Preparation method for nanosheet of uniformly dispersed layered double hydroxides (LDHs)

A hydrotalcite, monolithic technology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve problems such as unfavorable applications, and achieve the effects of wide application range, friendly production environment, and mild preparation conditions

Inactive Publication Date: 2013-04-03
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are two main methods for preparing hydrotalcite-like nanosheets with a single-layer or few-layer structure: "top-down method" and "bottom-up method"; "top-down method" is to prepare hydrotalcite-like nanosheets first. The crystal is then peeled off its sheet. This method is mainly carried out in organic solvents, such as: n-butanol, acrylic acid, formamide, etc., literature (Gardner, E.; Huntoon, K.M.; Pinnavaia, T.J.Direct synthesis of alkoxide -intercalated derivatives of hydrocalcite-like Layered double hydroxides: Precursors for the formation of colloidal layered double hydroxide suspensions and transparent thin films. Adv. Mater. 2001, 13, 1263) discloses a hydrotalcite-like exfoliation in aqueous solution The method of inserting the alkoxide into the hydrotalcite-like layer to form a hybrid, and then peeling off the layer in water, the surface of the hydrotalcite-like nanosheet obtained by this method is adsorbed with organic molecules, which is not conducive to the further assembly process. The "bottom-up method" is a method for directly preparing hydrotalcite-like monoliths, and there are few reports so far. Literature (Hu, G.; Wang, N.; O'Hare, D.; Davis, J. One-step synthesis and AFM imaging of hydrophobic LDH m...

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  • Preparation method for nanosheet of uniformly dispersed layered double hydroxides (LDHs)
  • Preparation method for nanosheet of uniformly dispersed layered double hydroxides (LDHs)
  • Preparation method for nanosheet of uniformly dispersed layered double hydroxides (LDHs)

Examples

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Embodiment 1

[0023] This embodiment first weighs 2.250g Al(NO 3 ) 3 9H 2 O and 3.078g Mg(NO 3 ) 2 ·6H 2 O was dissolved in 20ml of water to obtain a mixed salt solution, in which, Al 3+ with Mg 2+ The molar ratio of the solution is 1:2; the dilute ammonia solution of 7wt% is prepared by conventional technology; at a reaction temperature of 25°C, the flow rate of the mixed salt solution and the dilute ammonia solution is 15ml / min, and in the microreactor Mixing reaction in middle to obtain precipitate, centrifuge the precipitate and wash with distilled water, repeat three times, and the obtained product is homogeneously dispersed hydrotalcite-like nano single sheet.

[0024] In this example, the XRD-6000 X-ray powder diffractometer of Shimadzu Corporation was used to characterize the crystal structure of the homogeneously dispersed hydrotalcite-like nano-monolithic sheet. image 3 The XRD spectrum of the homogeneously dispersed hydrotalcite-like nano-monolithic sheet, it can be seen ...

Embodiment 2

[0026] This embodiment first weighs 0.250g Al(NO 3 ) 3 9H 2 O and 0.397g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 20ml of water to obtain a mixed salt solution, in which, Al 3+ with Zn 2+ The mol ratio of the solution is 1:2; the aqueous sodium hydroxide solution of 0.20mol / L is adopted in the preparation of conventional technology, and at a reaction temperature of 30°C, the flow rate of the mixed salt solution and the aqueous sodium hydroxide solution is 20ml / min. Mixing and reacting in a microreactor to obtain precipitates, centrifuging the precipitates and washing them with distilled water, repeating three times, the obtained product is uniformly dispersed hydrotalcite-like nano-sheets.

[0027] In this example, the XRD-6000 X-ray powder diffractometer of Shimadzu Corporation was used to characterize the crystal structure of the homogeneously dispersed hydrotalcite-like nano-monolithic sheet. Figure 4 For the XRD spectrogram of the homogeneously dispersed hydrotalcite-l...

Embodiment 3

[0029] This embodiment first weighs 0.750g Al(NO 3 ) 3 9H 2 O and 1.539g Mg(NO 3 ) 2 ·6H 2 O is dissolved in 20ml of water to obtain a mixed salt solution, wherein, Al 3+ with Mg 2+ The mol ratio of the solution is 1:3; the aqueous sodium hydroxide solution of 0.20mol / L is adopted in the preparation of conventional technology, and at a reaction temperature of 30°C, the flow rate of the mixed salt solution and the aqueous sodium hydroxide solution is 10ml / min. Mixing and reacting in a microreactor to obtain precipitates, centrifuging the precipitates and washing them with distilled water, repeating three times, the obtained product is uniformly dispersed hydrotalcite-like nano-sheets.

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Abstract

The invention belongs to the technical field of nanometer material preparation and relates to a preparation method for a nanosheet of uniformly dispersed layered double hydroxides (LDHs). The preparation method comprises the steps as follows: firstly, mixing a soluble bivalent inorganic salt M<2+>Y with a soluble trivalent inorganic salt M<3+>Y and dissolving in de-ionized water to prepare a salt solution; secondly, preparing an alkali solution by adopting the conventional technology; thirdly, fully mixing and reacting the salt solution with the alkali solution by utilizing a micro-channel reactor to obtain deposits of LDHs; and lastly, fully washing the deposits with the de-ionized water and centrifuging to obtain jelly with a single-layer nanosheet, which is the nanosheet of uniformly dispersed LDHs. The nanosheet of uniformly dispersed LDHs is simple to prepare, moderate in preparation conditions, low in cost, environment-friendly in production, wide in application range, and high in economic value.

Description

Technical field: [0001] The invention belongs to the technical field of nanomaterial preparation, and relates to a preparation process of nanomaterials, in particular to a preparation method of homogeneously dispersed hydrotalcite-like nanometer sheets. Background technique: [0002] Layered Double Hydroxides (LDHs for short), also known as hydrotalcite-like, is a typical anionic layered material, and its chemical composition formula is [M 2+ 1-x m 3+ x (OH) 2 ] x+ (A n- ) x / n ·yH 2 O, where M 2+ Represents the divalent metal ion Mg 2+ 、Co 2+ 、Ni 2+ , Fe 2+ , Mn 2+ , Zn 2+ any of the 3+ for Al 3+ or Fe 3+ ;A n- for NO 3 - , F - 、Br - , Cl - , CO 3 2- SO 4 2- Any one of them; 0.17≤x≤0.35; m is the amount of crystal water, the element type and composition ratio of the main layer of LDHs, and the type and quantity of interlayer objects can be adjusted in a wide range according to the needs, so as to obtain Materials with special structures and proper...

Claims

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Application Information

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IPC IPC(8): C01G5/00C01G9/00C01G53/00C01G49/00C01F7/00B82Y30/00B82Y40/00
Inventor 侯万国庞秀江孙美玉
Owner QINGDAO UNIV OF SCI & TECH
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