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Preparation method of metal complex functionalized hydrotalcite-like nano-layer sheet

A metal complex and functionalization technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. It is difficult to control the metering relationship and other problems, so as to reduce the surface hydroxyl concentration, enhance the hydrophobicity, and reduce the possibility of

Inactive Publication Date: 2012-02-01
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is more suitable for negatively charged metal complexes to be loaded on the HTLc nanosheets, and there are the following disadvantages for loading neutral metal complexes: 1) the surfactant anions of macromolecules are difficult to remove, which hinders the HTLc nanosheets The use of plates, especially in the preparation of multifunctional catalysts, can not give full play to the catalytic performance of HTLc laminates; 2) The reaction between APTS grafted on HTLc nano-layers and metal complexes is limited by steric constraints and diffusion , not only difficult to carry out but also difficult to control the stoichiometric relationship between the two, resulting in uncertain coordination number of the central ion of the supported iron metalloporphyrin, which in turn affects the catalytic performance of the prepared supported catalyst

Method used

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  • Preparation method of metal complex functionalized hydrotalcite-like nano-layer sheet
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  • Preparation method of metal complex functionalized hydrotalcite-like nano-layer sheet

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Embodiment approach

[0013] Realize the embodiment of the present invention as follows:

Embodiment approach 1

[0015] First, add 10 mL of absolute ethanol solution containing 1 mmol of diethylenetriamine to 5 mL of absolute ethanol solution containing 2 mmol of salicylaldehyde, and reflux for 2 hours under the protection of an inert gas to obtain the ligand N, N-bis (salicyledene ) diethylenetriamine (saldien). Next, add 10 mL of absolute ethanol solution of 1 mmol triethoxychloropropylsilane (CPTM) to 1 mmol of the prepared saldien absolute ethanol solution, and after reflux for 3 hours, add 30 mL of anhydrous ethanol solution in which 1 mmol of copper acetate is dissolved. Ethanol solution, continue to reflux for 5h, and remove the solvent in vacuum to obtain the desired copper Schiff base complex functionalized silane, which is denoted as Cusaldien-CPTM. Then, 1 g of MgAl HTLc intercalated with nitrate radicals with a molar ratio of Mg / Al of 2 was placed in 200 mL N, N-dimethylformamide for 1 h at 40 ° C and 40 W ultrasonic treatment conditions, and a homogeneous Translucent colloi...

Embodiment approach 2

[0017] First, add 50 mL of absolute ethanol solution containing 5 mmol of diethylenetriamine to 25 mL of absolute ethanol solution containing 10 mmol of salicylaldehyde, and reflux for 4 hours under the protection of an inert gas to obtain the ligand N, N-bis (salicyledene ) diethylenetriamine (saldien). Next, 30 mL of absolute ethanol solution of 5 mmol triethoxychloropropylsilane (CPTM) was added to 5 mmol of the prepared saldien absolute ethanol solution, and after reflux for 10 h, 30 mL of anhydrous copper acetate dissolved in 5 mmol was added. ethanol solution, continue to reflux for 10h, and remove the solvent in vacuum to obtain the desired copper Schiff base complex functionalized silane, which is designated as Cusaldien-CPTM. Then, 4g Mg / Al molar ratio is 10 glycinate radical intercalation MgAl HTLc is placed in 200mL formamide and carries out sonication 6h under room temperature, the sonication condition of 100W, obtains uniform translucent colloid stripping liquid a...

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Abstract

The invention relates to a preparation method of a metal complex functionalized hydrotalcite-like nano-layer sheet, which belongs to the field of physical chemistry and material chemistry. The preparation method comprises the following steps of: utilizing metal complex functionalized silane to be directly reacted with surface hydroxyl on a hydrotalcite-like nano-layer sheet after stripping a layer so as to graft a metal complex on the hydrotalcite-like nano-layer sheet, and simultaneously utilizing the reaction of the silane and the surface hydroxyl and the electronic and three-dimensional effects of the grafted metal complex to weaken the electrostatic interaction between the stripped layer and the nano-layer sheet, thereby improving the stability of the hydrotalcite-like nano-layer sheet, preventing the hydrotalcite-like nano-layer sheet from being compounded after a solvent is removed, and still keeping the state of the nano-layer sheet. An organic-inorganic composite material prepared by adopting the method has the characteristics of large specific surface area and high content of the metal complex, and simultaneously has the multifunctional catalytic performances of hydrotalcite-like and the metal complex.

Description

technical field [0001] The preparation method of the metal complex-functionalized hydrotalcite-like nano-sheets of the present invention belongs to the category of physical chemistry and material chemistry, and specifically relates to directly bonding the metal complex-functionalized silane to the surface on the stripped hydrotalcite-like nano-sheets Hydroxyl groups are reacted to prepare an organic-inorganic composite material with large specific surface area, high content of metal complexes and multiple catalytic functions of hydrotalcite-like and metal complexes. Background technique [0002] Hydrotalcite-like compounds (HTLc) are composed of positively charged metal hydroxide layers and interlayer charge-balancing anions. The structure is similar to brucite (Brucite), so it is also called layered bimetallic Hydroxide (layered double hydroxide, LDH). Usually, such compounds are composed of mutually co-edge Mg(OH) 2 The octahedral layered structure is stacked on top of e...

Claims

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Application Information

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IPC IPC(8): B01J31/26
Inventor 范彬彬史秀锋高升成白亚东李瑞丰
Owner TAIYUAN UNIV OF TECH
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