Nanometer hydrotalcite-like compound preparation method

A hydrotalcite and nano-technology, which is applied in the field of preparation of nano-hydrotalcites, can solve problems such as microchannel reactor blockage, and achieve the effects of short residence time, narrow distribution, and controllable particle size

Active Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a method for preparing nano-hydrotalcite-like materials using a microchannel reactor, which can realize the control

Method used

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  • Nanometer hydrotalcite-like compound preparation method
  • Nanometer hydrotalcite-like compound preparation method

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Experimental program
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Effect test

Embodiment 1

[0028] Weigh 48.1g of Mg(NO 3 ) 2 ·6H 2 O and 23.4g of Al(NO 3 ) 3 9H 2 O, configured as 500ml of an aqueous solution with a total concentration of metal ions of 0.5mol / L. Weigh 16g of NaOH and 13.25g of Na 2 CO 3 configured as OH - and CO 3 2- 500ml of aqueous solution with a total concentration of 1.05mol / L. Air is selected as the gas, and the flow rate is 100ml / min. Both the metal salt solution and the alkali solution enter the microchannel reactor at a flow rate of 150ml / min to contact, mix and react, and the reaction temperature is 80°C. Take part of the precipitate and put it into a hydrothermal reactor, and treat it at 150°C for 6h. The precipitate after hydrothermal treatment was fully washed with deionized water, and the precipitate obtained after centrifugation was nano-carbonate-type MgAl hydrotalcite. The XRD and TEM characterization results were as follows: image 3 , Figure 4 shown.

Embodiment 2

[0030] Weigh 48.1g of Mg(NO 3 ) 2 ·6H 2 O, 11.7g of Al(NO 3 ) 3 9H 2 O and 12.6g of Fe(NO 3 ) 3 9H 2 O, configured as 500ml of an aqueous solution with a total concentration of metal ions of 0.5mol / L. Weigh 16g of NaOH and 13.25g of Na 2 CO 3 configured as OH - and CO 3 2- 500ml of aqueous solution with a total concentration of 1.05mol / L. The gas is nitrogen, and the flow rate is 20ml / min. Both the metal salt solution and the alkali solution enter the microchannel reactor at a flow rate of 100ml / min to contact, mix and react, and the reaction temperature is 80°C. Take part of the precipitate and put it into a hydrothermal reactor, and treat it at 100°C for 4h. The precipitate after hydrothermal treatment is fully washed with deionized water, and the precipitate obtained after centrifugation is nano-carbonate-type MgAlFe hydrotalcite. The XRD pattern analysis results of the hydrotalcite are shown in the attached Figure 5 Show.

Embodiment 3

[0032] Weigh 24.0g of Mg(NO 3 ) 2 ·6H 2 O, 27.3g of Ni(NO 3 ) 2 ·6H 2 O, 11.7g of Al(NO 3 ) 3 9H 2 O and 12.6g of Fe(NO 3 ) 3 9H 2 O, configured as 500ml of an aqueous solution with a total concentration of metal ions of 0.5mol / L. Weigh 16g of NaOH and 13.25g of Na 2 CO 3 configured as OH - and CO 3 2- 500ml of aqueous solution with a total concentration of 1.05mol / L. The gas is nitrogen, and the flow rate is 150ml / min. Both the metal salt solution and the alkali solution enter the microchannel reactor at a flow rate of 150ml / min to contact, mix and react, and the reaction temperature is 80°C. Take part of the precipitate and put it into a hydrothermal reactor, and treat it at 100°C for 4h. The precipitate after hydrothermal treatment is fully washed with deionized water, and the precipitate obtained after centrifugation is nano-carbonate-type MgNiFeAl hydrotalcite. The XRD pattern analysis results of this hydrotalcite are shown in the attached Figure 6 Show...

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Abstract

The present invention relates to a nanometer hydrotalcite-like compound preparation method, wherein a flowing focusing type microchannel reactor is adopted, and gas introducing microscopic mixing strengthening is performed to achieve the controllable preparation of the nanometer hydrotalcite-like compound. According to the preparation method, a water-soluble divalent metal salt raw material A<2+>X and a trivalent metal salt raw material B<3+>X are mixed according to a certain concentration, a soluble strong alkali or a mixture of a strong alkaline and a carbonate is prepared into an aqueous solution, the metal salt solution, gas and the alkaline solution concurrently enter from the three inlets of the flowing focusing type microchannel reactor, and are mixed and react in the microchannel, and the obtained precipitate is subjected to a hydrothermal treatment, centrifugation and drying so as to obtain the hydrotalcite-like compound material. According to the present invention, the obtained hydrotalcite-like compound has advantages of short residence time, high flux, controllable particle size, narrow particle size distribution, and the like; and compared with the conventional microchannel reactor, the microchannel reactor of the present invention has the following characteristics that: the gas inlet channel is additionally arranged on the structure, and the gas is introduced during the process, such that the mixing effect is further strengthened, the product particle size is uniform, and the clogging problem of the microchannel reactor in the nanometer material synthesis process can be solved.

Description

technical field [0001] The invention relates to a method for preparing nanometer hydrotalcite, in particular to a method for preparing nanometer hydrotalcite by adopting a flow-focused microchannel reactor and introducing gas to strengthen the reaction process, and belongs to the field of nanometer material preparation. Background technique [0002] Layered double hydroxides (Layered Double Hydroxides, LDHs), also known as hydrotalcites, are an important class of anionic clay materials. The main layer of LDHs is a positively charged double metal hydroxide, and the interlayer is a negatively charged intercalation anion. sex. Since the metal composition of the main layer of LDHs, the type and quantity of interlayer anions, and the size of the inner space are all adjustable, LDHs have broad application prospects in the fields of catalytic materials, adsorption materials, biological / medical materials, etc. [0003] For hydrotalcites, the most common preparation method in the p...

Claims

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Application Information

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IPC IPC(8): C01F7/02C01G49/02C01G53/04B82Y30/00
CPCC01G53/006C01P2002/72C01P2004/04C01F7/785
Inventor 陈光文杨梅任明月
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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