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Method for centrifugally separating oil soluble nano particles by organic density gradient

A nanoparticle and density gradient technology is applied in the field of advanced nanomaterial separation technology to achieve a wide range of separation sizes, simple purification and good separation effect.

Active Publication Date: 2010-05-26
青岛搏流创新科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Then can we choose two organic solvents with different densities, mix them in different proportions, and then make a density gradient to separate oil-soluble nanoparticles? So far, no examples of separations in organic phases have been reported

Method used

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  • Method for centrifugally separating oil soluble nano particles by organic density gradient
  • Method for centrifugally separating oil soluble nano particles by organic density gradient
  • Method for centrifugally separating oil soluble nano particles by organic density gradient

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) First, use 10mg / ml of HAuCl 4 The oleylamine solution was reacted with 10ml cyclohexane at 80°C for 10h to generate a cyclohexane colloidal solution of about 1mg / ml Au nanoparticles.

[0026] (2) Make a density gradient: use carbon tetrachloride and cyclohexane to prepare 50%, 60%, 70%, 80%, and 90% carbon tetrachloride-cyclohexane solutions by volume. Starting from 90%, gradually take 2ml of the solution and gently add it to the centrifuge tube to prepare a gradient solution.

[0027] (3) Add 0.4 ml cyclohexane dispersion of Au nanoparticles to the gradient liquid.

[0028] (4) 15°C, 100×10 -6 Atmospheric pressure, 25000rpm, high-speed centrifugation under the condition of 10min.

[0029] (5) Divide the centrifuged mixture into 16 parts, and suck it out from the top with a pipette. Finally, Au nanoparticle dispersions with different sizes were obtained.

[0030] For separation results, see figure 1 ,2.

[0031] Change the separation conditions, change the de...

Embodiment 2

[0033] (1) First, use 10mg / ml of HAuCl 4 5ml of oleylamine solution was reacted with 5ml of cyclohexane at 50°C for 72h to generate a colloidal solution of about 5mg / ml Au nanowires / nanoparticles.

[0034] (2) Preparation of density gradient: use carbon tetrachloride and cyclohexane to prepare 50%, 60%, 70%, 80%, 90% carbon tetrachloride-cyclohexane solutions by volume. Starting from 90%, gradually take 2ml of the solution and gently add it to the centrifuge tube to prepare a gradient solution.

[0035] (3) Add 0.4 ml of the synthesized Au nanowire / nanoparticle colloidal solution to the gradient solution.

[0036] (4) 15°C, 100×10 -6 Atmospheric pressure, 30000rpm, high-speed centrifugation under the condition of 18min.

[0037] (5) Divide the centrifuged mixture into 26 parts, and suck it out from the top with a pipette. Finally, nanoparticle dispersions with different sizes and shapes are obtained.

[0038] For separation results, see image 3

[0039] Change the sepa...

Embodiment 3

[0041] (1) First, take 2ml of Fe wrapped in oleic acid 3 o 4 The cyclohexane colloidal solution of nanoparticles was ultrasonicated for 4 hours, and the water was changed every half hour.

[0042] (2) Make a density gradient: use carbon tetrachloride and cyclohexane to prepare 50%, 60%, 70%, 80%, and 90% carbon tetrachloride-cyclohexane solutions by volume. Starting from 90%, gradually take 2ml of the solution and gently add it to the centrifuge tube to prepare a gradient solution.

[0043] (3) Add 0.4ml of Fe 3 o 4 A colloidal solution of nanoparticles is added to the gradient.

[0044] (4) 15°C, 100×10 -6 Atmospheric pressure, 35000rpm, high-speed centrifugation under the condition of 35min.

[0045] (5) Divide the centrifuged mixture into 20 parts, and suck it out from the top with a pipette. Finally, Fe with different sizes is obtained 3 o 4 nanoparticle dispersion.

[0046] For separation results, see Figure 4

[0047] Change the separation conditions, change...

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Abstract

The invention relates to a method for centrifugally separating oil soluble nano particles by organic density gradient. The method comprises the following steps: 1) directly synthesizing nano particle colloidal solution, or carrying out ultrasonic and stirring and other methods on the nano particles in organic solvent to prepare colloidal nano particle solution with transparent homogeneity; 2) preparing organic density gradient medium by mixing organic solvent or high-molecular solution with different densities; 3) adding organic density gradient medium with different concentrations to a centrifuge tube in turn to prepare organic density gradient; and 4) adding the colloidal solution of nano particles into the organic density gradient for centrifuging. As the sedimentation rate of the nanoparticles with different sizes and appearances in the organic density gradient solution is different, the nano particles are retained at different positions of the organic density gradient solution, thus achieving the effect of separation. The invention has the advantage of volatilizing the organic solvent to obtain the monodisperse nano particles; the method of the invention is simple and rapid,is influenced little by the stability and purity of the sample, and the centrifuging effect can be strengthened by adjusting the centrifugal parameter.

Description

technical field [0001] The invention relates to a method for separating oil-soluble oil-soluble precious metals and semiconductor nanoparticles, in particular to a method for separating oil-soluble nanoparticles by organic density gradient high-speed centrifugation, which belongs to the technical field of advanced nanomaterial separation technology. Background technique [0002] Because of its size effect, the physical and chemical properties of nanomaterials are very different from those of ordinary materials, resulting in special physical and chemical properties in terms of light, electricity, and heat. Such excellent properties of nanomaterials have a great relationship with their size, so the acquisition of nanoparticles with a single size is of great significance to the application and development of nanomaterials. [0003] At present, although there are many nanomaterial synthesis methods, and some can even synthesize monodisperse nanoparticles with a single size, the ...

Claims

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Application Information

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IPC IPC(8): B03B5/32
Inventor 孙晓明白露
Owner 青岛搏流创新科技有限公司
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