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A kind of preparation method of nano hydrotalcite

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, uniform particle size, and narrow distribution

Active Publication Date: 2017-03-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 controllable preparation and batching of the particle size and particle size distribution of nano-hydrotalcite-like materials. Repeated production between times can also solve the problem of blockage in the microchannel reactor

Method used

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  • A kind of preparation method of nano hydrotalcite
  • A kind of preparation method of nano hydrotalcite
  • A kind of preparation method of nano hydrotalcite

Examples

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 invention relates to a preparation method of nanometer hydrotalcite, which adopts a flow-focused microchannel reactor, and realizes the controllable preparation of nanometer hydrotalcite by introducing gas to strengthen microscopic mixing. The water-soluble divalent metal salt raw material A2+X and the trivalent metal salt raw material B3+X are mixed according to a certain concentration, and a soluble strong base or a mixture of strong base and carbonate is prepared into an aqueous solution; the metal salt solution, gas and alkali solution are prepared by The three inlets of the flow-focused microchannel reactor enter at the same time, mix and react in the microchannel; the obtained precipitate is subjected to hydrothermal treatment, centrifugation, and drying to obtain nano-hydrotalcite-like materials. The invention has the advantages of short residence time, large throughput, controllable particle size, narrow distribution and the like. Compared with the conventional microchannel reactor, the gas inlet channel is added in the structure. Due to the introduction of gas in the process, the mixing effect is further strengthened, and the product particle size is more uniform. In addition, it can solve the problem of microchannel reactor in the process of nanomaterial synthesis. clogging problem.

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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Patent Type & Authority Patents(China)
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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