-plastics are shown in FIGS. 7 and 8, fig. 8a is a microscopic image, fig. 8b is a scanning electron microscopic image, and as can be seen from fig. 7, the magnetic ion exchange resin prepared in example 5 autonomously moves and changes its position during the process of adsorbing the electronegative polystyrene micro-plastic, which is beneficial to improving the adsorption efficiency of the surrounding micro-plastic, and as can be seen from fig. 8, it has a significant adsorption effect on the electronegative polystyrene micro-plastic. The adsorption effect of the magnetic ion exchange resin in the groups E to F and the group H on the polystyrene micro-plastic is basically the same as that of the group G. And the separation and recovery of the ion exchange resins of the E-H groups are realized by adopting the magnet, and a sodium sulfate solution with the concentration of 2mol/L is added into the magnetic ion exchange resin obtained by separation and recovery, so that the micro-plastic adsorbed on the resin falls off and is dispersed again. The obtained magnetic ion exchange resin motor was again placed in the above-mentioned microplastic solution to continue adsorption, and the above-mentioned magnetic separation and microplastic desorption processes were repeated for 5 cycles in this way, and then the adsorption removal rate of polystyrene microplastic in each group of solutions was measured, and the results are shown in table 2.
TABLE 2
| Group of | Group E | Group F | Group G | Group H |
| Adsorption removal rate/%) | 91.3 | 92.2 | 87.8 | 88.9 |
Fig. 9a is a statistical graph of the adsorption removal rate of the magnetic ion exchange resin motor prepared in example 3 on the polyvinyl chloride micro plastic, and fig. 9b is a statistical graph of the adsorption removal rate of the magnetic ion exchange resin motor prepared in example 5 on the polystyrene micro plastic, so that it can be seen that the magnetic ion exchange resin motor prepared in the present invention can be recycled, when the magnetic ion exchange resin motor prepared in example 3 is used to adsorb the polyvinyl chloride micro plastic, an adsorption experiment including 4 cycles can achieve a polyvinyl chloride micro plastic removal rate of 92.4%, and when the magnetic ion exchange resin motor prepared in example 3 is used to adsorb the polystyrene micro plastic, 5 cycles can achieve a polystyrene micro plastic removal rate of 91.3%. Similarly, the adsorption experiment is repeated, and the adsorption removal effect of the magnetic ion exchange resin motor on the polyvinyl chloride and polystyrene micro plastic is basically unchanged after the adsorption is repeated for 20 times, which shows that the magnetic ion exchange resin motor prepared by the invention has good stability and can be repeatedly used.
3. The magnetic ion exchange resins prepared in examples 3 to 6 are used for adsorbing polyamide micro-plastics, the particle size range of the polyamide micro-plastics is 5-100 μm, the polyamide micro-plastics are prepared into suspension with the concentration of 1g/L, 4 groups of I to L are set in the experiment, the electronegative glass culture dishes prepared in example 2 are adopted, 50mL of the polyamide micro-plastic suspension is added into the culture dishes of each group, then 30mg of the magnetic ion exchange resins prepared in examples 3 to 6 are added into the groups I to L respectively, the movement of the magnetic ion exchange resins and the adsorption of the magnetic ion exchange resins to the micro-plastics are observed in the adsorption process, wherein the adsorption effect of the magnetic ion exchange resins prepared in group K, namely example 5, on the polyamide micro-plastics is shown in figure 10, wherein a is a microscopic picture, b is a scanning electron microscopic picture, and as can be seen from figure 10, the composite material has a remarkable adsorption effect on electronegative polyamide micro-plastic. The adsorption effect of the magnetic ion exchange resin in the groups I to J and the group L on the polyamide micro-plastic is basically the same as that of the group K. The adsorption removal rate of the polyamide micro plastic after 1 cycle of adsorption was measured for each group, and the results are shown in table 3.
TABLE 3
| Group of | Group I | J group | Group K | Group L |
| Adsorption removal rate/%) | 99.12 | 96.5 | 97.19 | 97.51 |
And the magnets are adopted to realize separation and recovery of the I-L group ion exchange resins, and a sodium sulfate solution with the concentration of 2mol/L is added into the magnetic ion exchange resins obtained by separation and recovery, so that the micro-plastics adsorbed on the resins fall off and are dispersed again.
The results of the effect tests 1 to 3 show that: the magnetic ion exchange resin motor is obtained by carrying out magnetic modification on the ion exchange resin, and when the magnetic ion exchange resin motor is dispersed in the dispersion liquid of the micro-plastic, spontaneous movement can be generated due to asymmetric adsorption, so that the magnetic ion exchange resin motor has a good adsorption effect on the micro-plastic in the water body.
4. The same effect verification 1 is different in that the negative glass culture dishes used in each group are replaced by unmodified glass culture dishes, the groups are set to be M-P groups, the adsorption rate of polyvinyl chloride micro plastic after each group is adsorbed and saturated is measured, and as a result, the following results are found: when the adsorption experiment is carried out in the modified glass culture dish and the unmodified glass culture dish, the adsorption rate of the micro plastic is basically equivalent, but when the adsorption experiment is carried out in the modified glass culture dish, the adsorption motion of the ion exchange resin motor is more violent, the time for reaching saturated adsorption is shorter and is 20-30 min, and when the adsorption experiment is carried out in the unmodified glass culture dish, the time for reaching the saturated adsorption is longer and is more than 40 min. The glass culture dish is modified to enhance the surface electrical property, so that the electroosmotic flow is enhanced, the movement speed of the resin motor is accelerated, the micro-plastic adsorption speed of the resin motor is correspondingly accelerated, and the time for saturated adsorption is shortened.
The above description is only for the preferred embodiment of the present invention, and the protection scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention, the technical solution and the inventive concept of the present invention equivalent or change within the technical scope of the present invention.
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