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Method for synthesizing monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline

A synthesis method, technology of nanocrystals, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc.

Inactive Publication Date: 2013-03-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is still a challenge to obtain stable monodisperse LDHs colloidal nanocrystals with easily controlled nanometer size.

Method used

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  • Method for synthesizing monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline
  • Method for synthesizing monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline
  • Method for synthesizing monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline

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Experimental program
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Embodiment 1

[0032] 1. Preparation of stable MgAl-LDH colloidal nanocrystal solution;

[0033] (1) Dissolve 10 mL containing 3 mmol MgCl 2 and 1 mmol AlCl 3 The mixed salt solution and 40 mL of 0.15 M NaOH solution were simultaneously poured into a high-speed rotating colloid mill for 10 min to obtain a white slurry;

[0034] (2) Centrifuge the white slurry at 12,000 rpm for 15 minutes and wash it with water three times;

[0035] (3) Add 40mL deionized water and stir until there are no large particles, then import it into a hydrothermal kettle and react in an oven at 100°C for 10 hours to obtain a stable transparent colloidal solution;

[0036] 2. Density gradient centrifugation:

[0037] (1) Make a density gradient: Use ethylene glycol and water to prepare 20%, 40%, 60%, 80%, and 100% ethylene glycol aqueous solutions by volume. Starting with ethylene glycol, slowly add 2 mL of the solution to the centrifuge tube in sequence to prepare a gradient solution.

[0038] (2) Add 1 mL of th...

Embodiment 2

[0044] 1. Preparation of stable MgAl-LDH colloidal nanocrystal solution;

[0045] (1) Dissolve 10 mL containing 3 mmol MgCl 2 and 1 mmol AlCl 3 The mixed salt solution and 40 mL of 0.15 M NaOH solution were simultaneously poured into a high-speed rotating colloid mill for 10 min to obtain a white slurry;

[0046] (2) Centrifuge the white slurry at 12,000 rpm for 15 min and wash it with water three times;

[0047] (3) Add 40 mL of deionized water and stir until there are no large particles, then import it into a hydrothermal kettle and react in an oven at 100 °C for 10 h to obtain a stable transparent colloidal solution;

[0048] 2. Density gradient centrifugation:

[0049] (1) Make a density gradient: Use ethylene glycol and water to prepare 20%, 40%, 60%, 80%, and 100% ethylene glycol aqueous solutions by volume. Starting with ethylene glycol, slowly add 0.8 mL of the solution to the centrifuge tube to prepare a gradient solution.

[0050] (2) Add 0.5 mL of the stable ...

Embodiment 3

[0054] 1. Preparation of stable MgAl-LDH colloidal nanocrystal solution;

[0055] (1) Dissolve 10 mL containing 3 mmol MgCl 2 and 1 mmol AlCl 3 The mixed salt solution and 40 mL of 0.15 M NaOH solution were simultaneously poured into a high-speed rotating colloid mill for 10 min to obtain a white slurry;

[0056] (2) Centrifuge the white slurry at 12,000 rpm for 15 min and wash it with water three times;

[0057] (3) Add 40 mL of deionized water and stir until there are no large particles, then introduce it into a hydrothermal kettle and react in an oven at 80 °C for 16 h to obtain a stable transparent colloidal solution;

[0058] 2. Density gradient centrifugation:

[0059] (1) Make a density gradient: Use ethylene glycol and water to prepare 20%, 40%, 60%, 80%, and 100% ethylene glycol aqueous solutions by volume. Starting with ethylene glycol, slowly add 2 mL of the solution to the centrifuge tube in sequence to prepare a gradient solution.

[0060] (2) Add 1 mL of t...

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Abstract

The invention relates to a preparation method for synthesizing relatively strict monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline. The preparation method mainly comprises the following steps of: 1, synthesizing the LDHs through a colloid mill to obtain white slurry, then centrifugally washing three times, transferring to a hydrothermal kettle, re-crystallizing to obtain a stable colloid solution; 2, respectively preparing density gradient medium solutions with different densities; 3, sequentially adding quantitative gradient solutions according to different densities in a centrifugal tube for preparing a step type density gradient solution; 4, slowly adding the prepared colloid solution on the liquid level of the density gradient solution, centrifuging under a certain condition; and 5, since colloid nano particles with different sizes have different sedimentation rates in the density gradient solutions, after centrifugation is stopped, the colloid nano particles remain in the gradient solutions with different densities, so that an effective method for preparing the monodisperse LDH nanocrystalline is provided. The high-monodispersity nano material has great potential application on the aspects of medicines, genetic vectors, polymer / LDHs biological nano composite materials, LDH films and the like.

Description

technical field [0001] The invention relates to a method for synthesizing monodisperse and stable LDHs colloidal nanocrystals obtained by using a density gradient centrifugation method to separate LDHs nanocrystals and study their properties, and belongs to the technical field of inorganic nanomaterial synthesis. Background technique [0002] Hydrotalcite (Layered Double Hydroxides, abbreviated as LDHs) is a kind of anionic layered compound, and its chemical expression can be expressed as [M 2+ (1-x) m 3+ x (OH)]A n- (x / n) ﹒ mH 2 O , where M 2+ with M 3+ With metal cations. If n = 0, the laminates are neutral and held together only by van der Waals interactions. Thanks to M 3+ (x = 0.33 - 0.167 ) slight substitution makes the lamina positively charged, and the anion ( A n - ) combined together, and the anion can be most inorganic and organic anions. Because of their adjustable structure and performance, they can be widely used in many fields and industries...

Claims

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Application Information

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IPC IPC(8): C01F7/02B82Y30/00
Inventor 孙晓明吴彩英常铮张国新邝允段雪
Owner BEIJING UNIV OF CHEM TECH
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