Nonpolar macroporous adsorption resin carboxylation modification method for glycyrrhizic acid adsorption

A technology of non-polar macroporous and adsorbent resins, which is applied in the field of carboxylation modification of non-polar macroporous adsorbent resins, which can solve the problems of insignificant improvement of adsorbate adsorption effect, high crosslinking degree of macroporous adsorbent resins, functional low reaction efficiency

Inactive Publication Date: 2018-11-20
NINGXIA PAGODA CHEM CENT LAB CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the macroporous adsorption resin has a high degree of cross-linking, low functionalization reaction efficiency, and a low amount of functional groups introduced, and the improvement of the ads

Method used

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  • Nonpolar macroporous adsorption resin carboxylation modification method for glycyrrhizic acid adsorption

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Chloromethylation reaction

[0022] Accurately weigh 10.0 g of non-polar macroporous adsorption resin L1 that has been air-dried to constant weight and put it into a three-necked flask equipped with a stirrer and a condenser, and add 40 mL of CCl 4 After swelling at 60 °C for 30 h, the reaction device was moved into an ultrasonic reaction device. The pretreated ZnCl 2 Add 4.5 g of catalyst into the reactor, add 15 g of chloromethyl ether, and stop the reaction after reacting in an ultrasonic environment with ultrasonic power of 75 W at a temperature of 50 °C for 20 h. Transfer the macroporous adsorption resin in the reactor into the funnel of the sand core, wash with methanol and distilled water successively, repeatedly check and rinse until AgNO is added to the distilled water of the washing resin. 3 Until there is no obvious white precipitate, the chloromethylated L1 (L1-Cl) is obtained. After calculation, the degree of chloromethylation of the chloromethyl...

Embodiment 2

[0026] Step 1: Chloromethylation reaction

[0027] Precisely weigh 10 g of non-polar macroporous adsorption resin L1 that has been air-dried to constant weight and put it into a three-neck flask equipped with a stirrer and a condenser tube, add 40 mL of toluene to swell at 60 °C for 36 h, and put the reaction device Transfer to an ultrasonic reaction device. The pretreated ZnCl 2 5.0 g of catalyst was added into the reactor, 15 g of chloromethyl ether was added, and the reaction was stopped after 20 h of reaction in an ultrasonic environment with an ultrasonic power of 100 W at a temperature of 50 °C. Transfer the macroporous adsorption resin in the reactor into the funnel of the sand core, wash with methanol and distilled water successively, repeatedly check and rinse until AgNO is added to the distilled water of the washing resin. 3 Until there is no obvious white precipitate, the chloromethylated L1 (L1-Cl) is obtained. After calculation, the degree of chloromethylation ...

Embodiment 3

[0031] Step 1: Chloromethylation reaction

[0032] Accurately weigh 10 g of non-polar macroporous adsorption resin L1 that has been air-dried to constant weight and put it into a three-necked flask equipped with a stirrer and a condenser, and add a mixture of carbon tetrachloride and chloroform ( V CCl4 : V CHCl3 = 1:1) as a solvent, after swelling at 60 °C for 48 h, the reaction device was moved into an ultrasonic reaction device. The pretreated ZnCl 2 5.0 g of catalyst was added into the reactor, 20 g of chloromethyl ether was added, and the reaction was stopped after 36 h of reaction in an ultrasonic environment with an ultrasonic power of 75 W at a temperature of 50 °C. Transfer the macroporous adsorption resin in the reactor into the funnel of the sand core, wash with methanol and distilled water successively, repeatedly check and rinse until AgNO is added to the distilled water of the washing resin. 3Until there is no obvious white precipitate, the chloromethylat...

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Abstract

The invention discloses a nonpolar macroporous adsorption resin carboxylation modification method for glycyrrhizic acid adsorption. Macroporous adsorption resin modification mainly comprises two steps, namely, chloromethylation reactions are implemented on a nonpolar macroporous resin through an ultrasonic catalysis reaction firstly, and then the reaction activity of the macroporous adsorption resin can be improved; secondly, the resin is reacted with a carboxylic acid functional monomer, and then a carboxylation modification macroporous adsorption resin can be prepared. Through the ultrasoniccatalysis reaction, under the action of a chloromethylation reagent, the macroporous adsorption resin of a high carboxylation degree can be prepared, and adsorption capacity tests on glycyrrhizic acid with the modified macroporous adsorption resin show that the adsorption capacity of the modified carboxylation macroporous adsorption resin upon the glycyrrhizic acid is increased when being compared with that of an unmodified macroporous adsorption resin.

Description

technical field [0001] The invention relates to a preparation method for carboxylation modification of a non-polar macroporous adsorption resin used for glycyrrhizic acid adsorption. Background technique [0002] Macroporous adsorption resin is a kind of functional polymer material prepared by suspension polymerization or reverse suspension polymerization from polymerizable components such as polymers and crosslinking agents and additives such as porogens and dispersants. The interior also has high porosity, so it is called macroporous adsorption resin. Macroporous adsorption resin is a functional polymer material integrating adsorption and sieving due to its well-developed voids, high relative area, and different functional groups. It is mainly divided into non-polar Sexual, weakly polar and polar macroporous adsorption resins. By controlling the synthesis conditions, the pore structure of the macroporous adsorption resin can be changed, thereby producing different adsorp...

Claims

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Application Information

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IPC IPC(8): C08F8/32C08F8/24
CPCC08F8/24C08F8/32
Inventor 康磊于惠杨晓丽孙培华张秉钧杨惠琳
Owner NINGXIA PAGODA CHEM CENT LAB CO LTD
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