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Preparing method for thermosensitive magnetic composite microspheres

A technology of magnetic composite microspheres and magnetic microspheres, which is applied in the preparation of microspheres, the magnetism of organic materials/organic magnetic materials, and microcapsule preparations, and can solve the problem that the magnetic response performance of composite microspheres is not obvious and the magnetic response performance is not sensitive enough , Low monomer conversion rate and other issues, to achieve good magnetic response, good temperature sensitivity, and narrow molecular weight distribution

Active Publication Date: 2016-01-06
WUHAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The Chinese patent whose publication number is CN1454924 discloses a multifunctional organic-inorganic composite polymer microsphere and its preparation method, and the Chinese patent whose publication number is CN100575376C discloses a biocompatible magnetic thermosensitive nanoparticle and The disadvantage of its synthesis method is that the magnetic saturation intensity is relatively low and the magnetic response performance is not sensitive enough.
The disadvantages are that the organic monomers wrap the magnetic particles under the action of the cross-linking agent to obtain composite microspheres, and the magnetic particles and the organic matter are mostly combined with each other by physical cross-linking, covalent bonds, hydrogen bonds, and chelation. , the magnetic response performance of this composite microsphere is not obvious, and the monomer conversion rate is low

Method used

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  • Preparing method for thermosensitive magnetic composite microspheres
  • Preparing method for thermosensitive magnetic composite microspheres
  • Preparing method for thermosensitive magnetic composite microspheres

Examples

Experimental program
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Embodiment 1

[0032] Embodiment 1: as figure 1 , magnetic Fe 3 o 4 Preparation of microspheres: In a 500ml beaker, add 3.2436g FeCl 3 .6H 2 O, 2.164g urea, 7.056g trisodium citrate, 1.80g PAM (polyacrylamide) and 240ml deionized water, after mixing evenly, pour into four 80ml polytetrafluoroethylene reactors respectively, and react at 200°C for 12h. The obtained product was subjected to magnetic separation, the supernatant liquid was poured off, and magnetic separation was carried out after ultrasonic dispersion with ethanol and deionized water respectively, and repeated washing in this way, and dried at 80°C to obtain nano-core-shell structure Fe 3 o 4 magnetic microspheres.

[0033] Fe 3 o 4 -NH 2 Preparation of microspheres: In a 250ml three-neck flask, add 1.5g nano-core-shell structure Fe 3 o 4 Sonicate the magnetic microspheres and 100ml deionized water for 15min, adjust the pH of the solution to 10.20 with a concentration c=0.008M NaOH solution, activate at 55°C for 2.5h un...

Embodiment 2

[0044] Example 2: Fe 3 o 4 -NH 2 Preparation of microspheres: in a 250ml three-neck flask, add 0.4g of activated Fe in Example 1 3 o 4 Magnetic microspheres, the volume of ethanol and deionized water are 40ml / 40ml, ultrasonically dispersed for 15min, adjust the pH of the solution to 4.0 with glacial acetic acid, add 0.202ml of silane coupling agent KH-550, react at 55°C for 3h, wash with ethanol and deionized Washed several times with ion water and dried at 80°C to obtain Fe 3 o 4 -NH 2 The surface amino content of the microspheres measured by potentiometric titration is 497.05 μmol / g.

[0045] Fe 3 o 4 -NHCO-CH=CH 2 Preparation of microspheres: In a 250ml three-necked flask, 7ml of acrylic acid, 120mgEDC and 250mgNHS were dissolved in 30ml of deionized water, mechanically stirred at 3.4°C for 30min, and 0.75g of the above Fe 3 o 4 -NH 2 Disperse the microspheres in 150ml deionized water, ultrasonically disperse for 15min, add them to the flask, react for 1h, wash ...

Embodiment 3

[0048] Example 3: Fe 3 o 4 -NH 2 Preparation of microspheres: in a 250ml three-neck flask, add 0.4g of activated Fe in Example 1 3 o 4 The volume of microspheres, ethanol and deionized water are 55ml / 45ml respectively, ultrasonically disperse for 15min, adjust the pH of the solution to 4.0 with glacial acetic acid, add 0.606ml of silane coupling agent KH-550, react at 55°C for 3h, wash with ethanol and deionized Washed with water several times, dried at 80°C to obtain Fe 3 o 4 -NH 2 The surface amino content of the microspheres was measured by potentiometric titration to be 463.22 μmol / g.

[0049] Fe 3 o 4 -NHCO-CH=CH 2 Preparation of microspheres: In a 500ml three-necked flask, 15ml of acrylic acid, 300mgEDC and 500mgNHS were dissolved in 40ml of deionized water, mechanically stirred at 3.2°C for 30min, and 1.0g of the above Fe 3 o 4 -NH 2 Disperse the microspheres in 200ml deionized water, ultrasonically disperse for 15min, put them into the flask, react for 1h, ...

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Abstract

The invention discloses a preparing method for thermosensitive magnetic composite microspheres. Superparamagnetic microspheres are prepared through a hydrothermal method, subjected to surface modification through a silane coupling agent and then subjected to an amidogen carboxyl association reaction with unsaturated olefine acid to introduce double bonds; on the other hand, N-isopropylacrylamide or a derivative of the N-isopropylacrylamide serves as a monomer, sulfo ester serves as a chain transfer agent, a polymer with narrow molecular weight distribution is synthesized through a reversible addition-fragmentation chain transfer reaction under the action of an initiator, and then the prepared polymer is subjected to a reduction reaction under the effect of a nucleophilic reagent and a reducing agent; lastly, the thermosensitive magnetic composite microspheres are prepared through a click chemistry reaction. The microspheres have magnetic responsiveness and thermosensitivity, magnetic responsiveness is high, the saturated magnetic intensity ranges from 30 emu / g to 56.8 emu / g, and the particle size of the microspheres ranges from 290 nm to 590 nm. According to the preparing method, raw materials are easy to obtain, and the particle size of the prepared microspheres is controllable; the microspheres can be applied to the fields of medicine controlled release, intelligent separation and the like.

Description

technical field [0001] The invention relates to a preparation method of composite microspheres, in particular to a preparation method of temperature-sensitive and magnetic-responsive multifunctional organic-inorganic polymer composite microspheres. Background technique [0002] Magnetic polymer composite microspheres refer to polymer microspheres that contain magnetic metals or metal oxides and have magnetic response properties. On the one hand, magnetic polymer microspheres not only have the characteristics of ordinary polymer microspheres, for example, new functional groups can be endowed by means of surface modification, copolymerization and cross-linking; on the other hand, such polymer microspheres are Its unique magnetic responsiveness can reach the oriented region or separate under the action of an external magnetic field, making it very promising in the fields of biomedicine, bioengineering and cytology. [0003] The preparation of temperature-sensitive magnetic com...

Claims

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Application Information

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IPC IPC(8): C08F220/54C08F220/06C08F2/38C08F2/44C08K9/06C08K9/04C08K3/22H01F1/42B01J13/14
Inventor 戴红莲刘荣荣张平喻莹
Owner WUHAN UNIV OF TECH
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