Three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material and preparation method thereof

A layered hydroxide, salicylate technology, applied in the preparation of oxide/hydroxide, nickel oxide/nickel hydroxide, nanotechnology, etc. The problems of layered hydroxide nanomaterials and methods are troublesome, and the effects of simple process, high yield and low cost are achieved.

Inactive Publication Date: 2013-05-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Literature: Kang Zhiqiang, Du Baozhong, Chen Bo, Wang Junfeng. Chemical Engineer, 2007(1):9-11), this article is based on CO 3 2- Type magnesium aluminum hydrotalcite is the precursor, and ethylene glycol is the dispersion medium. The hydrotalcite with salicylate intercalation has been prepared by the ion exchange method, but the method is cumbersome and uses an organic solvent.
[0004] At present, there are no relevant reports on layered hydroxide nanomaterials intercalated with three-dimensional flower-like salicylic acid radicals

Method used

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  • Three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material and preparation method thereof
  • Three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material and preparation method thereof
  • Three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material and preparation method thereof

Examples

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Embodiment 1

[0024] A weighs 9.32g of Co(NO 3 ) 2 ·6H 2 O and 3.00g of Al(NO 3 ) 3 9H 2 O was dissolved in deionized water to make 100ml mixed salt solution; 4g of sodium hydroxide was weighed and dissolved in deionized water to make 200ml lye.

[0025] B takes by weighing 12.80g sodium salicylate and dissolves deionized water and is made into 150m sodium salicylate solution, wherein Co(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 The molar ratio of O and sodium salicylate is 4:1:10.

[0026] C. Pour the sodium salicylate solution and the mixed salt solution into a four-neck flask at the same time, and start electric stirring to rotate at a constant speed at 200r / min; after mixing evenly, adjust the pH of the solution to 6.8 with lye.

[0027] D Transfer the mixed solution of step C into a high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene liner, and hydrothermally crystallize at 140°C for 24 hours in a static state; wash the reacted product with deionized water, an...

Embodiment 2

[0029] A weighs 9.32g of Co(NO 3 ) 2 ·6H 2 O and 3.00g of Al(NO 3 ) 3 9H 2 O was dissolved in deionized water to make a 100ml mixed salt solution; 4g of sodium hydroxide was weighed and dissolved in deionized water to make a 200ml alkali solution.

[0030] B takes by weighing 19.20g sodium salicylate and dissolves deionized water and is made into 150m sodium salicylate solution, wherein Co(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 The molar ratio of O and sodium salicylate is 4:1:15.

[0031] C. Pour the sodium salicylate solution and the mixed salt solution into a four-necked flask at the same time, and start electric stirring to rotate at a constant speed at 200r / min; after mixing evenly, adjust the pH of the solution to 7.2 with lye.

[0032]D Transfer the mixed solution of step C into a high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene liner, and hydrothermally crystallize at 120°C for 24 hours in a static state; wash the reacted product with de...

Embodiment 3

[0034] A weighs 7.75g of Ni(NO 3 ) 2 ·6H 2 O and 5.00g of Al(NO 3 ) 3 9H 2 O was dissolved in deionized water to make 100ml mixed salt solution; 4g of sodium hydroxide was weighed and dissolved in deionized water to make 200ml lye.

[0035] B takes by weighing 12.80g sodium salicylate and dissolves deionized water and is made into 150m sodium salicylate solution, wherein Co(NO 3 ) 2 ·6H 2 O, Al(NO 3 ) 3 9H 2 The molar ratio of O and sodium salicylate is 2:1:8.

[0036] C Pour the sodium salicylate solution and the mixed salt solution into a four-necked flask at the same time, and start electric stirring to rotate at a constant speed at 200r / min; after mixing evenly, adjust the pH of the solution to 7 with lye.

[0037] D Transfer the mixed solution of step C into a high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene liner, and hydrothermally crystallize at 120°C for 24 hours in a static state; wash the reacted product with deionized water, and ...

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Abstract

The invention discloses a three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material and a preparation method thereof. The three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material is nano powder with uniform particles, the diameter of the three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material is 1-2mum, a microstructure of the three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material is a flower-like structure, petals are nano slices grown uniformly, and thickness of each nano slice is 5-20nm. The preparation method of the three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material comprises the following steps of: mixing mixed solution of soluble divalent metal and soluble aluminium salt with salicylate solution, and regulating pH value to be 6.5-7.5 with an alkaline solution; carrying out hydrothermal crystallization for 12-72 hours at the temperature of 120-160 DEG C under standing condition; and washing and drying, so that the three-dimensional flower-like salicylic acid radical intercalation layered hydroxide nano material is obtained. A hydrothermal method is adopted for preparation, the obtained material has uniform nano particles, and the petals are slices grown uniformly. The preparation method disclosed by the invention has the characteristics of available raw materials, simple equipment and process, no guiding agent or modifier, high efficiency, high speed and high yield and is applicable to large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic nanomaterials, in particular to a layered hydroxide nanomaterial intercalated with three-dimensional flower-shaped salicylic acid radicals and a preparation method thereof. Background technique [0002] In recent years, controlled synthesis of three-dimensional nanomaterials has been one of the hotspots in material science research. Because of its special physical and chemical properties, it will have good application prospects in electromagnetism, electronics, catalysis, water treatment and energy storage. [0003] Layered metal hydroxides are a typical type of anionic layered materials, which are composed of parallel and positively charged laminates, and the interlayers are composed of balanced anions and water molecules. Due to its unique crystal structure and physical and chemical properties, this kind of material shows extremely broad application prospects in many fields such as ion exc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01G53/04B82Y40/00
Inventor 王连英洪玲宋莹莹何静
Owner BEIJING UNIV OF CHEM TECH
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