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Imprinting-like MOF adsorbent prepared by microwave synthesis method and application of imprinting-like MOF adsorbent

An adsorbent and imprinting technology, applied in other chemical processes, chemical instruments and methods, essential oils/fragrances, etc., to achieve the effect of favorable adsorption, mild conditions, and uniform distribution

Pending Publication Date: 2022-07-19
广州华芳烟用香精有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the problem of adsorption and storage of fragrance in the current flavor and fragrance industry, and provides a novel imprinted MOF adsorbent capable of strongly adsorbing fragrance and its preparation method and application

Method used

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  • Imprinting-like MOF adsorbent prepared by microwave synthesis method and application of imprinting-like MOF adsorbent
  • Imprinting-like MOF adsorbent prepared by microwave synthesis method and application of imprinting-like MOF adsorbent
  • Imprinting-like MOF adsorbent prepared by microwave synthesis method and application of imprinting-like MOF adsorbent

Examples

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Embodiment 1

[0032] Preparation of MOF(Fe) materials: take 1.0 mmol of Fe(NO 3 ) 3 ·9H 2 O in a container, add 15mL ultrapure water to dissolve, add 0.6mmol trimesic acid under stirring conditions and stir for 1h, after thorough mixing, add 75μL of HF and HNO in turn 3 Obtain the suspension; then transfer the suspension to high temperature reaction in the autoclave, after the reaction finishes, clean and centrifuge and then dry to obtain MOF (Fe).

[0033] MOF(Fe) materials are all reacted at high temperature in a programmed temperature oven:

[0034] (a) Heating process: from room temperature to 150°C at a heating rate of 1-10°C / min;

[0035] (b) Constant temperature process: keep at 150℃ for 24h;

[0036](c) Cooling process: immediately after the constant temperature process is over, it is taken out from the drying box and cooled to room temperature naturally.

[0037] The following examples are all the same.

Embodiment 2

[0039] A preparation method of a new type of imprinted MOF (Fe) adsorbent, comprising the following steps:

[0040] (1) Take 1.0 mmol of Fe(NO 3 ) 3 ·9H 2 O in a container, add 15mL ultrapure water to dissolve, add 0.6mmol trimesic acid under stirring condition and stir for 1h, after thorough mixing, add 75μL of HF and HNO in turn 3 to obtain a suspension; then transfer the suspension to a high-temperature reaction in an autoclave, and after the reaction is finished, wash, centrifuge, and dry to obtain MOF (Fe);

[0041] (2) 1.0 mmol MOF (Fe) and 2,6-lutidine in step (1) are placed in a stainless steel ball mill jar according to a molar ratio of 1:0.1, and 6 stainless steel ball mill steel balls with different diameters are placed in ( One is 10.3mm in diameter, and the other 5 are 5.1mm in diameter), perform ball milling, set the ball milling time to 20 minutes, and set the ball milling frequency to 40 Hz; the solid particles obtained by ball milling are uniformly disperse...

Embodiment 3

[0043] A preparation method of a new type of imprinted MOF (Fe) adsorbent, comprising the following steps:

[0044] (1) Take 1.0 mmol of Fe(NO 3 ) 3 ·9H 2 O in a container, add 15mL of ultrapure water to dissolve, add 0.7mmol trimesic acid under stirring conditions and stir for 1h, after thorough mixing, add 75μL of HF and HNO in turn 3 to obtain a suspension; then transfer the suspension to a high-temperature reaction in an autoclave, and after the reaction is finished, wash, centrifuge, and dry to obtain MOF (Fe);

[0045] (2) In step (1), 1.0 mmol MOF (Fe) and anisaldehyde were placed in a stainless steel ball milling jar according to a molar ratio of 1:0.3, and 6 stainless steel ball milling steel balls with different diameters were placed among them (1 ball was 10.3 mm in diameter) , the other 5 particles are 5.1mm in diameter), carry out ball milling, set the ball milling time to 30min, and set the ball milling frequency to 50Hz; the solid particles obtained by ball m...

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Abstract

The invention discloses an imprinting-like MOF adsorbent prepared by a microwave synthesis method and application of the imprinting-like MOF adsorbent. The preparation method comprises the following steps: firstly, hydrothermally synthesizing MOF (Fe) according to an existing method; then placing the MOF (Fe) and imprinted molecules in a stainless steel ball milling tank for ball milling; after ball milling is completed, solid particles obtained through ball milling are evenly dispersed into an ethanol solvent, and then the solid particles are transferred into a microwave-assisted synthesizer to be subjected to a ligand replacement reaction; after the reaction is finished, carrying out centrifugal collection, and carrying out water bath activation in an ethanol water solution; and finally, cleaning, centrifuging and drying to obtain the imprinting-like MOF adsorbent. According to the preparation method, imprinting molecules can be uniformly dispersed in a framework of MOF through ball milling, the MOF generates lattice defects, then post-ligand replacement is realized through high energy generated by microwaves, an imprinting function is generated, and a powerful adsorption effect on perfume with an imprinting molecule similar structure is achieved.

Description

technical field [0001] The invention belongs to the field of porous crystal materials, and in particular relates to a kind of imprinted MOF adsorbent prepared by a microwave synthesis method and its application. Background technique [0002] At present, in my country's food flavoring and cigarette flavoring industries, consumers have gradually put forward higher requirements for various products, such as food and cigarettes with special or rich flavors. This also brings challenges and development to the flavor and fragrance industry. And how to realize the efficient storage of fragrance molecules is a problem that the flavor and fragrance industry needs to constantly explore and improve. Among many aroma storage methods, adsorption method is currently the most promising method in industry. It uses porous materials as aroma storage materials, and uses the pore structure and surface properties of materials to achieve adsorption and storage with aroma molecules. The core of t...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C11B9/00
CPCB01J20/226B01J20/3057C11B9/00
Inventor 黄艳卢真保周叶燕赵世兴林德洪孙胜南王学娟陈志雄
Owner 广州华芳烟用香精有限公司
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