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Method for preparing amino functional MCM-48 mesoporous material

A technology of MCM-48 and amino functionalization is applied in the field of preparation of amino functionalized MCM-48 mesoporous materials, which can solve the problems of complex synthesis process and achieve the effects of simple operation process, high adsorption capacity and excellent absorption performance.

Active Publication Date: 2013-07-03
海宁市袁花镇工业投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hideaki Yoshitake et al. (Bull.Chem.Soc.Jpn., 2003, 76, 847-852) synthesized amino-functionalized MCM-48 by grafting method, which has higher adsorption capacity for Cr(VI) and As(V), However, the synthesis process is complex and uses toluene that pollutes the environment, and does not adsorb other heavy metal ions

Method used

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  • Method for preparing amino functional MCM-48 mesoporous material
  • Method for preparing amino functional MCM-48 mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 5.278g (0.00091mol) of polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer into a round bottom flask, add an appropriate amount of deionized water, stir at a constant temperature of 40°C until completely dissolved, then add 3.316g (0.0091mol) cetyltrimethylammonium bromide, add 1.40g (0.035mol) NaOH and 0.294g (0.007mol) NaF, then add 15.5mL (0.07mol) of tetraethyl orthosilicate and 1.53 mL (0.00595mol) of 3-[2-(2-aminoethylamino)ethylamino]propyl-trimethoxysilane, continue to stir for a period of 24 hours, put the obtained sol in a high-pressure reactor, and crystallize at 100°C 24 hours. After the crystallization is complete, the obtained solid sample is washed twice with water and absolute ethanol, filtered and dried. The obtained sample is placed in a Soxhlet extractor, refluxed with ethanol at 85°C for 24h, and dried at a vacuum drying temperature of 50°C. The amino functionalized MCM-48 material is obtained.

Embodiment 2

[0019] Add 10-400 mg / L Mn(II) to a 50 mL Erlenmeyer flask with a stopper, adjust the pH to 7 with a buffer solution, then add 30 mg of amino-functionalized MCM-48 material, control the temperature at 25 ° C for 2 hours, and centrifuge , using ICP-AES to determine the concentration of metal ions remaining in the solution. According to the equilibrium ion concentration and adsorption capacity, draw the isotherm adsorption curve (see figure 1 ), the experimental data were fitted by Langmuir, and the saturated adsorption capacity was calculated to be 63.93mg / g.

Embodiment 3

[0021] In a 50mL Erlenmeyer flask with stopper, add 10-200mg / L Zn(II), adjust the pH to 7 with a buffer solution, then add 30mg of amino-functionalized MCM-48 material, control the temperature at 30°C for 2 hours, and centrifuge , using ICP-AES to determine the concentration of metal ions remaining in the solution. According to the equilibrium ion concentration and adsorption capacity, draw the isotherm adsorption curve (see figure 2 ), the experimental data were fitted by Langmuir, and the saturated adsorption capacity was calculated to be 83.33mg / g.

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Abstract

The invention provides a method for preparing an amino functional MCM-48 mesoporous material. The method comprises the following steps: dissolving a template agent hexadecyl trimethyl ammonium bromide and polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer in water, adding sodium hydroxide, adding sodium fluoride, finally adding tetraethoxysilane and 3-[2-(2-amino ethyl amino)ethyl amino] propyl-trimethoxysilane; wherein the mol ratio of materials is tetraethoxysilane: 3-[2-(2-amino ethyl amino)ethyl amino] propyl-trimethoxysilane: hexadecyl trimethyl ammonium bromide: polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer: NaOH: NaF =1:0.085: 0.13:0.013: 0.5:0.1; stirring for 24 hours under the temperature of 40 DEG C, crystallizing for 24 hours under the temperature of 100 DEG C, washing, filtering, drying to remove the template agent to obtain the amino functional MCM-48 mesoporous material. The method has the advantages of simple operation process and short synthesis time.

Description

technical field [0001] The invention belongs to a preparation method in the technical field of inorganic functional materials and wastewater treatment, and in particular relates to a preparation method of an amino functionalized MCM-48 mesoporous material. Background technique [0002] With the development of society, especially the development of industry, heavy metal pollution has become an increasingly serious environmental problem. Due to the toxicity and non-degradability of heavy metals, they can enter the human body through the food chain and accumulate in certain organs of the human body, causing chronic cumulative poisoning. In order to protect and improve the human living environment, people use various methods to remove heavy metal ions, mainly chemical precipitation, adsorption, ion exchange, solvent extraction and so on. Adsorption is a simple and easy treatment method. Commonly used adsorbents include minerals such as activated carbon, zeolite and bentonite. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/18B01J20/30
Inventor 陈建荣韩亚陈津津古兴兴胡雪娜
Owner 海宁市袁花镇工业投资有限公司