A kind of magnetic carboxymethyl chitosan nano material and preparation method thereof
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A technology of carboxymethyl chitosan and nanomaterials, applied in the field of material science, can solve the problems of poor water solubility of chitosan, achieve the effects of avoiding self-aggregation and uneven distribution, improving stability, and good water solubility
Active Publication Date: 2018-01-05
SOUTH CHINA UNIV OF TECH
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Problems solved by technology
At present, Fe3O4 nanoparticles coated with chitosan have been successfully prepared, however, the water solubility of chitosan is not good.
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Embodiment 1
[0029] (1) To purify chitosan, add 5g of chitosan powder to submerge in 1% acetic acid solution, soak for 5h under magnetic stirring, separate the solution from solid to liquid, wash the solid twice with deionized water, and then wash the block The chitosan is dried at 70°C, and then pulverized into purified chitosan powder.
[0030] (2) Prepare carboxymethyl chitosan, take 50g sodium hydroxide solid, add 100mL ultrapure water to make solution, get the chitosan powder of 2g purification and add above-mentioned solution, magnetic stirring 3h, put into refrigerator and freeze overnight, Transfer the swollen sample into a 200mL three-neck flask, slowly add 20mL of isopropanol and stir evenly, take 1g of chloroacetic acid and add it into the flask in 4 times, with an interval of 20min each time, mechanically stir for 12h after adding all of them, filter out the isopropanol, and add an appropriate amount Dissolve in ultrapure water, adjust the pH to be neutral with dilute acetic ac...
Embodiment 2
[0036] Step (1) and (2) among the embodiment 1 are discarded, do not add carboxymethyl chitosan in the step (3), all the other steps are exactly the same as embodiment 1, make the nano iron ferric oxide that is wrapped nanomaterials.
[0037] like figure 1 As shown, there is no characteristic peak of carboxymethyl chitosan in the infrared spectrum, at 587cm -1 The absorption peak at is the vibration peak of Fe-O. The XRD test results are shown in figure 2 (b), the diffraction peaks appear at 2θ=30.24°, 35.40°, 43.48°, 53.64°, 57.04°, 62.68°, corresponding to the cubic phase Fe 3 o 4 (220), (311), (400), (422), (511) and (440) planes, which proves that the prepared crystals are mainly Fe 3 o 4 . The particle size and particle size distribution of the nanoparticles are as follows image 3 As shown in (b), the particle size is about 9nm, PDI=0.242.
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Abstract
The invention discloses a magnetic carboxymethyl chitosan nano-material and a preparation method thereof. The preparation method comprises 1, mixing a ferric iron salt and a ferrous salt according to a mole ratio of Fe<3+> to Fe<2+> of 1.5-2: 1 and adding water into the mixture to obtain a solution, 2, dissolving carboxymethyl chitosan in water to obtain a solution, mixing the solution and the solution obtained by the step 1, uniformly stirring the mixed solution and treating the mixed solution through microwave for a reaction under conditions of microwave power of 700-900W and a temperature of 70-85 DEG C for 30min, wherein in the reaction, ammonium hydroxide is dropwisely added into the reaction system so that pH is stabilized in a range of 8-9, and 3, after the reaction, cooling the reaction product to the room temperature, separating solid and liquid phases through a magnet, removing the liquid in the upper layer, washing the particles through deionized water until the particles have pH of 7, washing the particles through anhydrous ethanol, and carrying out freeze drying on the solid particles to obtain the magnetic carboxymethyl chitosan nano-material. The preparation method has simple processes and the magnetic carboxymethyl chitosan nano-material has the uniform particle size and good superparamagnetism.
Description
technical field [0001] The invention relates to a green method for rapidly preparing water-soluble carboxymethyl chitosan-wrapped nanometer iron tetroxide material by microwave method, which belongs to the field of material science. Background technique [0002] As a new material, nano-magnetic materials show special properties different from conventional magnetic materials in physical and chemical aspects due to their unique physical and chemical properties. Moreover, when the size of the nanomagnetic material is smaller than a critical value, it will exhibit superparamagnetism, that is, when a magnetic field is applied from the outside, the atoms in the magnetic domain and the magnetic moments of the crystal will be arranged in the same direction; , the net magnetic moment is zero, making the magnetism disappear. Among many superparamagnetic materials, superparamagnetic iron oxide particles are widely used in magnetic fluids, targeted drug delivery, sensors and magnetic r...
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