CN103341349A - Imidazole and chitosan functional magnetic particle, as well as preparation method and application thereof - Google Patents
Imidazole and chitosan functional magnetic particle, as well as preparation method and application thereof Download PDFInfo
- Publication number
- CN103341349A CN103341349A CN2013102570753A CN201310257075A CN103341349A CN 103341349 A CN103341349 A CN 103341349A CN 2013102570753 A CN2013102570753 A CN 2013102570753A CN 201310257075 A CN201310257075 A CN 201310257075A CN 103341349 A CN103341349 A CN 103341349A
- Authority
- CN
- China
- Prior art keywords
- magnetic particle
- imidazoles
- preparation
- solution
- cts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses an imidazole and chitosan functional magnetic particle, as well as a preparation method and an application thereof. The imidazole and chitosan functional magnetic particle is a Fe3O4 magnetic particle jointly modified by imidazole and chitosan, and is represented as Fe3O4@OA@CTS-g-IMZ, wherein in the formula, the OA represents oleic acid, the CTS represents chitosan, and the IMZ represents imidazole. The method provided by the invention is convenient and economical in synthetic process and provides the preparation method and the application of the imidazole and chitosan jointly-modified magnetic particle which is more in functional group, and good in selectivity and has the environment-friendly effect, after the imidazole and chitosan functional magnetic particle disclosed by the invention is used, the sulfoacid dye in a water sample can be effectively, simply, quickly and innocuously removed.
Description
Technical field
The present invention relates to a kind of functional magnetic particle preparation methods and applications, especially relate to magnetic particle of a kind of imidazoles and shitosan functionalization and its preparation method and application.
Background technology
At present, the main method that removes sulfonic acid dyestuff in the waste water has chemical oxidization method, membrane separation process, flocculence, absorption method, microbial degradation method etc., these methods respectively have advantage, need to use a large amount of organic solvents but exist, product recovery rate is low, economic benefit is undesirable, complex operation and secondary pollution problems.
But the functional magnetic particle is because of its surface functionalization, have selective preferably, and can be in magnetic field directed separation rapidly, therefore, have broad application prospects aspect the sulfonic acid dyestuff in removing waste water.
At present, the research work for the sorbing material that removes the waste water dyestuff has obtained certain achievement.201210121603.8 disclose the dyestuff sorbing material that a kind of banana skin is made on August 15th, 2012, its preparation method is: (1) water cleans banana skin, and making beating is sent the banana latex into fermentation tank for the banana latex then; (2) inoculate bacterial classification in the fermentation tank, ventilating fermentation; (3) the product Separation of Solid and Liquid in the fermentation tank, collect solid portion washing back; (4) solid portion drying, pulverizing.The dyestuff of 40-60% in the adsorbable dyestuff waste liquid of this sorbing material, removal efficiency is lower, and can not reuse, and complicated operations, time-consuming consumption power such as also needs to filter, centrifugal.201110116052.1 but a kind of preparation method who removes the novel absorption material of dyestuff Magnetic Isolation was disclosed on September 14th, 2011, synthesis step is as follows: will adopt chemical vapour deposition technique gained CNT primary sample, ultrasonic being dispersed in the distilled water.Add a certain amount of oxidizing solution, solution is placed magnetic stirring apparatus, at a certain temperature back flow reaction a few hours.Magnetic carbon nano-tube sample filtering, washing, vacuum drying with after the modification can obtain the magnetic carbon nano-tube composite adsorbing material.This magnetic carbon nano-tube composite adsorbing material is stable and dispersive property is preferably arranged in the aqueous solution, dyestuff is had removal effect preferably, but this material is selectively relatively poor, and not reproducible use, needed carbon nano-tube material is expensive, and the source is not abundant, is difficult to industrialization.201110219902.0 disclose a kind of preparation method and application of dyestuff sorbing material on February 6th, 2013.The present invention utilizes cdear needle oven dry to pulverize, and utilizes alcohol degreasing, takes off organic pigment, and through the phosphate buffer flushing, precipitation oven dry is again made sorbing material and is used for the removal of dyestuff after sieving.This biology sorbing material is to the removal efficiency height of dyestuff, and preparation process is simple, and the aspect of drawing materials, material abundance, cost are lower, but sorbing material can't recycle, and complicated operations such as needs to filter, centrifugal, time-consuming consumption power.201210112650 disclose a kind of preparation method with magnetic mesoporous carbon nanometer micro ball of high absorption property on August 1st, 2012, and the method for its solvent-applied heat is introduced Fe in mesoporous carbon
3O
4Magnetic particle is prepared a kind of mesoporous carbon microballoon with high saturation degree, uses it for removing of pollutants such as dyestuff in the waste water.The magnetic mesoporous carbon nanometer micro ball of preparation has high specific area (741.8m
2G
-1), can be widely used in fields such as water treatment, catalyst carrier and biomedicine, but selectively good inadequately.Remove the method that contains the sulfonic group dyestuff in the alkaline waste water 201110020472.X disclose the chitosan magnetic sorbing material on June 29th, 2011, the preparation method is as follows: (1) is dissolved into shitosan in the ferric chloride in aqueous solution, stir, separate out solid after adding ethanol, solid after filtration, washing is back and nano-magnetic Fe
3O
4Mix, carry out cross-linking reaction with glutaraldehyde water solution again, cross-linking reaction is finished by post processing and is obtained the chitosan magnetic sorbing material; (2) chitosan magnetic is joined in the aqueous solution that contains the sulfonic group dyestuff, stir, filter, obtain reclaiming solution and the chitosan magnetic sorbing material of dyestuff.This method is simple to operate, environmental friendliness and with low cost, but functional group is less relatively, can influence the saturated extent of adsorption of adsorbent p-sulfonic acid radical dye.
Dyestuff sorbing material kind is various, can be as sorbing material as materials such as active carbon, CNT, zeolites.Be the natural dye sorbing material of representative with the shitosan, wide material sources, cheap, receive much concern.Imidazoles cheap and easy to get is a kind of protonated material easily, and the pollutant that exists with anionic form is had good absorption.Thereby, with the common modification magnetic Fe of these two kinds of materials
3O
4, obtain being rich in functional group-NH
2The magnetic particle of ,-NH-can remove the sulfonic acid dyestuff that exists with anionic form in the waste water effectively.
In the sorbing material of using always that removes the sulfonic group dyestuff in the waste water, selectively relatively poor, functional group is less relatively and single at present.With regard to our document of retrieval as can be known, the magnetic particle of preparation imidazoles and the common functionalization of shitosan, and be applied to remove with recycle-water in MO, CR and the research of three kinds of sulfonic acid classes of ACBK dyestuff do not see reported in literature.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, and a kind of imidazoles and shitosan functional magnetic particle and its preparation method and application are provided.
The present invention's modification magnetic particle is the magnetic particle of imidazoles and shitosan functionalization, is expressed as: Fe
3O
4@OA@CTS-g-IMZ, in the formula, OA represents oleic acid, and CTS represents shitosan, and IMZ represents imidazoles.
The preparation method of the present invention's functional magnetic particle may further comprise the steps:
(1) Fe
3O
4The synthetic method of @OA: under 25 ℃, with 5.8g Fe (NO
3) 9H
2O and 2.3g FeSO
46H
2O adds in the three-necked bottle, adds the 100mL redistilled water of logical nitrogen 30min deoxidation, and mechanical agitation 5min under the nitrogen protection adds the 10mL concentrated ammonia liquor in three-necked bottle, continues mechanical agitation 10min, adds 1.0g oleic acid again, mechanical agitation 1h.Shift out, washing obtains Fe to neutral
3O
4@OA, stand-by.
The mol ratio of described trivalent iron salt and divalent iron salt is 1: 0.5.
(2) Fe
3O
4The synthetic method of @OA@CTS-g-IMZ; The Fe that drying is good
3O
4The @OA magnetic particle is scattered in the 50mL redistilled water again, is transferred in the three-necked bottle mechanical agitation 10min under the room temperature; Add 50mL3% chitosan solution (using 1% acetate dissolution), 0.23g SDS, continue to stir 10min; Add 25mL imidazoles solution, add 2mL ECH again, be warming up to 70 ℃, reaction 16h; Shift out, washing is extremely neutral, and 70 ℃ of vacuum drying 24h are stand-by.Mixing speed is 1200rmin in the whole process
-1
The preparation of described imidazoles solution: 1.5g IMZ is dissolved in the mixed solution of 25mL NaOH solution/methyl alcohol, wherein the mixed solution of NaOH and methyl alcohol is: V (NaOH): V (methyl alcohol)=1: 4, ultrasonic agitation is uniformly dispersed.The concentration of NaOH is 2M in the mixed liquor.
The present invention's imidazoles and shitosan functional magnetic particle are applied to remove sulfonic acid dyestuff in the waste water, may further comprise the steps:
(1) preparation of simulated wastewater: pipette the dyestuff storing solution of a certain amount of MO, CR, ACBK respectively, being diluted to concentration with deionized water is 100mgL
-1The homogencous dyes standard liquid, and be placed in 4 ℃ the refrigerator standby;
(2) regulating MO, CO and ABCK sample solution pH is 2～12; Claim 20mgFe
3O
4The functional magnetic particle of @OA@CTS-g-IMZ adds 10.00mL10mgL in the 25mL volumetric flask
-1Sample solution (MO, CR or ACBK solution), 10 ℃～50 ℃ constant temperature vibration absorption; 5～25min after the time takes out sample, and magnetic separates, and shifts out solution, and is stand-by.
(3) magnetic particle with second distillation water washing three times after, use 10.00mL0.8molL
-1NaOH/ acetone (V: V=80: 20) wash-out MO, CR and ACBK, magnetic separates, and obtains strip liquor and magnetic particle;
(4) respectively to material liquid, extraction back feed liquid and strip liquor sampling, regulating pH is 6, measures their concentration with visible/UV-detector.
The optimum condition of described subtractive process is: the optimal pH of MO, CR and ACBK is 4; Reaction temperature is 30 ℃; The extraction time is 10min; Back extraction time 10min.
Advantage of the present invention: (1) magnetic particle particle diameter is little, is rich in than function groups, is easy to be combined with electrostatic interaction with target substance; Studies show that remove sulfonic acid dyestuff in the waste water with the magnetic particle of imidazoles and shitosan functionalization, speed is fast, the removal efficiency height, and magnetic particle is reusable; (2) because the distinctive magnetic responsiveness of magnetic particle self of imidazoles and shitosan functionalization can promptly separate, do not need centrifugally operated under the effect of externally-applied magnetic field, be conducive to simplification and the automation of separation process; (3) adopt imidazoles cheap and easy to get, that the source is abundant and shitosan to Fe
4O
3Modification has not only reduced cost, can also remove effectively and the sulfonic acid dyestuff that reclaims in the waste water; (4) the whole process that removes the sulfonic acid dyestuff is not used toxic solvent, neither can influence health of operators, can not cause secondary pollution again; (5) whole process operation is simple, and weak point consuming time can be raised the efficiency, and saves manpower and the energy.
Description of drawings
Fig. 1 is imidazoles and the shitosan functional magnetic particle Fe of embodiment 1
3O
4The transmission electron microscope figure of @OA@CTS-g-IMZ;
Fig. 2 is the Fe of embodiment 1
3O
4@OA@CTS-g-IMZ (c), Fe
3O
4@OA@CTS (b) and Fe
3O
4(a) infared spectrum of three kinds of magnetic particles;
Fig. 3 is the Fe of embodiment 1
3O
4@OA@CTS-g-IMZ (c), Fe
3O
4@OA@CTS (b) and Fe
3O
4(a) X-ray diffractogram of three kinds of magnetic particles;
Fig. 4 is the Fe of embodiment 1
3O
4@OA@CTS-g-IMZ (c), Fe
3O
4@OA (b) and Fe
3O
4(a) the hysteresis curve figure of three kinds of magnetic particles;
Fig. 5 is the Fe of embodiment 1
3O
4The N of @OA@CTS-g-IMZ
2(illustration is Fe to adsorption and desorption figure among the figure
3O
4The pore volume of @OA@CTS-g-IMZ and graph of pore diameter distribution.
Fig. 6 is the Fe of embodiment 1
3O
4The @OA@CTS-g-IMZ access times are to the influence of the removal efficiency of MO, CR and three kinds of sulfonic acid dyestuffs of ACBK.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
The imidazoles of present embodiment and shitosan functional magnetic particle Fe
3O
4The preparation method of @OA@CTS-g-IMZ may further comprise the steps:
(1) Fe
3O
4The synthetic method of @OA: under 25 ℃, with 5.8g Fe (NO
3) 9H
2O and 2.3g FeSO
46H
2O adds in the three-necked bottle, adds the 100mL redistilled water of logical nitrogen 30min deoxidation, and mechanical agitation 5min under the nitrogen protection adds the 10mL concentrated ammonia liquor in three-necked bottle, continues mechanical agitation 10min, adds 1.0g oleic acid again, mechanical agitation 1h.Shift out, washing obtains Fe to neutral
3O
4@OA, stand-by.
The mol ratio of described trivalent iron salt and divalent iron salt is 1: 0.5.
(2) Fe
3O
4The synthetic method of @OA@CTS-g-IMZ; The Fe that drying is good
3O
4The @OA magnetic particle is scattered in the 50mL redistilled water again, is transferred in the three-necked bottle mechanical agitation 10min under the room temperature; Add 50mL3% chitosan solution (using 1% acetate dissolution), 0.23g SDS, continue to stir 10min; Add 25mL imidazoles solution, add 2mL ECH again, be warming up to 70 ℃, reaction 16h; Shift out, washing is extremely neutral, and 70 ℃ of vacuum drying 24h are stand-by.Mixing speed is 1200rmin in the whole process
-1
The preparation of described imidazoles solution: 1.5g IMZ is dissolved in the mixed solution of 25mL NaOH solution/methyl alcohol, wherein the mixed solution of NaOH and methyl alcohol is: V (NaOH): V (methyl alcohol)=1: 4, ultrasonic agitation is uniformly dispersed.The concentration of NaOH is 2M in the mixed liquor.
Adopt transmission electron microscope, FTIS, X-ray diffraction analysis instrument, vibrating specimen magnetometer and specific surface area measuring instrument to imidazoles and the shitosan functional magnetic particle Fe of preparation
3O
4@OA@CTS-g-IMZ characterizes, referring to accompanying drawing 1-Fig. 5.Characterization result shows: this magnetic particle is spherical in shape substantially, has hole to exist, and average grain diameter is about 90nm, has good superparamagnetism and stability, and the N of magnetic particle
2Isothermal absorption meets IV isothermal absorption mode.
The imidazoles of present embodiment and shitosan functional magnetic particle are applied to remove sulfonic acid dyestuff in the waste water, may further comprise the steps:
(1) preparation of standard liquid: accurately take by weighing 0.50g respectively and analyze pure MO, CR, ACBK in the 500mL volumetric flask, after being dissolved in water, constant volume; Pipette a certain amount of dyestuff storing solution respectively, be diluted to 100mgL with deionized water
-1The homogencous dyes standard liquid, and then be diluted to the standard liquid of a series of variable concentrations.Storing solution and standard liquid are placed in 4 ℃ the refrigerator standby.
The preparation of simulated wastewater: pipette the dyestuff storing solution of a certain amount of MO, CR and ACBK respectively, being diluted to concentration with deionized water all is 100mgL
-1The homogencous dyes standard liquid, and be placed in 4 ℃ the refrigerator standby;
(2) regulating MO, CR and ACBK sample solution pH is 4; Claim 20mg Fe
3O
4The functional magnetic particle of @OA@CTS-g-IMZ adds 10.00mL10mgL in the 25mL volumetric flask
-1Sample solution (MO, CR or ACBK solution), in the time of 30 ℃, constant temperature vibration 10min takes out sample, and magnetic separates, and shifts out solution, and is stand-by.
(3) magnetic particle with second distillation water washing three times after, use 10.00mL0.8molL
-1NaOH/ acetone (V: V=80: 20) wash-out MO, CR and ACBK, magnetic separates, and obtains strip liquor and magnetic particle;
(4) respectively to material liquid, extraction back feed liquid and strip liquor sampling, regulating pH is 6, measures their concentration with visible/UV-detector.Parallelly do three experiments.
The detection wavelength of above-mentioned three kinds of sulfonic acid dyestuff MO, CR and ACBK is respectively: 464nm, 499nm, 522nm; Hydrophily polypropylene filter membrane with 0.45 aperture before the sample detection filters.
The final analysis result shows: Fe
3O
4The functional magnetic particle of @OA@CTS-g-IMZ is fine to the removal effect of MO, CR and these three kinds of sulfonic acid dyestuffs of ACBK, and the removal efficiency of correspondence was respectively 92.1%, 93.2%, 94.3% when homogencous dyes removed; Use 10.00mL0.8molL
-1(V: V=80: 20) back extraction MO, CO and ABCK, the rate of recovery is all more than 90% for NaOH/ acetone.
This magnetic particle particle reproducible utilization recycles five times, and to the nearly all not variation of removal efficiency of MO, CR and these three kinds of sulfonic acid dyestuffs of ACBK, its result as shown in Figure 6.
Embodiment 2
The shitosan functional magnetic particle Fe of present embodiment
3O
4The preparation method of @OA@CTS may further comprise the steps:
(1) Fe
3O
4The synthetic method of @OA: under 25 ℃, with 5.8g Fe (NO
3) 9H
2O and 2.3g FeSO
46H
2O adds in the three-necked bottle, adds the 100mL redistilled water of logical nitrogen 30min deoxidation, and mechanical agitation 5min under the nitrogen protection adds the 10mL concentrated ammonia liquor in three-necked bottle, continues mechanical agitation 10min, adds 1.0g oleic acid again, mechanical agitation 1h.Shift out, washing obtains Fe to neutral
3O
4@OA, stand-by.
The mol ratio of described trivalent iron salt and divalent iron salt is 1: 0.5.
(2) Fe
3O
4The synthetic method of @OA@CTS; The Fe that drying is good
3O
4The @OA magnetic particle is scattered in the 50mL redistilled water again, is transferred in the three-necked bottle mechanical agitation 10min under the room temperature; Add 50mL3% chitosan solution (using 1% acetate dissolution), 0.23g SDS, continue to stir 10min; Add 2mL ECH again, be warming up to 70 ℃, reaction 16h; Shift out, washing is extremely neutral, and 70 ℃ of vacuum drying 24h are stand-by.Mixing speed is 1200rmin in the whole process
-1
The magnetic particle of the imidazoles of present embodiment and shitosan functionalization is applied to remove sulfonic acid dyestuff in the waste water, may further comprise the steps:
(1) preparation of standard liquid: accurately take by weighing 0.50g respectively and analyze pure MO, CR, ACBK in the 500mL volumetric flask, after being dissolved in water, constant volume; Pipette a certain amount of dyestuff deposit respectively, be diluted to 100mgL with deionized water
-1The homogencous dyes standard liquid, and then be diluted to the standard liquid of a series of variable concentrations.Storing solution and standard liquid are placed in 4 ℃ the refrigerator standby.
The preparation of simulated wastewater: pipette the dyestuff storing solution of a certain amount of MO, CR and ACBK respectively, being diluted to concentration with deionized water all is 100mgL
-1The homogencous dyes standard liquid, and be placed in 4 ℃ the refrigerator standby;
(2) regulating MO, CR and ACBK sample solution pH is 4; Claim 20mg Fe
3O
4The functional magnetic particle of @OA@CTS adds 10.00mL10mgL in the 25mL volumetric flask
-1Sample solution (MO, CR or ACBK solution), in the time of 30 ℃, constant temperature vibration 10min takes out sample, and magnetic separates, and shifts out solution, and is stand-by.
(3) magnetic particle with second distillation water washing three times after, use 10.00mL0.8molL
-1NaOH/ acetone (V: V=80: 20) wash-out MO, CR and ACBK, magnetic separates, and obtains strip liquor and magnetic particle;
(4) respectively to material liquid, extraction back feed liquid and strip liquor sampling, regulating pH is 6, measures their concentration with visible/UV-detector.Parallelly do three experiments.
The preparation method of the imidazoles of present embodiment and shitosan functional magnetic particle may further comprise the steps:
(1) Fe
3O
4The synthetic method of @OA: under 25 ℃, with 5.8g Fe (NO
3) 9H
2O and 2.3g FeSO
46H
2O adds in the three-necked bottle, adds the 100mL redistilled water of logical nitrogen 30min deoxidation, and mechanical agitation 5min under the nitrogen protection adds the 10mL concentrated ammonia liquor in three-necked bottle, continues mechanical agitation 10min, adds 1.0g oleic acid again, mechanical agitation 1h.Shift out, washing obtains Fe to neutral
3O
4@OA, stand-by.
The mol ratio of described trivalent iron salt and divalent iron salt is 1: 0.5.
(2) Fe
3O
4The synthetic method of @OA@CTS-g-IMZ; The Fe that drying is good
3O
4The @OA magnetic particle is scattered in the 50mL redistilled water again, is transferred in the three-necked bottle mechanical agitation 10min under the room temperature; Add 50mL3% chitosan solution (using 1% acetate dissolution), 0.23g SDS, continue to stir 10min; Add 25mL imidazoles solution, add 2mL ECH again, be warming up to 70 ℃, reaction 16h; Shift out, washing is extremely neutral, and 70 ℃ of vacuum drying 24h are stand-by.Mixing speed is 1200rmin in the whole process
-1
The preparation of described imidazoles solution: 1.5g IMZ is dissolved in the mixed solution of 25mL KOH solution/methyl alcohol, wherein the mixed solution of KOH and methyl alcohol is: V (KOH): V (methyl alcohol)=1: 4, ultrasonic agitation is uniformly dispersed.The concentration of KOH is 2M in the mixed liquor.
The imidazoles of present embodiment and shitosan functional magnetic particle are applied to remove sulfonic acid dyestuff in the waste water, may further comprise the steps:
(1) preparation of standard liquid: accurately take by weighing 0.50g respectively and analyze pure MO, CR, ACBK in the 500mL volumetric flask, after being dissolved in water, constant volume; Pipette a certain amount of dyestuff storing solution respectively, be diluted to 100mgL with deionized water
-1The homogencous dyes standard liquid, and then be diluted to the standard liquid of a series of variable concentrations.Storing solution and standard liquid are placed in 4 ℃ the refrigerator standby.
The preparation of simulated wastewater: pipette the dyestuff storing solution of a certain amount of MO, CR and ACBK respectively, being diluted to concentration with deionized water all is 100mgL
-1The homogencous dyes standard liquid, and be placed in 4 ℃ the refrigerator standby;
(2) regulating MO, CR and ACBK sample solution pH is 4; Claim 20mg Fe
3O
4The functional magnetic particle of @OA@CTS-g-IMZ adds 10.00mL10mgL in the 25mL volumetric flask
-1Sample solution (MO, CR or ACBK solution), in the time of 30 ℃, constant temperature vibration 10min takes out sample, and magnetic separates, and shifts out solution, and is stand-by.
(3) magnetic particle with second distillation water washing three times after, use 10.00mL0.8molL
-1NaOH/ acetone (V: V=80: 20) wash-out MO, CR and ACBK, magnetic separates, and obtains strip liquor and magnetic particle;
(4) respectively to material liquid, extraction back feed liquid and strip liquor sampling, regulating pH is 6, measures their concentration with visible/UV-detector.Parallelly do three experiments.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (3)
1. the preparation method of an imidazoles and shitosan functional magnetic particle is characterized in that, may further comprise the steps:
(1) Fe
3O
4The synthetic method of @OA: under 25 ℃, be 2.5 Fe (NO with mass ratio
3)
39H
2O and FeSO
46H
2O adds in the three-necked bottle, adds the 100mL redistilled water of logical nitrogen 30min deoxidation, and mechanical agitation 5min under the nitrogen protection adds the 10mL concentrated ammonia liquor in three-necked bottle, continues mechanical agitation 10min, adds 1.0g oleic acid again, mechanical agitation 1h.Shift out, washing obtains Fe to neutral
3O
4@OA, stand-by; The mol ratio of described trivalent iron salt and divalent iron salt is 1: 0.5～0.75;
(2) Fe
3O
4The synthetic method of @OA@CTS-g-IMZ: the Fe that drying is good
3O
4The @OA magnetic particle is scattered in the redistilled water again, is transferred in the three-necked bottle mechanical agitation 10min under the room temperature; Add 50mL3% chitosan solution (using 1% acetate dissolution), 0.23g dodecyl sodium sulfate, continue to stir 10min; Add imidazoles solution, add the 2mL epoxychloropropane again, be warming up to 70 ℃, reaction 16h; Shift out, washing is extremely neutral, and 70 ℃ of vacuum drying 24h are stand-by; Mixing speed is 1200rmin in the whole process
-1
The preparation of described imidazoles solution: the 1.5g imidazoles is dissolved in the mixed solution of 25mL NaOH solution/methyl alcohol, wherein the mixed solution of NaOH and methyl alcohol is: V (NaOH): V (methyl alcohol)=1: 4, ultrasonic agitation is uniformly dispersed.
2. imidazoles and the chitin modified magnetic particle of preparation method's preparation as claimed in claim 1 is characterized in that, are the common Fe that modifies of imidazoles and shitosan
3O
4Magnetic particle is expressed as: Fe
3O
4@OA@CTS-g-IMZ, in the formula, OA represents oleic acid, and CTS represents shitosan, and IMZ represents imidazoles.
3. imidazoles as claimed in claim 2 and the chitin modified magnetic particle application aspect the sulfonic acid dyestuff in removing waste water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310257075.3A CN103341349B (en) | 2013-06-26 | 2013-06-26 | A kind of imidazoles and chitosan functional magnetic particle and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310257075.3A CN103341349B (en) | 2013-06-26 | 2013-06-26 | A kind of imidazoles and chitosan functional magnetic particle and its preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103341349A true CN103341349A (en) | 2013-10-09 |
| CN103341349B CN103341349B (en) | 2015-12-23 |
Family
ID=49276202
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310257075.3A Active CN103341349B (en) | 2013-06-26 | 2013-06-26 | A kind of imidazoles and chitosan functional magnetic particle and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103341349B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920472A (en) * | 2014-04-11 | 2014-07-16 | 江苏大学 | Preparation method of magnetic chitosan composite microsphere adsorbent |
| CN108636366A (en) * | 2018-04-17 | 2018-10-12 | 江苏国创环保科技有限公司 | A kind of preparation method and application of the magnetic adsorptive material of absorption heavy metal |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102114411A (en) * | 2011-01-18 | 2011-07-06 | 湖南师范大学 | Lecithin magnetic nano-composite and preparation method and application thereof |
| CN102360659A (en) * | 2011-06-24 | 2012-02-22 | 中国科学院宁波材料技术与工程研究所 | Magnetic submicron composite core-shell particles, and preparation method and application thereof |
| CN102489264A (en) * | 2011-12-21 | 2012-06-13 | 湖南师范大学 | Chitosan magnetic nano particle as well as preparation method and application thereof |
| CN102653891A (en) * | 2012-05-03 | 2012-09-05 | 东华大学 | Method for preparing magnetic benzoxazinyl carbon nanofiber material |
-
2013
- 2013-06-26 CN CN201310257075.3A patent/CN103341349B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102114411A (en) * | 2011-01-18 | 2011-07-06 | 湖南师范大学 | Lecithin magnetic nano-composite and preparation method and application thereof |
| CN102360659A (en) * | 2011-06-24 | 2012-02-22 | 中国科学院宁波材料技术与工程研究所 | Magnetic submicron composite core-shell particles, and preparation method and application thereof |
| CN102489264A (en) * | 2011-12-21 | 2012-06-13 | 湖南师范大学 | Chitosan magnetic nano particle as well as preparation method and application thereof |
| CN102653891A (en) * | 2012-05-03 | 2012-09-05 | 东华大学 | Method for preparing magnetic benzoxazinyl carbon nanofiber material |
Non-Patent Citations (1)
| Title |
|---|
| LAM DAI TRAN ET AL: "Electrochemical detection of short HIV sequences on chitosan/Fe3O4 nanoparticle based screen printed electrodes", 《MATERIALS SCIENCE AND ENGINEERING C》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920472A (en) * | 2014-04-11 | 2014-07-16 | 江苏大学 | Preparation method of magnetic chitosan composite microsphere adsorbent |
| CN108636366A (en) * | 2018-04-17 | 2018-10-12 | 江苏国创环保科技有限公司 | A kind of preparation method and application of the magnetic adsorptive material of absorption heavy metal |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103341349B (en) | 2015-12-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105170095B (en) | A kind of In bases organic backbone graphene oxide composite material and its preparation method and application | |
| CN101574645B (en) | Magnetic nano-material extractant and preparation method thereof | |
| CN105251448B (en) | A kind of preparation method of magnetic graphene composite | |
| CN102716718B (en) | Modified starch magnetic nano compound and preparation method and application thereof | |
| CN109529775B (en) | Synthesis method and adsorption performance of graphene oxide-lanthanum hydroxide composite material | |
| CN105312028A (en) | Zinc and copper bi-metal organic framework material and preparation method and application thereof | |
| CN103627022A (en) | Method for preparing magnetic porous polystyrene microspheres on basis of suspension polymerization | |
| Wang et al. | Highly efficient and selective capture Pb (II) through a novel metal-organic framework containing bifunctional groups | |
| CN102489264A (en) | Chitosan magnetic nano particle as well as preparation method and application thereof | |
| CN102091605A (en) | Preparation and application of high-capacity magnetic mesoporous silica gel solid phase extracting agent | |
| CN102641753B (en) | Method for preparing magnetic strong-basicity ion exchange resin for removing organic matters in water | |
| CN110115984B (en) | Magnetic cyclodextrin-based cross-linked polymer adsorption material and preparation method thereof | |
| CN109621910A (en) | Nano zero valence iron-metal organic frame core-shell material preparation method and applications | |
| CN107930592A (en) | A kind of MOF magnetic graphenes hybrid material and its application in terms of chiral resolution and vitro cytotoxicity | |
| CN108176346A (en) | A kind of preparation method and application of the velvet-like polymolecularity carbonitride of magnetism swan | |
| CN104098729A (en) | Preparing method and application of MGO-MIP (Magnetic Graphene Oxide-Molecular Imprinting) composite material | |
| CN104984740A (en) | Preparation and application of cobalt ferrite-quasi-graphene carbon nano-composite magnetic adsorption material | |
| CN107008230A (en) | Magnetic composite adsorbent and preparation method thereof | |
| CN108927101A (en) | A kind of acicular nanometer FeOOH adsorbent and preparation method thereof | |
| CN108636360A (en) | A kind of preparation method and application of functionalized nano iron sulfide | |
| CN103341349A (en) | Imidazole and chitosan functional magnetic particle, as well as preparation method and application thereof | |
| CN105126916A (en) | Magnetic recyclable copper tetranitrophthalocyanine composite catalyst and application thereof in phenolic pollutant chromogenic recognition reaction | |
| El-Deen et al. | Recent developments in green magnetic nanoparticles for extraction and preconcentration of pollutants from environmental samples | |
| CN101811032B (en) | Preparation and application methods of Cd (II) imprinted magnetic material | |
| CN105502564A (en) | Adsorbent for selectively removing dye containing sulfonic acid group in wastewater and method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |