CN112275261A - Method for preparing magnetic nanoparticles by ultrasonic waves and application thereof - Google Patents
Method for preparing magnetic nanoparticles by ultrasonic waves and application thereof Download PDFInfo
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Abstract
The invention relates to a method for preparing magnetic nanoparticles by ultrasonic waves and application thereof, belonging to the field of nanoparticle preparation and application; the method comprises the following steps: and dispersing the multi-wall carbon nano tube in a sodium hypochlorite solution to prepare a suspension, carrying out ultrasonic treatment, filtering and drying to obtain MWCNT-COOH. Dissolving a certain amount of chitosan powder by using acetic acid, uniformly stirring by using a magnetic stirrer to prepare a chitosan solution, dispersing MWCNT-COOH in the chitosan solution, and performing ultrasonic treatment to prepare MWCNT-CA. Adding hydrochloric acid into ferric chloride hexahydrate and ferrous chloride tetrahydrate, heating, degassing with nitrogen gas, adding MWCNT-CA, adding ammonia water, introducing nitrogen gas, stirring, separating with magnet, washing with distilled water and ethanol respectively for three times, and drying to obtain Fe3O4-MWCNT-CA. Mixing Fe3O4Suspending MWCNT-CA in distilled water, diluting with ethanol, adding ammonia water and phenanthroline solution, performing ultrasonic treatment reaction, cooling, filtering, washing with distilled water and ethanol for three times, and drying to obtain Fe3O4-MWCNT-CA-phenanthroline. The method has the advantages of simple process, low cost, easy control and high enrichment.
Description
Technical Field
The invention relates to a preparation method and application of magnetic nanoparticles, in particular to a method for preparing magnetic nanoparticles with strong capacity of enriching heavy metal mercury in tea by ultrasonic waves, and belongs to the field of preparation and application of nanoparticles.
Background
Along with the improvement of living standard, the sanitary requirement of people on tea is increasingly improved, and on the basis of paying attention to the pesticide residue index which can cause quick-acting harm to human bodies, the indexes of heavy metal elements which can cause slow-acting harm to human bodies, particularly the contents of mercury, lead, arsenic and other elements in the tea, are paid attention to, and the national food sanitation standard has strict limit regulations. The accurate determination of the content of the heavy metal remaining in the tea leaves or the tea soup by using an analytical instrument is an effective means for realizing the strict control of the heavy metal, and under the condition that a sample with a complex matrix or the content of the heavy metal in the sample is extremely low, a separation and enrichment method is required to be adopted to enhance the sensitivity and specificity of the sample. The magnetic iron oxide nano particles have the advantages of small particle size, large specific surface area, good dispersibility, strong adsorption force, easy separation and the like, thereby being a common magnetic nano material for preparing the solid phase extraction filler; the multi-wall carbon nano-tube has larger specific surface area and strong adsorption capacity, so the multi-wall carbon nano-tube is commonly used for enriching a target object, and particularly, various functional groups are introduced to the surface of the multi-wall carbon nano-tube to increase adsorption sites and improve the selective adsorption performance of the target object.
Chinese patent CN103400677A discloses magnetic Fe3O4@SiO2-NH2Method for preparing nano-microsphere comprising magnetic Fe3O4Nano microsphere, magnetic Fe3O4@SiO2Nano-microsphere and magnetic Fe3O4@SiO2-NH2The synthesis of the nano-microsphere can be applied to a plurality of fields of biotechnology. Chinese patent CN108896676A provides a magnetic nanoparticle and a method for extracting and analyzing five trace fluoroquinolone antibiotics in water, based on a magnetic solid phase extraction technology, the preparation process of the magnetic nanoparticle is as follows: dissolving cysteine in water, and adding Fe3O4Fully dissolving by ultrasonic, performing magnetic separation, pouring out supernatant, performing ultrasonic cleaning by an ultrasonic cleaner, sequentially adding tetrabutyl titanate, 2-amino terephthalic acid, dimethylformamide and methanol, performing ultrasonic homogenization, adding into a hydrothermal synthesis kettle, adding N, N-dimethylformamide into solid substances obtained by reaction magnet separation, placing into an ultrasonic cleaner, and performing ultrasonic cleaning to obtain the magnetic nano-microspheres. Chinese patent CN106432644A discloses a hydrophilic polymer functionalized magnetic nano-scaleThe preparation method and the application of the microsphere take ferroferric oxide as a core, a hydrophilic polymer is formed on the surface of the ferroferric oxide through precipitation polymerization reaction after double bonds on the surface of the ferroferric oxide are functionalized, and the magnetic nano microsphere is used as an adsorbent for separating and enriching glycopeptide or glycoprotein. None of the above methods relates to a method for promoting chitosan modification of magnetic multi-walled carbon nanotubes by using ultrasonic waves.
Disclosure of Invention
The invention aims to provide a method for promoting chitosan to modify magnetic multi-walled carbon nanotubes by ultrasonic waves, which adopts chitosan, magnetic iron oxide, multi-walled carbon nanotubes and the like as materials, promotes modification reaction by an ultrasonic method, ensures high efficiency of the reaction, improves selectivity and associativity of magnetic nanomaterials, and has mild reaction conditions, rapid reaction and easy control; the modified multi-wall carbon nano tube has improved selectivity and increased capability of enriching heavy metal mercury.
In order to achieve the purpose, the invention adopts the technical scheme that: the chitosan and the multi-walled carbon nano-tube are subjected to ultrasonic treatment and then are wound on the surface, a magnetic iron oxide core is added to prepare a magnetic nano-material with a core-shell structure, and finally a certain amount of phenanthroline is added to modify surface groups to form magnetic nano-microspheres with strong chelating properties.
The invention relates to a method for preparing magnetic nanoparticles by ultrasonic waves, which comprises the following specific steps:
(1) dissolving a certain amount of chitosan powder by using 0.1% acetic acid, uniformly stirring by using a magnetic stirrer to prepare a 0.01% Chitosan (CA) solution, adding a certain amount of multi-walled carbon nanotubes (MWCNT-COOH), and carrying out ultrasonic treatment for 10-30 minutes to prepare MWCNT-CA;
(2) in the presence of ferric chloride hexahydrate and ferrous chloride tetrahydrate (Fe)3+/Fe2+=2, molar ratio), adding 12.5mL of 6.0 mol/L hydrochloric acid, heating at 60 ℃ for 5min, fully degassing with nitrogen, adding a certain amount of MWCNT-CA, adding 15mL of 25% ammonia water, charging nitrogen at 60 ℃ for 30min, stirring, separating with magnet, washing with distilled water and ethanol respectively for three times, drying at 60 ℃ to obtain Fe3O4-MWCNT-CA；
(3) 20 mL of the suspension (10 mg Fe)3O4-MWCNT-CA +10 mL of distilled water), diluting with 30 mL of ethanol, performing ultrasonic treatment for 15min, adding 1mL of ammonia water and 10mL of 0.15% o-diazaphenanthrene solution, performing ultrasonic reaction for 30-60 min, cooling, filtering, washing with distilled water and ethanol for three times respectively, and drying at 60 ℃ to obtain Fe3O4-MWCNT-CA-phenanthroline magnetic nanoparticles;
the application of the magnetic nanoparticles prepared by ultrasonic waves is used for enriching heavy metal mercury in tea leaves, and the accurate measurement of the mercury content in the tea leaves is convenient to detect.
The invention has the beneficial effects that:
(1) the invention adopts the multi-walled carbon nanotube as the base material, introduces various functional groups for surface modification, and can improve the enrichment capacity of the magnetic nanoparticles while selectively enriching heavy metal ions;
(2) the invention adopts ultrasonic waves to promote modification reaction, promotes the reaction between the carbon nano tube and the chitosan and the phenanthroline by utilizing the cavitation effect of the ultrasonic waves, greatly shortens the reaction time, increases the modification degree of reaction products, has mild reaction conditions and easy control, improves the enrichment capacity of modified magnetic nano particles, and enhances the selectivity;
(3) the method has the advantages of simple process, low cost, high reaction efficiency and easy control.
Detailed Description
The present invention is further illustrated by the following examples, which are provided only for illustrating the present invention and do not limit the scope of the present invention.
Example 1
(1) Dissolving a certain amount of chitosan powder in 0.1% acetic acid, uniformly stirring by a magnetic stirrer to prepare 200mL of 0.01% Chitosan (CA) solution, adding 500mg of multi-walled carbon nanotubes (MWCNT-COOH), carrying out ultrasonic treatment for 10 minutes, filtering, washing until the pH of the filtrate is neutral, and drying at 70 ℃ to prepare the MWCNT-CA.
(2) In the presence of ferric chloride hexahydrate and ferrous chloride tetrahydrate (Fe)3+/Fe2+=2, molar ratio) 7.2g, dilute was addedHeating hydrochloric acid 12.5mL at 60 deg.C for 5min, degassing with nitrogen, adding 400mg MWCNT-CA prepared in (1), adding 25% ammonia water 15mL, charging nitrogen at 60 deg.C for 30min, stirring, separating with magnet, washing with distilled water and ethanol respectively for three times, and drying at 60 deg.C to obtain Fe3O4-MWCNT-CA。
(3) Mixing 10 mg of Fe3O4Suspending MWCNT-CA in 10mL of distilled water, diluting with 30 mL of ethanol, adding 1mL of ammonia water and 10mL of 0.15% o-diazaphenanthrene solution, performing ultrasonic reaction for 30min, cooling, filtering, washing with distilled water and ethanol for three times respectively, and drying at 60 ℃ to obtain Fe3O4-MWCNT-CA-phenanthroline magnetic nanoparticles.
(4) The test analysis of the heavy metal mercury in the tea soup and the tea digestion solution is carried out on the magnetic nano particles prepared by the ultrasonic-assisted method, the results are shown in the following table,
according to the detection result, the magnetic nano-microspheres prepared by ultrasonic modification by the method are black granular powder, so that the dispersibility is good, the adsorption capacity is improved, and the recovery rate of mercury in the sample liquid is increased.
Example 2
(1) Dissolving a certain amount of chitosan powder in 0.1% acetic acid, uniformly stirring by using a magnetic stirrer to prepare 200mL of 0.02% Chitosan (CA) solution, adding 500mg of multi-walled carbon nanotubes (MWCNT-COOH), carrying out ultrasonic treatment for 20 minutes, filtering, washing until the pH value of the filtrate is neutral, and drying at 70 ℃ to prepare the MWCNT-CA.
(2) In the presence of ferric chloride hexahydrate and ferrous chloride tetrahydrate (Fe)3+/Fe2+=2, molar ratio) 7.2g, adding 12.5mL of dilute hydrochloric acid, heating at 60 ℃ for 5min, sufficiently degassing with nitrogen, adding 400mg of MWCNT-CA prepared in the above (1), adding 15mL of 25% ammonia water, introducing nitrogen at 60 ℃ for 30min, stirring, separating with magnet, washing with distilled water and ethanol respectively three times, drying at 60 ℃ to obtain Fe3O4-MWCNT-CA。
（3）Mixing 10 mg of Fe3O4Suspending MWCNT-CA in 10mL of distilled water, diluting with 30 mL of ethanol, adding 1mL of ammonia water and 10mL of 0.15% o-diazaphenanthrene solution, performing ultrasonic reaction for 50min, cooling, filtering, washing with distilled water and ethanol for three times respectively, and drying at 60 ℃ to obtain Fe3O4-MWCNT-CA-phenanthroline magnetic nanoparticles.
(4) The test analysis of the heavy metal mercury in the tea soup and the tea digestion solution is carried out on the magnetic nano particles prepared by the ultrasonic-assisted method, the results are shown in the following table,
according to the detection result, the magnetic nano-microspheres prepared by ultrasonic modification by the method are black granular powder, so that the dispersibility is good, the adsorption capacity is improved, and the recovery rate of mercury in the sample liquid is increased.
Example 3
(1) Dissolving a certain amount of chitosan powder in 0.1% acetic acid, uniformly stirring by using a magnetic stirrer to prepare 200mL of 0.02% Chitosan (CA) solution, adding 500mg of multi-walled carbon nanotubes (MWCNT-COOH), carrying out ultrasonic treatment for 30 minutes, filtering, washing until the pH value of the filtrate is neutral, and drying at 70 ℃ to prepare the MWCNT-CA.
(2) In the presence of ferric chloride hexahydrate and ferrous chloride tetrahydrate (Fe)3+/Fe2+=2, molar ratio) 7.2g, adding 12.5mL of dilute hydrochloric acid, heating at 60 ℃ for 5min, sufficiently degassing with nitrogen, adding 400mg of MWCNT-CA prepared in the above (1), adding 15mL of 25% ammonia water, introducing nitrogen at 60 ℃ for 30min, stirring, separating with magnet, washing with distilled water and ethanol respectively three times, drying at 60 ℃ to obtain Fe3O4-MWCNT-CA。
(3) Mixing 10 mg of Fe3O4Suspending MWCNT-CA in 10mL of distilled water, diluting with 30 mL of ethanol, adding 1mL of ammonia water and 10mL of 0.1% o-diazaphenanthrene solution, performing ultrasonic reaction for 50min, cooling, filtering, washing with distilled water and ethanol for three times respectively, and drying at 60 ℃ to obtain Fe3O4-MWCNT-CA-phenanthroline magnetic nanoparticles.
(4) The test analysis of the heavy metal mercury in the tea soup and the tea digestion solution is carried out on the magnetic nano particles prepared by the ultrasonic-assisted method, the results are shown in the following table,
according to the detection result, the magnetic nano-microspheres prepared by ultrasonic modification by the method are black granular powder, so that the dispersibility is good, the adsorption capacity is improved, and the recovery rate of mercury in the sample liquid is increased.
Claims (5)
1. A method for preparing magnetic nanoparticles by ultrasonic waves is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving a certain amount of chitosan powder by using 0.1% acetic acid, uniformly stirring by using a magnetic stirrer to prepare a 0.01% chitosan CA solution, adding a certain amount of multi-walled carbon nano-tube MWCNT-COOH, and carrying out ultrasonic treatment to prepare MWCNT-CA;
(2) adding 6.0 mol/L hydrochloric acid 12.5mL into ferric chloride hexahydrate and ferrous chloride tetrahydrate, heating at 60 deg.C for 5min, degassing with nitrogen gas, adding a certain amount of MWCNT-CA, adding 25% ammonia water 15mL, charging nitrogen gas at 60 deg.C for 30min, stirring, separating with magnet, washing with distilled water and ethanol respectively for three times, and drying at 60 deg.C to obtain Fe3O4-MWCNT-CA；
(3) Mixing 10 mg of Fe3O4Suspending MWCNT-CA in 10mL of distilled water, diluting with 30 mL of ethanol, adding 1mL of ammonia water and 10mL of 0.15% o-diazaphenanthrene solution, performing ultrasonic treatment reaction, filtering, washing with distilled water and ethanol for three times respectively, and drying at 60 ℃ to obtain Fe3O4-MWCNT-CA-phenanthroline magnetic nanoparticles.
2. The method for preparing magnetic nanoparticles by ultrasonic waves according to claim 1, wherein the method comprises the following steps: the frequency of ultrasonic treatment in the steps (1) and (3) is 20-25 kHz, the power is 200W, and the diameter of the probe is 0.6 cm.
3. The method for preparing magnetic nanoparticles by ultrasonic waves according to claim 1, wherein the method comprises the following steps: the ultrasonic treatment method in the steps (1) and (3) is characterized in that a probe is inserted into the solution for 1-2 cm in depth, ultrasonic work is carried out for 4s, the interval is 2s, the highest temperature is 60 ℃, then an ice water bath is adopted to control the temperature to be 30-60 ℃, and ultrasonic treatment is carried out for 10-60 min to carry out modification reaction.
4. The method for preparing magnetic nanoparticles by ultrasonic waves according to claim 1, wherein the method comprises the following steps: fe of ferric chloride hexahydrate and ferrous chloride tetrahydrate in step (2)3+/Fe2+The molar ratio was 2.
5. The application of the ultrasonic wave to prepare the magnetic nano particles is characterized in that: the magnetic nanoparticles are used for enriching heavy metal mercury in tea leaves, and are convenient for accurate measurement of mercury content in the tea leaves.
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