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Method used for preparing layered double metal hydroxides through mechanical ball milling

A layered bimetallic and hydroxide technology, applied in the direction of oxygen/ozone/oxide/hydroxide, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of poor crystallinity of products and achieve good crystallinity and purity High, low-cost effect

Inactive Publication Date: 2019-01-11
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One-step dry ball milling uses metal salts, oxides and hydroxides as raw materials without introducing any solvent to obtain LDHs. This method is simple and convenient but has the disadvantage of poor crystallinity of the product
One-step wet ball milling uses metal salt solution as raw material to prepare LDHs, but it is currently limited to the preparation of iron-based LDHs

Method used

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  • Method used for preparing layered double metal hydroxides through mechanical ball milling
  • Method used for preparing layered double metal hydroxides through mechanical ball milling
  • Method used for preparing layered double metal hydroxides through mechanical ball milling

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Take 0.7624g MgCl 2 •6H 2 O with 0.3018g AlCl 3 •6H 2 O is placed in the ball mill tank of a planetary ball mill, dripped with 7mL of ammonia water, put in 85g of grinding balls, and ball milled at a speed of 470r / min for 2.5h, take out the slurry obtained after ball milling, add 20mL of distilled water and place it in a beaker for 30min of ultrasonication, and let it stand After precipitation for 20 minutes, discard the supernatant, then add 20 mL of distilled water, sonicate 5 times (add 5 mL of distilled water for the last time), centrifuge, and vacuum-dry the sample at 120°C until the sample has constant weight, and grind to obtain a nano-Mg-Al LDH sample.

[0014] figure 1 It is the X-ray powder diffraction pattern of the Mg-Al LDH sample prepared in Example 1, and the diffraction peaks are symmetrical sharp peaks, indicating good crystallinity. Comparing the standard XRD pattern of Mg-Al LDH, it can be seen that the peak positions of the prepared Mg-Al LDH and...

Embodiment 2

[0017] Take 0.7624g MgCl 2 •6H 2 O with 0.3018g AlCl 3 •6H 2 O is placed in the ball mill tank of a planetary ball mill, dripped with 14mL of ammonia water, put in 85g of grinding balls, and ball milled at a speed of 470r / min for 2.5h, take out the slurry obtained after ball milling, add 20mL of distilled water and place it in a beaker for ultrasonication for 30min, and let it stand After precipitation for 20 minutes, discard the supernatant, then add 20 mL of distilled water, sonicate 5 times (add 5 mL of distilled water for the last time), centrifuge, and vacuum-dry the sample at 120°C until the sample has constant weight, and grind to obtain a nano-Mg-Al LDH sample.

Embodiment 3

[0019] Take 0.7624g MgCl 2 •6H 2 O with 0.3018g AlCl 3 •6H 2O is placed in the ball mill tank of a planetary ball mill, dripped with 6mL of ammonia water, put in 85g ball mill balls, and milled at a speed of 470r / min for 2h. During the milling period, add 3mL of ammonia water dropwise every 30min, and finish dripping twice. After taking out the ball mill Add 20mL of distilled water to the obtained slurry and put it in a beaker for ultrasonication for 30min, let it settle for 20min, pour off the supernatant, then add 20mL of distilled water, ultrasonicate for 5 times in total (add 5mL of distilled water for ultrasonication at the last time), centrifuge, and place in a vacuum at 120°C Dry the sample to a constant weight, and grind to prepare a nano-Mg-Al LDH sample.

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Abstract

The invention discloses a method used for preparing layered double metal hydroxides through mechanical ball milling, and belongs to the technical field of nanometer functional material synthesis. Themethod comprises following steps: a divalent metal salt and a trivalent metal salt are introduced into a ball milling tank of a planetary ball mill, ammonium hydroxide liquid and grinding balls are introduced into the ball milling tank, ball milling is carried out for 2 to 3h at a rotating speed of 470r / min, a slurry obtained through ball milling is taken out from the ball milling tank, distilledwater is added for ultrasonic treatment and centrifugation, an obtained sample is subjected to vacuum drying at 120 DEG C until the weight is constant, and grinding is carried out so as to obtain a target product nanometer layered double metal hydroxide. The layered double metal hydroxide is high in stability, excellent in crystallinity, and low in cost; the method is simple, is benefit for largescale industrialized production, and is promising in application prospect.

Description

technical field [0001] The invention belongs to the technical field of synthesis of nanometer functional materials, and in particular relates to a method for preparing layered double metal hydroxide by one-step mechanical ball milling. Background technique [0002] Layered double hydroxides (Layered Double Hydroxides, LDHs for short), also known as hydrotalcites, are a class of layered compounds composed of positively charged metal hydroxides and exchangeable anions filled between layers. Since LHDs have the advantages of both intercalation guest and LDHs host, they show extremely broad application prospects in the fields of environment, medicine, chemistry, materials and so on. The current preparation methods of LDHs mainly include coprecipitation method, ion exchange method, hydrothermal synthesis method and roasting reduction method. Co-precipitation method and ion exchange method are time-consuming and easy to produce waste liquid, while hydrothermal synthesis method an...

Claims

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Application Information

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IPC IPC(8): C01B13/36B82Y40/00C01F7/00
CPCB82Y40/00C01B13/363C01P2004/04C01P2002/72C01P2002/22C01F7/782C01F7/78
Inventor 吕香英张啸天张哲张琳惠李小品
Owner HENAN NORMAL UNIV
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