Amino-functionalization ordered mesopore phenolic resin material and preparing method thereof

A technology of amino functionalization and phenolic resin, applied in the field of phenolic resin materials, can solve the problems of high cost, low utilization rate of nitrogen source, harmful environment, etc., and achieve the effect of short synthesis cycle, large specific surface area and avoiding post-processing

Inactive Publication Date: 2016-05-11
SHANGHAI NORMAL UNIVERSITY
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Problems solved by technology

Traditional amino-functionalized ordered mesoporous materials are mostly synthesized in the following two ways: the first is to graft amino groups onto them by post-treatment, that is, to synthesize ordered mesoporous materials first, and then through nitration or ammonia gas treatment. Amino groups are connected, but this synthesis method is tedious, the order degree of ordered mesoporous materials is low, the cost is very high, and the nitrogen source utilization rate is low, harmful to the environment, and the industrialization feasibility is low; the second method uses phenol and metaspores. Aminophenol and other nitrogen sources are co-doped and synthesized by polymerization, but in this method, the amino group will react with the carbonyl group to form a Schiff base, which will affect the degree of cross-linking polymerization. Therefore, the nitrogen content of the ordered mesoporous material obtained by this method very low

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  • Amino-functionalization ordered mesopore phenolic resin material and preparing method thereof
  • Amino-functionalization ordered mesopore phenolic resin material and preparing method thereof
  • Amino-functionalization ordered mesopore phenolic resin material and preparing method thereof

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[0018] Some embodiments of one aspect of the present invention provide a method for preparing an amino-functionalized ordered mesoporous phenolic resin material, which includes: using m-nitrophenol and formaldehyde as raw materials, synthesizing a soluble phenolic resin in an alkaline liquid phase environment The precursor is then mixed with the template agent in an organic solution, and the cured intermediate is obtained by the method of solvent volatilization and self-assembly, and finally the cured intermediate is placed in a protective atmosphere and roasted to remove the template agent, that is, the amino functionalized Ordered mesoporous phenolic resin materials.

[0019] In a preferred embodiment, the preparation method comprises the following steps:

[0020] (1) reacting m-nitrophenol and formaldehyde in an alkaline liquid phase system environment and at a temperature of 100-120°C for more than 1 hour to form a nitro-functionalized phenolic resin precursor,

[0021] (...

Embodiment 1

[0053] Step 1: Synthesis of nitro-functionalized polymer precursors: Add 1.127g m-nitrophenol to a three-necked flask equipped with a stirrer in an oil bath at 40°C, and then add 2.413ml of 35-40wt% formaldehyde solution, stirred for 30min to dissolve and mix well. Add saturated sodium hydroxide alcohol solution, adjust the pH between 8 and 9, stir for 30min, raise the temperature to 110°C, adjust the rotation speed to 350rpm, stir at constant temperature for 2h, cool to room temperature after the reaction, and then adjust with 2mol / L hydrochloric acid solution The pH of the reaction solution is 7. After concentrating and evaporating to remove water at 50° C., four times of absolute ethanol is added to dilute and dissolve according to the mass ratio of the reaction solution to obtain a soluble precursor of nitro-functionalized resole phenolic resin.

[0054] Step 2: Self-assembly of nitro-functionalization: Mix and stir 1gF127, a triblock copolymer template agent, and 20g abso...

Embodiment 2

[0057] Step 1: Synthesis of nitro-functionalized polymer precursors: Add 3.381g m-nitrophenol to a three-necked flask equipped with a stirrer in an oil bath at 40°C, and then add 7.239ml of 35-40wt% formaldehyde solution, stirred for 30min to dissolve and mix well. Add saturated sodium hydroxide alcohol solution, adjust the pH between 8 and 9, stir for 30min, raise the temperature to 110°C, adjust the rotation speed to 350rpm, stir at constant temperature for 2h, cool to room temperature after the reaction, and then adjust with 2mol / L hydrochloric acid solution The pH of the reaction solution is 7. After concentrating and evaporating to remove water at 50° C., four times of absolute ethanol is added to dilute and dissolve according to the mass ratio of the reaction solution to obtain a soluble nitro-functionalized resole phenolic resin precursor.

[0058] Step 2: Nitro-functionalized self-assembly: Mix and stir 1gF127, a triblock copolymer template agent, and 20g absolute etha...

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Abstract

The invention discloses an amino-functionalization ordered mesopore phenolic resin material and a preparing method thereof. The amino-functionalization ordered mesopore phenolic resin material comprises ordered mesopore phenolic resin and amino at least distributed on a pore path inner wall of the ordered mesopore phenolic resin, and the port path is regular and ordered and has an aperture of 3-5nm. The preparing process is simple, short in synthetic period, good in controllability, low in cost and suitable for large scale implementation, and accords with the requirements of green chemistry. The amino-functionalization ordered mesopore phenolic resin material has a two dimensional hexagonal ordered mesopore structure, is high in degree of order, large in specific area, rich in active amino sites, and has wide application prospect in fields of organic alkali catalytic reaction, CO2 adsorption and heavy metal ion adsorption, and the like.

Description

technical field [0001] The invention relates to a phenolic resin material, in particular to an amino functionalized ordered mesoporous phenolic resin material and a preparation method thereof. Background technique [0002] Amino-functionalized ordered mesoporous phenolic resin polymer materials play an important role in the fields of energy storage and conversion, catalysis, adsorption and separation due to their special structure and surface properties. The pore size of ordered mesoporous polymers is 2-50nm, the pore size is uniform, and the pores are arranged in an orderly manner, which is a hot topic emerging in recent years. Traditional amino-functionalized ordered mesoporous materials are mostly synthesized in the following two ways: the first is to graft amino groups onto them by post-treatment, that is, to synthesize ordered mesoporous materials first, and then through nitration or ammonia gas treatment. Amino groups are connected, but this synthesis method is tediou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/16C08J9/26
CPCC08G8/16C08J9/26C08J2361/10
Inventor 张昉王凯旋阳利平赵伟亮李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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