Preparation method of organic/layered double hydroxide (LDH) complex

A complex and organic technology, applied in the field of organic/LDH complex and its preparation, can solve the problems of Mg/Al ratio reduction, layer composition change, and destruction of LDH precursor morphology, etc.

Inactive Publication Date: 2011-10-26
BEIJING NORMAL UNIVERSITY +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The traditional methods for preparing organic / LDH composite materials include coprecipitation, ion exchange and roasting recovery methods, etc. Recently, there are stripping / rearrangement and swelling / recovery methods, but the inventors found that using stripping / rearrangement and swelling / recovery methods In the process of preparing composites by the method, the composition of the laminates changes, that is, the Mg / Al ratio decreases, and the stripping / arrangement method will destroy the morphology of the LDH precursor

Method used

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  • Preparation method of organic/layered double hydroxide (LDH) complex
  • Preparation method of organic/layered double hydroxide (LDH) complex
  • Preparation method of organic/layered double hydroxide (LDH) complex

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preparation example Construction

[0053] The preparation method of this organic / LDH complex comprises the following steps:

[0054] a) Preparation of 4,7,13,16-tetracarboxymethyl-1,10-dioxo-4,7,13,16-tetraazacycloctadecane (TECA for short in the present invention):

[0055] CH 2 Cl 2 As a solvent, dissolve 1,10-dioxo-4,7,13,16-tetraza-18-crown-6 (abbreviated as L in the present invention, the structure diagram is as follows), CH 2 Cl 2 The ratio of the volume of L to the number of moles of L is 5L / mol~10L / mol. Then add anhydrous potassium carbonate to the solution for mixing, and heat to reflux for 15 minutes to 40 minutes. The mass ratio of anhydrous potassium carbonate to L is preferably 2 to 5. Add ethyl bromoacetate to the solution and reflux for 20h to 25h. The molar ratio of the volume of ethyl bromoacetate to L is 0.5L / mol to 1L / mol. The resulting solution was filtered and evaporated to obtain an oily substance (hereinafter referred to as L1 in the present invention). Hydrochloric acid solution was...

Embodiment 1

[0067] 1. Preparation of MgAl-NO 3 -LDH:

[0068] 3.20gMg(NO 3 ) 2 ·6H 2 O(0.02mmol), 2.34gAl(NO 3 ) 3 9H 2 O (0.01mmol) and 2.28g HMT (0.026mmol) were added with 50ml distilled water, reacted in the reaction kettle at 140°C for 24h, cooled at room temperature, filtered with suction, washed with water, and dried naturally to obtain MgAl-CO 3 -LDH.

[0069] MgAl-CO 3 The XRD pattern of -LDH is shown in figure 2 . Layer spacing d basal = 0.76nm indicating the formation of CO 3 -LDH, the sharp diffraction peaks at 0.76 and 0.38nm correspond to the diffraction of its (003) and (006) planes, respectively.

[0070] Weigh 1.0g MgAl-CO 3 -LDH, add 1L containing NaNO 3 (Concentration is 1.5mol L -1 ) and HNO 3 (Concentration is 5mmol·L -1 ) in the mixed solution, sonicate for 20min, pass N 2 5min, stirred for 24h, suction filtered, exhausted and washed with water, and vacuum dried at 40°C to obtain MgAl-NO 3 -LDH.

[0071] MgAl-NO 3 -XRD of LDH see image 3 . L...

Embodiment 2

[0078] Step 1 and 2 are the same as embodiment 1, add MgAl-NO in step 3 3 -The resting time of LDH after shaking is 12h, and the other steps are the same.

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Abstract

The invention provides a preparation method of an organic/layered double hydroxide (LDH) complex. The preparation method comprises the following steps of a) dissolving 1,10-dioxo-4,7,13, 16-tetranitro-18-crown-6 in a CH2Cl2 solvent, adding anhydrous potassium carbonate into the solution and mixing them, heating and refluxing the mixed solution, then adding ethyl bromoacetate into the mixed solution and refluxing it, then filtering and evaporating the refluxed solution to obtain an oil-like substance, adding hydrochloric acid solution into the oil-like substance, heating, refluxing and filtering the mixed solution, and evaporating the filtrate to make crystals be separated out to obtain 4,7,13,16-tetracarboxymethyl-1,10-dioxo-4,7,13, 16-tetraazaoctadecane (TECA), and b) mixing TECA, NaOH and methanamide, adding MgAl-NO3-LDH into the mixture, standing for 10 minutes to 16 hours, and then centrifuging, washing and drying the mixture to obtain a TECA/LDH complex, wherein a mass ratio of TECA to MgAl-NO3-LDH is 1. Through the preparation method, a TECA/LDH complex can be prepared in a short reaction time thus a production period of the TECA/LDH complex is saved; corrosive effects of methanamide on LDH laminates are reduced and compositions of the laminates are maintained well; and a crystallinity and a yield of complex products are improved.

Description

technical field [0001] The invention relates to the field of synthesis of organic / LDH composite materials, in particular to a carboxylic acid derivative of tetraazacrown ether, an organic / LDH composite prepared from the carboxylic acid derivative and a preparation method. Background technique [0002] The size of nanomaterials is between 1-100nm, and its volume effect, surface effect, quantum size effect and macroscopic quantum tunneling effect make nanoparticles have unique properties in terms of mechanics, magnetism, optics, and chemical activity. However, nanomaterials are highly active and very unstable, so organic / inorganic nanocomposites have been proposed to improve the stability of nanomaterials. [0003] Organic / inorganic nanocomposites refer to the hybridization of organic and inorganic materials at the nanoscale, which is a special functional material. Inorganic compounds have good electrical conductivity, mechanical properties, thermal stability, magnetic and op...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D273/00B82Y30/00
Inventor 马淑兰王娟杜丽楚楠凯
Owner BEIJING NORMAL UNIVERSITY
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