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Method for preparing adsorption resin from aromatic ether micromolecule

A technology for adsorbing resins and small molecules, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of low oxygen content of resins, carcinogenicity, complicated reaction steps, etc., and achieve large pore size, high polarity, and preparation process. simple effect

Inactive Publication Date: 2015-04-08
HENAN AGRICULTURAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction steps of the above-mentioned preparation method are loaded down with trivial details, and the oxygen content of the obtained resin is not high
[0003] At present, there are many literature reports on the synthesis of adsorption resins. Chinese invention patent CN101698702B discloses a method for preparing high specific surface area adsorption resins from aromatic hydrocarbon small molecule compounds. Specifically, aromatic small molecules and chloromethyl ether are used to catalyze Chloromethylation first, and then post-crosslinking under the catalysis of anhydrous ferric chloride to obtain a non-polar ultra-high crosslinking adsorption resin. The chloromethylation reagent chloromethyl ether used in the synthesis of the resin is carcinogenic

Method used

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  • Method for preparing adsorption resin from aromatic ether micromolecule
  • Method for preparing adsorption resin from aromatic ether micromolecule

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Embodiment 1

[0026] A method for preparing ultra-high cross-linked adsorption resins by aromatic ether small molecules, comprising the following steps:

[0027] (1) Take 2.0 mL (16.5 mmol) of aromatic ether small molecule phenetole and 3.2517 g (16.5 mmol) of 1,4-dichloromethoxybutane as basic raw materials, add them to the reaction vessel, and then add solvent 1,4 - 20 mL of dichloroethane, stirred at room temperature for 5 min until the raw materials were completely dissolved, then added the catalyst anhydrous zinc chloride 3.2150 g (24 mmol), raised the temperature to 60 °C for chloromethylation reaction, and the reaction time was 3 h;

[0028] (2) Then raise the temperature to 75 °C and continue the reaction for 7 h. After the reaction is completed, cool to room temperature;

[0029] (3) The cooled product obtained in step (2) was added to 30 mL of 2% dilute hydrochloric acid, heated and boiled for 3 h, and then Soxhlet extracted for 6 h;

[0030] (4) Wash the resin extracted in step ...

Embodiment 2

[0032] A method for preparing ultra-high cross-linked adsorption resins by aromatic ether small molecules, comprising the following steps:

[0033] (1) Add 0.87 mL (8 mmol) of aromatic ether small molecule anisole and 1.5766 g (8 mmol) of 1,4-dichloromethoxybutane as basic raw materials into the reaction vessel, and then add solvent 1, 15 mL of 4-dichloroethane was stirred at room temperature for 10 min until the raw material was completely dissolved, then 1.4320 g (10.5 mmol) of anhydrous zinc chloride was added as a catalyst, and the temperature was raised to 40 °C for chloromethylation reaction, and the reaction time was 4 h .

[0034] (2) Then raise the temperature to 65 °C and continue the reaction for 8 h. After the reaction is completed, cool to room temperature;

[0035] (3) Add the cooled product obtained in step (2) into 20 mL of 3% dilute hydrochloric acid and heat to boil for 6 h, then Soxhlet extraction for 3 h;

[0036] (4) Wash the resin extracted in step (3) ...

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Abstract

The invention discloses a method for preparing adsorption resin from an aromatic ether micromolecule. The aromatic ether micromolecule and 1,4-bis(chloromethoxy)butane as basic raw materials undergo a reaction in the presence of a catalyst to produce the adsorption resin. The method has simple processes and utilizes the nontoxic and harmless raw materials. The prepared adsorption resin has a high specific surface area and large apertures, has polarity superior to that of adsorption resin synthesized by the traditional method and has good adsorption effects.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a method for preparing an adsorption resin from aromatic ether small molecules. Background technique [0002] With the gradual expansion of the application fields of adsorption resins, the design and synthesis of oxygen-containing adsorption resins has always been one of the research hotspots of material scientists. At present, the method of synthesizing this kind of oxygen-containing adsorption resin is as follows: the prepared adsorption resin is firstly swollen with a solvent, then chloromethylated, and finally modified with oxygen-containing aromatic small molecules. The reaction steps of the above preparation method are cumbersome, and the oxygen content of the obtained resin is not high. [0003] At present, there are many literature reports on the synthesis of adsorption resins. Chinese invention patent CN101698702B discloses a method for preparing high specific s...

Claims

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Application Information

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IPC IPC(8): C08G61/02B01J20/26B01J20/30
Inventor 金秋李潮海张泽志谢普会原思国
Owner HENAN AGRICULTURAL UNIVERSITY