Preparation method and product of superparamagnetism nano particles
A magnetic nanoparticle and superparamagnetic technology, applied in the field of nanomaterials, can solve the problems of low adsorption capacity and low positive charge of natural proteins, and achieve improved stability and biocompatibility, short synthesis cycle, and adsorption capacity. strong effect
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[0026] The preparation method of superparamagnetic nanoparticles provided by the invention comprises the following steps:
[0027] (1) Under the condition of isolating oxygen, the Fe 3+ 、Al 3+ , Fe 2+ Evenly dispersed in water to form a precursor solution, so that Fe 3+ The concentration is between 0.05mol / L and 0.5mol / L, Fe 3+ and Fe 2+ The molar ratio of Fe is 2:1, Fe 3+ and Al 3+ The molar ratio is between 15:1 and 4:1.
[0028] (2) Under the condition of cutting off oxygen, keep stirring the precursor solution obtained in step (1), maintain the temperature at 30°C to 60°C, and slowly add lye dropwise to adjust the pH value of the solution to be greater than or equal to 9 to form a suspension ; Preferably, the stirring speed is 800rpm to 2000rpm, and the dropping rate of lye is 0.5mL / min to 4mL / min. The lye is sodium carbonate solution, ammonia solution or sodium hydroxide solution with pH ≥ 9.5. In order to make the product more evenly dispersed, citrate ions can ...
Embodiment 1
[0034] A preparation method of superparamagnetic nanoparticles, comprising the following steps:
[0035] (1) Take 250mL of ultrapure water, pass nitrogen gas for 10 minutes, then add 7.78g of FeCl in sequence 3 ·6H 2 O, 1.60g Al(NO 3 ) 3 9H 2 O and 2.86 g FeCl 2 4H 2 O, the Fe 3+ 、Al 3+ , Fe 2+ Evenly dispersed in water to form a precursor solution, so that Fe 3+ The concentration is 0.115mol / L, Fe 3+ and Fe 2+ The molar ratio of Fe is 2:1, Fe 3+ and Al 3+ The molar ratio is 6.4:1.
[0036] (2) Under the protection of nitrogen, keep stirring the precursor solution obtained in step (1), maintain the temperature at 40°C, and add 100mL of lye dropwise, the lye is 2mol / L ammonia solution, and the pH of the final solution is ≥9 , forming a suspension; the stirring speed is 1500rpm, and the dropping rate of lye is 2mL / min.
[0037](3) Under the protection of nitrogen, keep stirring the suspension obtained in step (2), and raise the temperature to 80°C, react for 0.5 h...
Embodiment 2
[0040] (1) Take 250mL of ultrapure water, pass nitrogen gas for 10 minutes, then add 20.27g of FeCl in sequence 3 ·6H 2 O, 7.03g Al(NO 3 ) 3 9H 2 O and 7.46 g FeCl 2 4H 2 O, the Fe 3+ 、Al 3+ , Fe 2+ Evenly dispersed in water to form a precursor solution, so that Fe 3+ The concentration is 0.3mol / L, Fe 3+ and Fe 2+ The molar ratio of Fe is 2:1, Fe 3+ and Al 3+ The molar ratio is 4:1.
[0041] (2) Under the protection of nitrogen, keep stirring the precursor solution obtained in step (1), maintain the temperature at 30°C, and add dropwise 200 mL of lye, which is 1 mol / L NaOH solution, and the final pH value of the solution is ≥9 , forming a suspension; the stirring speed is 2000rpm, and the dropping rate of the lye is 4mL / min. While adding the lye dropwise, use a 400kHz, 50W ultrasonic generator to supplement the entire reaction vessel with ultrasonic vibration.
[0042] (3) Under the protection of nitrogen, keep stirring the suspension obtained in step (2), and r...
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