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Hydrotalcite preparation method

A hydrotalcite, trivalent metal technology, applied in the preparation of oxide/hydroxide, alumina/aluminum hydroxide, etc., can solve the problems of large environmental pollution, large equipment investment, large water consumption, etc., and achieve simple experimental steps. , The effect of low process cost and small equipment investment

Inactive Publication Date: 2013-12-18
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As recorded in Chinese patent application 201110091118.6, the technical problems of the prior art also include: (1) The sol-gel method requires the use of metal alkoxides, which are relatively expensive
(2) The roasting reduction method requires high temperature and large investment in equipment
(3) The nucleation / crystallization isolation method requires a special "full reverse mixing explosive nucleation reactor" and "constant temperature reflux crystallization process equipment" to increase the complexity of the process
Synthetic methods in the prior art all need to consume a large amount of water, and are more polluting to the environment. Therefore, it is necessary to study a new synthetic method with less water consumption, low cost, simple operation and little environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Weigh 2.565g of Mg(NO 3 ) 2 ?6H 2 O and 1.876g of Al(NO 3 ) 3 ?9H 2 O, fully grind in a mortar for 10-15min, and put it into a small kettle. Weigh again 3.360g of (NH 4 ) 2 CO 3 , into the cauldron.

[0041] (2) Put the small kettle into the big kettle, and crystallize in an oven at 150°C for 1 day. After the reaction, wash and filter with deionized water, put it in an oven at 80°C to dry, and finally obtain the product.

[0042] In this example, hydrotalcite was prepared under the condition of pH=8.5. The XRD and SEM characterization results of the prepared product are as follows Figure 3a , Figure 3b as shown, Figure 3a It shows that using nitrate as a reactant, hydrotalcite, Figure 3b It shows that the synthesized hydrotalcite is lamellar, and the layers are stacked together.

Embodiment 2

[0044] (1) Weigh 2.033g of MgCl 2 ?6H 2 O and 1.209 g of AlCl 3 ?6H 2 O, fully grind in a mortar for 10-15 minutes, and put it into a small kettle. Then weigh 4.206g of urea and 3g of deionized water and add them to the large kettle.

[0045] (2) Put the small kettle into the big one, crystallize in an oven at 150°C for 1 day, wash and filter with deionized water after the reaction, put it in an oven at 80°C to dry, and finally get the product.

[0046] In this example, hydrotalcite was prepared under the condition of pH=9.0. XRD and SEM characterization results such as Figure 4a , Figure 4b as shown, Figure 4a It shows that when a small amount of deionized water is added, the synthetic hydrotalcite has high crystallinity, less impurities, Figure 4b It shows that lamellar crystals can be clearly seen, and the distribution is relatively uniform.

Embodiment 3

[0048] (1) Weigh 2.566g of Mg(NO 3 ) 2 ?6H 2 O and 1.877g of Al(NO 3 ) 3 ?9H 2 O, fully grind in a mortar for 10-15 minutes, and put it into a small kettle. Weigh again 3.360g of (NH 4 ) 2 CO 3 And 5g deionized water, add to the big kettle.

[0049] (2) Put the small kettle into the big kettle, and crystallize in an oven at 150°C for 1 day. After the reaction, wash and filter with deionized water, put it in an oven at 80°C to dry, and finally obtain the product.

[0050] In this example, hydrotalcite was prepared under the condition of pH=8.5. XRD and SEM characterization results such as Figure 5a , 5b as shown, Figure 5a It shows that deionized water has a certain influence on the synthesis of hydrotalcite, and the characteristic peak of hydrotalcite is strong, but there are small impurity peaks, Figure 5b It shows that the sheets of hydrotalcite crystals are thin and irregular.

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Abstract

The invention discloses a hydrotalcite preparation method. The method comprises the following steps: mixing and grinding raw materials comprising a divalent metal salt and a trivalent metal salt in a reaction container; adding urea or ammonium carbonate as a mineralizer; adding a small amount of water or not adding water; and reacting at 100-200DEG C under a seal condition to prepare a target product hydrotalcite. The method which allows hydrotalcite to be synthesized through vapor phase transfer without added water or in the presence of a small amount of water has the advantages of simple experiment steps, small apparatus investment and low technological cost, and the prepared hydrotalcite has a high crystallization degree.

Description

technical field [0001] The invention specifically relates to a preparation method of hydrotalcite. Background technique [0002] Hydrotalcite Compound is a kind of anion-intercalated double-layer structure substance, which is generally believed to have the general formula: , where M 2+ and M 3+ It is a divalent and trivalent metal cation with a hydroxide double-layer structure, and x is M 3+ / M 3+ +M 2+ The molar ratio of A n- It is an anion with n negative charges, and m is the content of crystal water. Divalent metal cations have Mg 2+ , Zn 2+ 、Cu 2+ 、Ni 2+ 、Co 2+ , Fe 2+ , Ca 2+ Wait, the trivalent metal cation has Al 3+ , Mn 3+ , Fe 3+ 、Cr 3+ , Ga 3+ 、Co 3+ and many more. [0003] The hydrotalcite material has tunable layer cations and exchangeability of interlayer anions. After years of research, it has been found that it has great application value in many aspects such as catalysis, adsorption, ion exchange, and environmental protection. Research ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01F7/02
Inventor 王一萌曹涛苏秦吴海虹
Owner EAST CHINA NORMAL UNIV