Metal ion imprinted amino functionalized mesoporous silicon adsorbent and preparation method thereof

A technology of metal ion imprinting and amine-based functions, which is applied in the fields of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., and can solve the problem of weak anti-interference ability of coexisting ions, poor selective adsorption capacity, etc. problems, to achieve the effects of environmental protection, good regeneration performance, and simple preparation process

Inactive Publication Date: 2015-12-30
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the biggest disadvantage of this kind of adsorption material is that its selective ad

Method used

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  • Metal ion imprinted amino functionalized mesoporous silicon adsorbent and preparation method thereof
  • Metal ion imprinted amino functionalized mesoporous silicon adsorbent and preparation method thereof
  • Metal ion imprinted amino functionalized mesoporous silicon adsorbent and preparation method thereof

Examples

Experimental program
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Example Embodiment

[0056] Example 1: The adsorbent adopts the sol-gel method to synthesize metal ion-imprinted amine functionalized mesoporous silica sol under alkaline conditions. During the evaporation of solvent ethanol, the sol is gradually hydrolyzed and polycondensed to form a mesoscopic structure. After solvent volatilization, crystallization, template removal, filtration, washing, drying and other steps, the metal ion imprinted amine functionalized mesoporous silica adsorbent is finally obtained.

[0057] The metal ion imprinted amine group functionalized mesoporous silica sol is a synthetic sol, and the substance type and molar ratio of the synthetic sol are amine group-containing silane coupling agent: orthosilicate: surfactant: HCl: quaternary ammonium base :H 2 O:ethanol:metal ion=(0.04-0.35):1:(0.03-0.25):(0.01-0.10):(0.04-0.30):(4.55-10.50):(27-54):(0.01-0.35) ;

[0058] At 25°C, 2.32g of bishexadecyldimethylammonium bromide was dissolved in 40g of ethanol, and stirred at 400 rpm...

Example Embodiment

[0059] Example 2: At 40 ° C, 3.73 g of dodecyl glycoside (mass concentration 50%) was dissolved in 20 g of ethanol, and sonicated for 1.0 hour (ultrasonic power 300 W); at the same time, 1.37 g of N-β-aminoethyl- γ-Aminopropyltrimethoxysilane was dissolved in 30g of ethanol, under the condition of ultrasonic power of 500W, 0.86g of copper nitrate was added, and 3.14g of 15% tetraethylammonium hydroxide aqueous solution was added dropwise. The pH value of the 10 mol / L hydrochloric acid solution was adjusted to 12. After 1.0 hours, the above two solutions were mixed, and 4.34 g of methyl orthosilicate was added dropwise under the condition that the stirring speed was 300 rpm. After 1.5 hours, the prepared silica sol was placed in a constant temperature and humidity box until the solvent was completely volatilized (humidity 30% RH, temperature 40°C). The product was microwave crystallized at 100°C for 2 hours (microwave power 300W), extracted with a mixed solution of ethanol and ...

Example Embodiment

[0060] Example 3: At 50°C, dissolve 2.00g of polyethylene glycol 2000 in 30g of ethanol, and ultrasonicate for 2.0 hours (ultrasonic power 400W); dissolve 1.98g of γ-diethylenetriaminopropylmethyldimethoxysilane In 40g of ethanol, under the condition that the stirring speed is 500 rev / min, add 1.38g of zinc nitrate, dropwise add 2.88g of tetramethylammonium hydroxide aqueous solution with a mass concentration of 10%, adjust with 10mol / L of hydrochloric acid solution The pH of the system was 13.5, and the mixture was stirred for 2 hours. The above two solutions were mixed, and under the condition of ultrasonic power 400W, 7.85g propyl orthosilicate was added dropwise. After 2 hours, the prepared silica sol was placed in a constant temperature and humidity box until the solvent was completely evaporated (humidity 25% RH, temperature 30°C). The product was hydrothermally crystallized at 110°C for 2 days, and then the mixture of the product and acidic ethanol was extracted by mic...

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Abstract

The invention relates to a metal ion imprinted amino functionalized mesoporous silicon adsorbent and a preparation method thereof, belonging to a mesoporous silicon adsorbent and a preparation method thereof. According to the preparation method, the metal ion imprinted amino functionalized mesoporous silicon adsorbent is prepared by taking a surfactant and metal ions as templates, ethyl alcohol as a solvent, an amino-containing silane coupling agent as a functional monomer and orthosilicate as a crosslinking agent on the basis of a chelation of metal ions and amino under the condition of adding quaternary ammonium base through a sol-gel method; the adsorbent is synthesized into metal ion imprinted amino functionalized mesoporous silicon sol under an alkaline condition by adopting a sol-gel method, and the sol is subjected to gradually hydrolytic polycondensation to form a mesostructure in a volatilization process of the solvent, namely the ethyl alcohol, and the metal ion imprinted amino functionalized mesoporous silicon adsorbent is obtained by the steps of solvent volatilization, crystallization, template removal, filtering, washing and drying. The metal ion imprinted amino functionalized mesoporous silicon adsorbent has the advantages of simple preparation process, easiness in control of conditions, high selective adsorption capability of the obtained materials and convenient in regeneration.

Description

technical field [0001] The invention relates to a mesoporous silicon adsorbent and a preparation method thereof, in particular to an amine functionalized mesoporous silicon imprinted with metal ions and a preparation method thereof. Background technique [0002] Since its appearance in 1992, mesoporous silicon materials have been widely used in the fields of adsorption, catalysis, separation and purification, and new assembly materials due to their characteristics such as large specific surface area, adjustable pore size, controllable shape, high stability, and surface modification. favored; however, relying solely on the performance of mesoporous silica is far from meeting its application requirements. Therefore, organic modification of mesoporous silicon materials and the introduction of functional groups are important methods to enhance the performance of mesoporous silicon materials and broaden their applications. [0003] As an important functional group, the amine gro...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30
Inventor 杨虹冯启言田慧娟石林
Owner CHINA UNIV OF MINING & TECH
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