CN108043336A - A kind of dendrimer modified magnetic microballoon of uniform particle sizes and its preparation method and application - Google Patents
A kind of dendrimer modified magnetic microballoon of uniform particle sizes and its preparation method and application Download PDFInfo
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- CN108043336A CN108043336A CN201711144386.3A CN201711144386A CN108043336A CN 108043336 A CN108043336 A CN 108043336A CN 201711144386 A CN201711144386 A CN 201711144386A CN 108043336 A CN108043336 A CN 108043336A
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
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Abstract
Magnetic microsphere modified the present invention relates to the dendrimer of uniform particle sizes a kind of and its preparation method and application, the magnetic microsphere is obtained by introducing dendrimer in surfaces of magnetic carriers, the magnetic carrier is magnetic nano-particle or magnetic micrometer particle.Dendrimer is directly dispersed in the solution of synthesizing magnetic microballoon by its preparation method, and the magnetic microsphere of dendrimer modification is directly synthesized by hydrothermal synthesis one kettle way.The magnetic microsphere of the present invention has better accumulation ability, and magnetic microsphere grain size is uniform, and production method is simple, and the magnetic microsphere of dendrimer modification is can obtain without modifying afterwards.
Description
Technical field
The present invention relates to functionalization Material Fields, and in particular to a kind of magnetism of the dendrimer modification of uniform particle sizes
Microballoon and its preparation method and application.
Background technology
Magnetic microsphere includes magnetic nano-particle and micro particles, due to its special physicochemical properties, makes it in material
The fields such as material, biology, which exist, is widely applied prospect, such as Magneto separate, the transport of drug magnetic targeted etc..It is different in order to adapt to
Purposes, using various modified magnetic microspheres and its composite construction, such as the magnetic microsphere that functionalized silicon coats, polymer connects
The materials such as the modified magnetic microsphere of branch are widely prepared and are on the actual application.The functional magnetic usually prepared
Microsphere surface group content is relatively low, it is necessary to be detected and characterized with highly sensitive detection method, such as fluorescence [referring to
Chem.Eur.J.2006,12,6341].Therefore, development prepares the method for the magnetic microsphere that surface functional group enriches for carrying
The application effect and application range of high magnetic microsphere have great importance.
Dendrimer have the characteristics that it is highly branched, with multi-functional group and with good solubility, in nanometer
Material preparation and bio-medical etc., which exist, is widely applied prospect.The preparation side of the magnetic microsphere of dendrimer modification
Method has been reported [CN101955231B, CN103157447B], but generally use be after modify method, step is more, and time-consuming.
CN102092795A reports a kind of preparation method of the ferroso-ferric oxide multi-stage ball of organic polymer modification, but by
It is uneven in its grain size, its performance, such as poor reproducibility can be influenced in specific application.
The content of the invention
In view of the above-mentioned problems, the invention discloses a kind of uniform particle sizes, dendrimer modification prepared by one-step method
Magnetic microsphere and its preparation method and application, to meet the needs in different application field.
For such purpose, we are using dendrimer as dressing agent, using ethylene glycol as reaction dissolvent, and in reactant
Anhydrous sodium acetate is added in system to increase electrostatic stabilization effect, prevents magnetic nanoparticle from reuniting, grain size is prepared using hydro-thermal method
The magnetic microsphere of uniform dendrimer modification.
A kind of dendrimer modified magnetic microballoon for providing uniform particle sizes of the present invention, the magnetic microsphere pass through
Dendrimer is introduced in surfaces of magnetic carriers to obtain；The magnetic carrier is magnetic nano-particle or magnetic micrometer grain
Son.
Preferably, the dendrimer is the dendrimer that end group is amino.
It is furthermore preferred that the dendrimer is polyamide-amide dendrimer.
It is further preferred that the dendrimer is any generation in the 0th generation to the 7th generation.
The present invention also provides a kind of preparation method of the dendrimer modified magnetic microballoon of uniform particle sizes, the sides
Method comprises the following steps：
S100, the solution for preparing synthesizing magnetic microballoon
S200, dendrimer is dispersed in the solution of synthesizing magnetic microballoon；
S300, the mixed solution for being obtained step S200 by hydrothermal synthesis one kettle way synthesize what dendrimer was modified
Magnetic microsphere.
Wherein, the solution of the synthesizing magnetic microballoon is：Uniform dissolution is in 20.0-50.0 parts by weight ethylene glycol solutions
1.0-5.0 parts by weight generate iron compound, the 2-10 parts by weight anhydrous sodium acetates of magnetic carrier.
Alternatively, the solution of the synthesizing magnetic microballoon is：Uniform dissolution is in 20.0-50.0 parts by weight ethylene glycol solutions
Cobalt compound, the 2-10 parts by weight anhydrous sodium acetates of 2.0-10.0 parts by weight.
The dosage of the dendrimer is 0.5-5.0 parts by weight.
Preferably, the hydrothermal synthesis one kettle way can comprise the following steps：
S301, the mixed solution is transferred to hydrothermal reaction kettle, 180 to 250 DEG C of hydrothermal temperature, the reaction time is
When 6-10 is small；
S302, the magnetic microsphere that will be prepared, methanol clean 3-5 times, and ethyl alcohol cleans 3-5 times, and water cleans 3-5 times, then
Ethyl alcohol cleans 3-5 times；
S303, by the magnetic microsphere after cleaning in 50 DEG C vacuum drying 12 it is small when it is spare.
Preferably, the hydrothermal synthesis one kettle way can also comprise the following steps：
S311, the mixed solution is transferred to hydrothermal reaction kettle, 200 to 350 DEG C of hydrothermal temperature, the reaction time is
When 6-10 is small；
S312, the magnetic microsphere that will be prepared, methanol clean 3-5 times, and ethyl alcohol cleans 3-5 times, and water cleans 3-5 times, then
Ethyl alcohol cleans 3-5 times；
The present invention also provides a kind of applications of dendrimer modified magnetic microballoon, and foregoing dendrimer is repaiied
Decorations magnetic microsphere is transported applied to Magneto separate, sewage disposal and drug magnetic targeted.
Compared with the existing technology, the magnetic microsphere preparation method step of dendrimer of the invention modification is few, simply
It is easy, uniform particle sizes.The magnetic microsphere of dendrimer modification obtained is dispersed in aqueous solution or alcoholic solution and stablizes
Property is good.Transport that there is huge application prospects with each side such as Magneto separate in sewage disposal, drug magnetic targeted.
Description of the drawings
The transmission electron microscope picture of the magnetic ferroferric oxide microballoon of the PAMAM dendrimers modification of Fig. 1 forth generations；
The oxidation of magnetism four three modified in Fig. 2 one embodiment of the invention on the PAMAM dendrimers of forth generation
The infrared schematic diagram of iron microballoon；
To adenosine after the magnetic ferroferric oxide microballoon modification boric acid of the PAMAM dendrimers modification of Fig. 3 forth generations
Extraction quantity (3 in Fig. 3), and background document Chem.Eur.J.2006, the amino functional prepared in 12,6341. documents is magnetic
The prepared after microballoon modification boric acid to modification method after in the extraction quantity (1 in Fig. 3) of adenosine, background document CN 103157447B
Signal is compared to the extraction quantity (2 in Fig. 3) of adenosine after the magnetic microsphere modification boric acid of the PAMAM dendrimers modification in four generations
Figure.
Specific embodiment
The disclosure is described in further detail with embodiment shown in 1-3 below in conjunction with the accompanying drawings.It is understood that this
Locate described specific embodiment to be only used for explaining related content rather than the restriction to the disclosure.It also should be noted that
For ease of description, illustrated only in attached drawing 1-3 and the relevant part of the disclosure.
1-3 and it is described in detail the disclosure in conjunction with the embodiments below with reference to the accompanying drawings.
An embodiment provided by the invention is the dendrimer modified magnetic microballoon of uniform particle sizes a kind of, described
Magnetic microsphere is obtained by introducing dendrimer in surfaces of magnetic carriers；The magnetic carrier for magnetic nano-particle or
Person's magnetic micrometer particle.
An aspect of of the present present invention, the dendrimer are the dendrimer that end group is amino, are preferably
Polyamide-amide dendrimer.
It is furthermore preferred that the dendrimer is any generation in the 0th generation to the 7th generation.
The present invention also provides a kind of preparation method of the dendrimer modified magnetic microballoon of uniform particle sizes, the sides
Method comprises the following steps：S100, the solution for preparing synthesizing magnetic microballoon；S200, dendrimer is dispersed in synthesis
In the solution of magnetic microsphere；S300, the mixed solution for being obtained step S200 by hydrothermal synthesis one kettle way synthesize dendroid height
The magnetic microsphere of molecular modification.As Fig. 1 forth generations PAMAM dendrimers modify magnetic ferroferric oxide microballoon it is saturating
Penetrate electron microscope；To gland after the magnetic ferroferric oxide microballoon modification boric acid that PAMAM dendrimers such as Fig. 3 forth generations are modified
The extraction quantity (3 in Fig. 3) of glycosides, and background document Chem.Eur.J.2006, the amino functional magnetic prepared in 12,6341. documents
Property microballoon modification boric acid after it is prepared by modification method after in the extraction quantity (1 in Fig. 3) of adenosine, background document CN103157447B the
Signal is compared to the extraction quantity (2 in Fig. 3) of adenosine after the magnetic microsphere modification boric acid of the PAMAM dendrimers modification in four generations
Figure.
Another aspect of the present invention, the solution of the synthesizing magnetic microballoon can be：Uniform dissolution is in 20.0-50.0 weight
Iron compound, the 2-10 parts by weight anhydrous sodium acetates of 1.0-5.0 parts by weight generation magnetic carrier in part ethylene glycol solution.
Another aspect of the present invention, the solution of the synthesizing magnetic microballoon can also be：Uniform dissolution is in 20.0-50.0 weights
Measure cobalt compound, the 2-10 parts by weight anhydrous sodium acetates of the 2.0-10.0 parts by weight in part ethylene glycol solution.
One aspect of the present invention, the dosage of the dendrimer is 0.5-5.0 parts by weight.
Another aspect of the present invention, the hydrothermal synthesis one kettle way can comprise the following steps：S301, by it is described mixing it is molten
Liquid is transferred to hydrothermal reaction kettle, 180 to 250 DEG C of hydrothermal temperature, when the reaction time is 6-10 small；S302, will be prepared
Magnetic microsphere, methanol clean 3-5 time, ethyl alcohol clean 3-5 time, water cleaning 3-5 times, then ethyl alcohol cleaning 3-5 times；S303, incite somebody to action clearly
Magnetic microsphere after washing is spare when 50 DEG C of vacuum drying 12 are small.
Another aspect of the present invention, the hydrothermal synthesis one kettle way can also comprise the following steps：S311, by the mixing
Solution is transferred to hydrothermal reaction kettle, 200 to 350 DEG C of hydrothermal temperature, when the reaction time is 6-10 small；S312, will be prepared into
The magnetic microsphere arrived, methanol clean 3-5 times, and ethyl alcohol cleans 3-5 times, and water cleans 3-5 times, then ethyl alcohol cleans 3-5 times；Such as Fig. 2 sheets
The infrared of magnetic ferroferric oxide microballoon modified in invention one embodiment on the PAMAM dendrimers of forth generation is shown
It is intended to.
The present invention also provides a kind of applications of dendrimer modified magnetic microballoon, and foregoing dendrimer is repaiied
Decorations magnetic microsphere is transported applied to Magneto separate, sewage disposal and drug magnetic targeted.
The present invention is illustrated in further detail below by way of specific embodiment, and the explanation of following embodiment is only intended to help to understand
The method and its core concept of the present invention.
Embodiment 1：Fe 3 O 4 magnetic microballoon is obtained according to following preparation methods：
The ferric chloride hexahydrate of 1.0 parts by weight, 2.0 parts by weight anhydrous sodium acetates, the PAMAM branches of 1 parts by weight forth generation
Shape macromolecule is dissolved in successively in 35.0 parts by weight ethylene glycol solutions, is uniformly mixed, is transferred to hydrothermal reaction kettle, hydro-thermal reaction
200 DEG C of temperature.When reaction time is 6 small.The magnetic microsphere that will be prepared, methanol clean 3-5 times, and ethyl alcohol cleans 3-5 times, water
Cleaning 3-5 times, ethyl alcohol clean 3-5 times.It is spare when 50 DEG C of vacuum drying 12 are small.
As shown in Figure 1, the magnetic ferroferric oxide microballoon that the PAMAM dendrimers that Fig. 1 is the forth generation are modified
Transmission electron microscope picture, it can be seen that its uniform particle sizes, about 100nm from figure.
The infrared figure for the magnetic ferroferric oxide microballoon that Fig. 2 modifies for the PAMAM dendrimers of forth generation, 580cm-1
Be Fe-O characteristic absorption peak proof generate magnetic ferroferric oxide microballoon, characteristic absorption peak 1642cm-1, 1549cm-1With
1048cm-1PAMAM modifications are demonstrated to magnetic ferroferric oxide microsphere surface.
Embodiment 2：Prepare cobalt oxide magnetic microsphere：
The cobalt chloride hexahydrate of 2.0 parts by weight, 10 parts by weight anhydrous sodium acetates, 2 parts by weight dendrimers are molten successively
Solution is uniformly mixed in 45 parts by weight ethylene glycol solutions, is transferred to hydrothermal reaction kettle, 300 DEG C of hydrothermal temperature.Reaction time
For 8 it is small when.The magnetic microsphere that will be prepared, methanol clean 3-5 times, and ethyl alcohol cleans 3-5 times, and water cleans 3-5 times, ethyl alcohol cleaning
3-5 times.It is spare when 50 DEG C of vacuum drying 12 are small.
Embodiment 3：Magnetic Isolation application experiment
The oxidation of magnetism four three that the PAMAM dendrimers of the forth generation prepared according to the method for embodiment 1 are modified
The upper phenyl boric acid of iron microballoon and 4- formylphenylboronic acids reaction modification, extracts adenosine solution that (boric acid functionalization material can be with
Extract adenosine), calculate material to the extraction quantity (3 in Fig. 3) of adenosine, while with ammonia in background document (CN 103157447B)
The forth generation prepared after base functional magnetic material modification boric acid to the extraction quantity (1 in Fig. 3) of adenosine and rear modification method
The magnetic ferroferric oxide microballoon of PAMAM dendrimers modification compares the extraction quantity (2 in Fig. 3) of adenosine, from
After Fig. 3 can be seen that the upper phenyl boric acid of magnetic microsphere modification of the method for the present invention preparation, the extraction quantity increase by 58% to adenosine, and
And preparation process is simpler easy compared with the prior art, more fast.
Comparative example 1：The ferroso-ferric oxide that organic polymer modification is prepared for using method disclosed in CN102092795A is more
Grade ball.
It is as follows that embodiment 1 compares difference with comparative example 1：
| Embodiment 1 | Comparative example 1 | |
| Preparation time | 6 it is small when | When 12-72 is small |
| Grain size | (100±5)nm | (250±50)nm |
| Particle uniformity coefficient | Uniformly | It is uneven |
By comparing it can be found that dendrimer modified magnetic microballoon ratio comparison prepared by method using the present invention
Shorter the time required to example 1, grain size evenly, and uses the time of the magnetic microsphere needs of the method preparation of comparative example 1 long, from text
The attached drawing 1 for offering CN102092795A can be seen that its uniform particle sizes' degree is poor.
The present invention is described in detail above, specific case used herein is to the principle of the present invention and embodiment party
Formula is set forth, and the explanation of above example is only intended to help to understand method and its core concept of the invention；It is meanwhile right
In those skilled in the art, thought according to the invention, there will be changes, comprehensive in specific embodiments and applications
Upper described, this specification content should not be construed as limiting the invention.
Claims (10)
1. a kind of dendrimer modified magnetic microballoon of uniform particle sizes, it is characterised in that：
The magnetic microsphere is obtained by introducing dendrimer in surfaces of magnetic carriers；
The magnetic carrier is magnetic nano-particle or magnetic micrometer particle.
2. dendrimer modified magnetic microballoon according to claim 1, which is characterized in that preferred, the branch
Shape macromolecule is the dendrimer that end group is amino, is preferably polyamide-amide dendrimer.
3. dendrimer modified magnetic microballoon according to claim 1, which is characterized in that the dendroid high score
Son is any generation in the 0th generation to the 7th generation.
4. as right requires the preparation side of the dendrimer modified magnetic microballoon of 1-3 any one of them uniform particle sizes
Method, which is characterized in that comprise the following steps：
S100, the solution for preparing synthesizing magnetic microballoon
S200, dendrimer is dispersed in the solution of synthesizing magnetic microballoon；
S300, the mixed solution for being obtained step S200 by hydrothermal synthesis one kettle way synthesize the magnetism that dendrimer is modified
Microballoon.
5. according to the method described in claim 4, it is characterized in that, the solution of the synthesizing magnetic microballoon is：
The iron chemical combination of 1.0-5.0 parts by weight generation magnetic carrier of the uniform dissolution in 20.0-50.0 parts by weight ethylene glycol solutions
Object, 2-10 parts by weight anhydrous sodium acetates.
6. according to the method described in claim 4, it is characterized in that, the dosage of the dendrimer is 0.5-5.0 weight
Part.
7. method according to claim 5 or 6, which is characterized in that the hydrothermal synthesis one kettle way comprises the following steps：
S301, the mixed solution is transferred to hydrothermal reaction kettle, 180 to 250 DEG C of hydrothermal temperature, reaction time 6-10
Hour；
S302, the magnetic microsphere that will be prepared, are cleaned 3-5 times with methanol, and ethyl alcohol cleans 3-5 times, and water cleans 3-5 times, then uses
Ethyl alcohol cleans 3-5 times；
S303, by the magnetic microsphere after cleaning in 50 DEG C vacuum drying 12 it is small when it is spare.
8. according to the method described in claim 4, it is characterized in that, the solution of the synthesizing magnetic microballoon is：
The cobalt compound of 2.0-10.0 parts by weight of the uniform dissolution in 20.0-50.0 parts by weight ethylene glycol solutions, 2-10 weight
Part anhydrous sodium acetate.
9. according to the method described in claim 8, it is characterized in that, the hydrothermal synthesis one kettle way comprises the following steps：
S311, the mixed solution is transferred to hydrothermal reaction kettle, 200 to 350 DEG C of hydrothermal temperature, reaction time 6-10
Hour；
S312, the magnetic microsphere that will be prepared, are cleaned 3-5 times with methanol, and ethyl alcohol cleans 3-5 times, and water cleans 3-5 times, then uses
Ethyl alcohol cleans 3-5 times；
S313, by the magnetic microsphere after cleaning in 50 DEG C vacuum drying 12 it is small when it is spare.
10. according to any one of claim 1-3 any one of them dendrimer modified magnetic microballoon or claim 4-9
The application of dendrimer modified magnetic microballoon prepared by the method, which is characterized in that repair the dendrimer
Decorations magnetic microsphere is transported applied to Magneto separate, sewage disposal and drug magnetic targeted.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112250884A (en) * | 2020-08-21 | 2021-01-22 | 江苏省农业科学院 | Dendritic polymeric antibacterial peptide and preparation method and application thereof |
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| CN101955231A (en) * | 2010-10-20 | 2011-01-26 | 华东师范大学 | Preparation method of surface dendritic macromolecule modified superparamagnetism ferroferric oxide nano particle |
| CN103285838A (en) * | 2013-07-02 | 2013-09-11 | 景德镇陶瓷学院 | Preparation method of functional magnetic absorbent used for treating industrial wastewater |
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2017
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| CN101901659A (en) * | 2010-07-30 | 2010-12-01 | 北京化工大学 | Preparation method of magnetic nanoparcles modified with surface functional groups |
| CN101955231A (en) * | 2010-10-20 | 2011-01-26 | 华东师范大学 | Preparation method of surface dendritic macromolecule modified superparamagnetism ferroferric oxide nano particle |
| CN103285838A (en) * | 2013-07-02 | 2013-09-11 | 景德镇陶瓷学院 | Preparation method of functional magnetic absorbent used for treating industrial wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112250884A (en) * | 2020-08-21 | 2021-01-22 | 江苏省农业科学院 | Dendritic polymeric antibacterial peptide and preparation method and application thereof |
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