CN106378112A - Preparation method of amino-containing magnetic microspheres - Google Patents
Preparation method of amino-containing magnetic microspheres Download PDFInfo
- Publication number
- CN106378112A CN106378112A CN201611015101.1A CN201611015101A CN106378112A CN 106378112 A CN106378112 A CN 106378112A CN 201611015101 A CN201611015101 A CN 201611015101A CN 106378112 A CN106378112 A CN 106378112A
- Authority
- CN
- China
- Prior art keywords
- magnetic
- preparation
- amino
- microsphere
- deionized water
- 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.)
- Pending
Links
Classifications
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to the technical field of function materials, in particular to a preparation method of amino-containing magnetic microspheres. The preparation method of amino-containing magnetic microspheres comprises the following steps of (1) magnetofluid preparation; (2) magnetic microsphere preparation; (3) surface amino-containing magnetic microsphere preparation. The glycidyl methacrylate is used as a functional monomer; ethanediamine is used for modification; the amino functional magnetic polymer microspheres are prepared; the protonated amino groups have strong combination effects with acid orange 7 molecules through the electrostatic adsorption effects; in addition, magnetic adsorbents can be easily separated through external magnetic fields; therefore the problem of separation difficulty of a method through centrifugation or filtration and the like can be effectively solved.
Description
Technical field
The present invention relates to technical field of function materials is and in particular to a kind of preparation method containing amino-magnetic microsphere.
Background technology
With the fast development of printing and dyeing industry, substantial amounts of waste water from dyestuff has become one of major polluting sources of water environment.Dye
Material waste water is big because of complicated component, colourity depth, discharge capacity, and most of dyestuff and its metabolic intermediate have mutagenicity, cause
Carcinous and other toxicity, have become important polluter, serious to environmental and biological materials harm.In recent years, the place of waste water from dyestuff
Reason is increasingly subject to the attention of numerous scholars, and common minimizing technology has flocculence, biological degradation method, electrochemical process, absorption method etc.,
Wherein, absorption method, because it is easily handled, the features such as low cost and efficiency high, is widely used in processing waste water from dyestuff.Due to
Adsorbent has the big and abundant pore structure of its specific surface area, such as activated carbon, clay, zeolite and natural material etc., these
Adsorbent removes organic dye pollutant from aqueous solution and shows huge potentiality.But because these adsorbents have regeneration
This high and low flow velocity and separate, from waste water, the shortcomings of re-use difficult, so being subject to certain restrictions in application process, and magnetic
Property material then can be utilized externally-applied magnetic field centrifugation solves the problems, such as separate difficulty.
At present, magnetic material is used for the research report of various waste water from dyestuff advanced treating, magnetic poly phosphazene nanometer
Pipe, ethylenediamine modified magnetic chitin nanometer, the magnetic PDVB microsphere of sulfonation, mesoporous magnetic silica microballoon] etc.,
These magnetic materials show preferable absorption property in the adsorption process of dyestuff, and be easy to magnetic separation method reclaim and can be again
Raw recycling.Particularly the polymer microballoon containing functional group is increasingly favored by researcher, and this has benefited from easily right
Its modifying surface is so as to have the advantages that more excellent absorption property and high selectivity.Metering system ethylene oxidic ester
(GMA) contain vinyl and three-membered ring oxy radical, easily carry out radical polymerization and ring-opening reaction, and reactivity compares
Height, therefore Many researchers have carried out substantial amounts of research to the modification of PGMA.Using iminodiacetic acid, poly is changed
Property simultaneously have studied the absorption property to indium.It is prepared for poly (glycidyl methacrylate) microsphere, then polyethyleneimine is connect
Branch is in microsphere surface, and uses it for bilirubinic absorption.
Content of the invention
It is contemplated that proposing a kind of preparation method containing amino-magnetic microsphere.
Technical program of the present invention lies in：
Preparation method containing amino-magnetic microsphere, comprises the steps：
（1）The preparation of magnetic fluid
By n (Fe3+)∶n (Fe2+)=2: 1, by FeCl3And FeCl2It is stirred vigorously in the distilled water adding 100mL, completely molten
Xie Hou, is added in the there-necked flask equipped with thermometer and condensing tube, is passed through N simultaneously2;When maintaining the temperature at 60 DEG C, slowly
To pH value=9, after stirring at low speed 20min under 55 DEG C of constant temperature, Deca is dissolved in 30mL H to Deca NaOH2The 0.5g SDS of O and
1g PEG, constant temperature stirs 1h;Isolate Fe with Magnet3O4, repeatedly wash to solution ph=7 through deionized water, prepared magnetic current
Body；
（2）The preparation of magnetic microsphere
Add 3g polyethylene glycol 6000 and 100mL deionized water in the three-necked bottle of 250mL, at constant turn of 400r/min
It is allowed to be completely dissolved under speed；After temperature is increased to 55 DEG C, add above-mentioned magnetic fluid, rise temperature under nitrogen protection to 75 DEG C.So
After weigh 2.5g benzoyl peroxide in beaker, be separately added into 5mL PEGDA, 10 mLGMA and 1mL DVB are dissolved into
Mixed liquor, is slowly added dropwise mixed liquor into above-mentioned system, carries out polyreaction 5h；Obtain magnetic microsphere, deionized water cleaning 2 ~ 3
Secondary, vacuum drying；
（3）Surface contains the preparation of amino-magnetic microsphere
Accurately weigh the above-mentioned microsphere of 5g to pour in clean three-necked bottle, be separately added into 20mL DMF and 20mL ethylenediamine, connect
Condensing tube simultaneously assembles instrument, 75 DEG C of stirring 8h of constant temperature on magnetic stirring apparatuss；After reaction terminates, by products obtained therefrom deionized water
Cleaning 3 ~ 5 times, puts in baking oven and is dried, obtain modified magnetic microspheres.
The method have technical effect that：
It is function monomer that the present invention utilizes glycidyl methacrylate, and modified to it by ethylenediamine, is prepared for amino
The magnetic polymer microsphere of functionalization, the amino of protonation has stronger combination by electrostatic adsorption and acid orange 7 molecule
Effect；And magnetic adsorbent is easily isolated by externally-applied magnetic field, therefore efficiently solve by the method such as centrifugation or filtration
Separate difficult problem.
Specific embodiment
Preparation method containing amino-magnetic microsphere, comprises the steps：
（1）The preparation of magnetic fluid
By n (Fe3+)∶n (Fe2+)=2: 1, by FeCl3And FeCl2It is stirred vigorously in the distilled water adding 100mL, completely molten
Xie Hou, is added in the there-necked flask equipped with thermometer and condensing tube, is passed through N simultaneously2;When maintaining the temperature at 60 DEG C, slowly
To pH value=9, after stirring at low speed 20min under 55 DEG C of constant temperature, Deca is dissolved in 30mL H to Deca NaOH2The 0.5g SDS of O and
1g PEG, constant temperature stirs 1h;Isolate Fe with Magnet3O4, repeatedly wash to solution ph=7 through deionized water, prepared magnetic current
Body；
（2）The preparation of magnetic microsphere
Add 3g polyethylene glycol 6000 and 100mL deionized water in the three-necked bottle of 250mL, at constant turn of 400r/min
It is allowed to be completely dissolved under speed；After temperature is increased to 55 DEG C, add above-mentioned magnetic fluid, rise temperature under nitrogen protection to 75 DEG C.So
After weigh 2.5g benzoyl peroxide in beaker, be separately added into 5mL PEGDA, 10 mLGMA and 1mL DVB are dissolved into
Mixed liquor, is slowly added dropwise mixed liquor into above-mentioned system, carries out polyreaction 5h；Obtain magnetic microsphere, deionized water cleaning 2 ~ 3
Secondary, vacuum drying；
（3）Surface contains the preparation of amino-magnetic microsphere
Accurately weigh the above-mentioned microsphere of 5g to pour in clean three-necked bottle, be separately added into 20mL DMF and 20mL ethylenediamine, connect
Condensing tube simultaneously assembles instrument, 75 DEG C of stirring 8h of constant temperature on magnetic stirring apparatuss；After reaction terminates, by products obtained therefrom deionized water
Cleaning 3 ~ 5 times, puts in baking oven and is dried, obtain modified magnetic microspheres.
Claims (1)
1. contain amino-magnetic microsphere preparation method it is characterised in that：Comprise the steps：
（1）The preparation of magnetic fluid
By n (Fe3+)∶n (Fe2+)=2: 1, by FeCl3And FeCl2It is stirred vigorously in the distilled water adding 100mL, completely molten
Xie Hou, is added in the there-necked flask equipped with thermometer and condensing tube, is passed through N simultaneously2;When maintaining the temperature at 60 DEG C, slowly
To pH value=9, after stirring at low speed 20min under 55 DEG C of constant temperature, Deca is dissolved in 30mL H to Deca NaOH2The 0.5g SDS of O and
1g PEG, constant temperature stirs 1h;Isolate Fe with Magnet3O4, repeatedly wash to solution ph=7 through deionized water, prepared magnetic current
Body；
（2）The preparation of magnetic microsphere
Add 3g polyethylene glycol 6000 and 100mL deionized water in the three-necked bottle of 250mL, at constant turn of 400r/min
It is allowed to be completely dissolved under speed；After temperature is increased to 55 DEG C, add above-mentioned magnetic fluid, rise temperature under nitrogen protection to 75 DEG C；So
After weigh 2.5g benzoyl peroxide in beaker, be separately added into 5mL PEGDA, 10 mLGMA and 1mL DVB are dissolved into
Mixed liquor, is slowly added dropwise mixed liquor into above-mentioned system, carries out polyreaction 5h；Obtain magnetic microsphere, deionized water cleaning 2 ~ 3
Secondary, vacuum drying；
（3）Surface contains the preparation of amino-magnetic microsphere
Accurately weigh the above-mentioned microsphere of 5g to pour in clean three-necked bottle, be separately added into 20mL DMF and 20mL ethylenediamine, connect
Condensing tube simultaneously assembles instrument, 75 DEG C of stirring 8h of constant temperature on magnetic stirring apparatuss；After reaction terminates, by products obtained therefrom deionized water
Cleaning 3 ~ 5 times, puts in baking oven and is dried, obtain modified magnetic microspheres.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611015101.1A CN106378112A (en) | 2016-11-18 | 2016-11-18 | Preparation method of amino-containing magnetic microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611015101.1A CN106378112A (en) | 2016-11-18 | 2016-11-18 | Preparation method of amino-containing magnetic microspheres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106378112A true CN106378112A (en) | 2017-02-08 |
Family
ID=57959118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611015101.1A Pending CN106378112A (en) | 2016-11-18 | 2016-11-18 | Preparation method of amino-containing magnetic microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106378112A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107262054A (en) * | 2017-07-28 | 2017-10-20 | 江苏大学 | A kind of preparation method and applications of magnetic lignin base adsorbent |
| CN108283918A (en) * | 2018-02-13 | 2018-07-17 | 上海市刑事科学技术研究院 | Magnetic microsphere and its scared detection application |
| CN108467461A (en) * | 2018-02-28 | 2018-08-31 | 苏州为度生物技术有限公司 | The preparation method of surface carboxyl groups nucleocapsid superparamagnetism microballoon |
| CN108704587A (en) * | 2018-05-14 | 2018-10-26 | 苏州知益微球科技有限公司 | A kind of preparation method for the magnetic microsphere that monodisperse is amido modified |
| CN111013504A (en) * | 2019-12-11 | 2020-04-17 | 深圳先进技术研究院 | Surface modification method of magnetic polymer microspheres |
| CN112646092A (en) * | 2020-12-15 | 2021-04-13 | 南京亘闪生物科技有限公司 | Preparation method of magnetic microspheres with uniform particle size |
| CN113385149A (en) * | 2021-06-28 | 2021-09-14 | 西安理工大学 | Preparation method of amino modified magnetic cellulose adsorption material |
-
2016
- 2016-11-18 CN CN201611015101.1A patent/CN106378112A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107262054A (en) * | 2017-07-28 | 2017-10-20 | 江苏大学 | A kind of preparation method and applications of magnetic lignin base adsorbent |
| CN108283918A (en) * | 2018-02-13 | 2018-07-17 | 上海市刑事科学技术研究院 | Magnetic microsphere and its scared detection application |
| CN108283918B (en) * | 2018-02-13 | 2020-07-31 | 上海市刑事科学技术研究院 | Magnetic microsphere and hair detection application thereof |
| CN108467461A (en) * | 2018-02-28 | 2018-08-31 | 苏州为度生物技术有限公司 | The preparation method of surface carboxyl groups nucleocapsid superparamagnetism microballoon |
| CN108467461B (en) * | 2018-02-28 | 2020-06-05 | 苏州为度生物技术有限公司 | Preparation method of surface carboxyl core-shell superparamagnetic microspheres |
| CN108704587A (en) * | 2018-05-14 | 2018-10-26 | 苏州知益微球科技有限公司 | A kind of preparation method for the magnetic microsphere that monodisperse is amido modified |
| CN111013504A (en) * | 2019-12-11 | 2020-04-17 | 深圳先进技术研究院 | Surface modification method of magnetic polymer microspheres |
| CN111013504B (en) * | 2019-12-11 | 2021-11-26 | 深圳先进技术研究院 | Surface modification method of magnetic polymer microspheres |
| CN112646092A (en) * | 2020-12-15 | 2021-04-13 | 南京亘闪生物科技有限公司 | Preparation method of magnetic microspheres with uniform particle size |
| CN112646092B (en) * | 2020-12-15 | 2022-03-08 | 南京亘闪生物科技有限公司 | Preparation method of magnetic microspheres with uniform particle size |
| CN113385149A (en) * | 2021-06-28 | 2021-09-14 | 西安理工大学 | Preparation method of amino modified magnetic cellulose adsorption material |
| CN113385149B (en) * | 2021-06-28 | 2024-03-01 | 深圳万知达科技有限公司 | Preparation method of amino modified magnetic cellulose adsorption material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106378112A (en) | Preparation method of amino-containing magnetic microspheres | |
| CN102516679B (en) | Magnetic microsphere resin with high specific surface area and preparation method and application thereof | |
| CN104448131B (en) | A kind of preparation method of porous magnetic polyacrylamide PAM microsphere adsorbing agent | |
| CN101485973B (en) | Preparation and application of alginic acid polymer coated Fe3O4@C18 magnetic nano solid phase extractive agent | |
| CN100467120C (en) | Macroporous adsorption resin special used for separating antibiotic and its preparation method | |
| CN105664884A (en) | Magnetic adsorbent for removing heavy metal in water and method for preparing magnetic adsorbent | |
| CN107118354B (en) | Preparation method and application of ochratoxin metal organic framework-molecular imprinting composite separation medium | |
| CN105504331A (en) | Preparation method of porous integral material | |
| CN103159891B (en) | Magnetic amino-modified superhighly-crosslinked resin and preparation method thereof | |
| CN102659982A (en) | Flavone magnetic molecularly imprinted polymer, preparation of flavone magnetic molecularly imprinted polymer, and application of flavone magnetic molecularly imprinted polymer to bamboo-leaf flavone separation | |
| CN104226274A (en) | Adsorbing agent for removing petroleum type pollutants in environmental water sample and preparation method of adsorbing agent | |
| CN107632077A (en) | The quantitative approach of micro- plastics in a kind of percolate | |
| CN108970589A (en) | A kind of hydrotalcite plural gel ball and its preparation method and application | |
| CN104927063A (en) | Method for adsorbing and recycling phenolic compounds in industrial wastewater and method for manufacturing adsorption materials | |
| CN105129898B (en) | Renewable amino functional magnetic carbon nano-composite material and its preparation method and application | |
| Huang et al. | Efficient and selective capture of uranium by polyethyleneimine-modified chitosan composite microspheres from radioactive nuclear waste | |
| CN106868622B (en) | Nanofiber capable of being used for detecting tetracycline and preparation and application thereof | |
| CN103232572A (en) | Molecular imprinting polymer for roxarsone detection, and preparation method thereof | |
| CN106238010B (en) | A kind of chelating type metal ion floating agent, preparation method and its application method | |
| CN105295059B (en) | A kind of method of the chloromethylated polystyrene polymer and adsorption recovery Phenols In Industrial Liquid Waste class of immobilized cationization beta-cyclodextrin | |
| CN104311861A (en) | Method for adsorbing and recycling aromatic compound in industrial wastewater | |
| CN105854844B (en) | Arteannuic acid magnetic blotting microballoon and its preparation method and application | |
| CN111013554A (en) | Composite macroporous adsorption resin for removing perfluorinated compounds in water | |
| CN108250339A (en) | A kind of novel chelate resin material and its preparation method and application | |
| CN114225924A (en) | Method for recovering bismuth by using plant polyphenol modified adsorption resin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170208 |
|
| WD01 | Invention patent application deemed withdrawn after publication |