Method for preparing nanoscale anionic laminar material continuously

A layered material and anion technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of non-continuous production, complex processing, high reaction temperature, etc., and achieve shortened nucleation induction period and particle size distribution The effect of narrowing and uniform particle size distribution

Inactive Publication Date: 2010-12-08
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN101665233 prepares layered double metal hydroxides with particles of 12-80nm, but the reaction requires high-energy autoclave crystallization and the addition of combustible sodium borohydride. The process is complex, the production cost is high, and it is difficult for large-scale industrial production
The nano-hydrotalcite particle size prepared by CN101538019 is between 30-70nm, but toluene extraction is required after the reaction, the follow-up treatment is complicated, and three wastes are generated
The preparation process of ZL01134425.3 magnesium-aluminum double hydroxyl compound metal oxide requires secondary reaction and crystallization, the process opera

Method used

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  • Method for preparing nanoscale anionic laminar material continuously
  • Method for preparing nanoscale anionic laminar material continuously
  • Method for preparing nanoscale anionic laminar material continuously

Examples

Experimental program
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Example Embodiment

[0017] Example 1

[0018] Such as figure 1 , figure 2 As shown, the preparation of 3.0L Mg 2+ The concentration is 0.0067mol / L, Al 3+ MgCl with a concentration of 0.0033mol / L 2 ·6H 2 O and AlCl 3 ·6H 2 O metal salt solution, press Mg 2+ With Al 3+ The molar ratio is 2 to form a soluble metal salt mixture, where Mg 2+ Is 0.0201mol, Al 3+ Is 0.0099mol; the preparation concentration is 0.1mol / L ammonium carbonate (NH 4 ) 2 CO 3 The solution is used as the precipitant solution, (NH 4 ) 2 CO 3 The amount of substance and the anion Cl in the soluble metal salt mixture - The total molar ratio is 0.5. The soluble metal salt mixture is added to the preheating tank of the spiral channel rotating bed supergravity reactor 4 and preheated to 20° C., valve 3 is closed, and valve 14 is opened. Start up the spiral channel type rotating bed supergravity reactor 4, and after the liquid flow rate in the spiral channel type rotating bed supergravity reactor 4 reaches 50L / h stable, transfer it to th...

Example Embodiment

[0019] Example 2

[0020] Such as figure 1 , figure 2 As shown, the preparation of 3.0L Mg 2+ The concentration is 0.04mol / L, Al 3+ MgCl with a concentration of 0.01mol / L 2 ·6H 2 O and AlCl 3 ·6H 2 O metal salt solution, press Mg 2+ With Al 3+ The molar ratio is 4 to form a soluble metal salt mixture, in which Mg 2+ 0.12mol, Al 3+ Is 0.03mol; the preparation concentration is 5.0mol / L ammonium carbonate (NH 4 ) 2 CO 3 The solution is used as the precipitant solution, (NH 4 ) 2 CO 3 The amount of substance and the anion Cl in the soluble metal salt mixture - The total molar ratio is 3. Add 0.5% Mg(OH) 2 The seed crystal is added to the soluble metal salt mixture, and the soluble metal salt and the seed crystal mixture are added to the preheating tank of the spiral channel rotating bed supergravity reactor 4 and preheated to 60°C, then close valve 3 and open valve 14. Start up the spiral channel type rotating bed supergravity reactor 4, after the liquid flow rate in the spiral cha...

Example Embodiment

[0021] Example 3

[0022] Such as figure 1 , figure 2 As shown, the preparation of 3.0L Mg 2+ The concentration is 0.075mol / L, Al 3+ The concentration of 0.025mol / L Mg(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 ·9H 2 O metal salt solution, press Mg 2 With Al 3+ The molar ratio is 3 to form a soluble metal salt mixture, where Mg 2+ 0.225mol, Al 3+ It is 0.075mol; the preparation concentration is 10.0mol / L urea as the precipitant solution, the amount of urea substance and the anion NO in the soluble metal salt mixture 3 - The total molar ratio is 5. Add 3.0% MgO seed crystals to the soluble metal salt mixture, and add the soluble metal salt and seed crystal mixture to the preheating tank of the spiral channel rotating bed supergravity reactor 4, and then close it after preheating to 95°C Valve 3, open valve 14. Start up the spiral channel type rotating bed supergravity reactor 4, and after the liquid flow rate in the spiral channel type rotating bed supergravity reactor 4 reaches 700L / h an...

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Abstract

The invention discloses a method for preparing a nanoscale anionic laminar material continuously, which mainly comprises the steps of reacting, filtering, washing and drying. Compared with the conventional method for preparing the anionic laminar material in China, the method has the following advantages: (1) a helix channel rotating bed high gravity reactor is adopted to enable nucleus formation to be formed in a uniform micro hybrid environment quickly with a narrowed particle size distribution, the reaction solution in the reactor is kept under a stable high pH value condition by condensing NH3 so as to avoid generating an impurity phase, the reaction time is short and the operation is simple; (2) crystal seeds are added during reaction to greatly reduce the induction period of nucleus formation and accelerate nucleus formation, the crystallinity is high, the particle size distribution is more uniform, the size and distribution of newly generated particles can be controlled according to the particle size of the added crystal seeds, and thus, the particle size is controllable; (3) a crystallization process is not required for product post processing; and (4), the process is quick and allows for continuous production, and the average particle size of the prepared anionic laminar material is 30 to 90 nanometers.

Description

technical field [0001] The invention relates to a method for continuously preparing nanoscale anion layered materials, in particular to a method for continuously preparing nanoscale anion layered materials with uniform particle size distribution under supergravity conditions. Background technique [0002] As a new type of anionic clay material, anionic layered materials have broad application prospects in many fields such as catalysis, adsorption, flame retardancy, medicine, electronics and environmental protection. At present, the relatively mature preparation method in China is the co-precipitation method, but due to the uneven microscopic mixing of the co-precipitation method, it is easy to cause nucleation and crystallization to proceed at the same time, resulting in heterogeneous phases, resulting in uneven grain size of the product. At the same time, follow-up treatment such as crystallization is required, and the crystallization time is long. For example, in CN128807...

Claims

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Application Information

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IPC IPC(8): C01B13/36
Inventor 曾虹燕赵策王亚举黄炎杨永杰魏英民
Owner XIANGTAN UNIV
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