Preparation method of phenolic resin with cross-linked amino structure and application thereof

A technology of phenolic resin and cross-linked amine groups, which is applied in the field of preparation of highly selective adsorption resins, can solve the problems of limiting the reaction efficiency of amine functional groups, limited content of amine functional groups, complex resin synthesis steps, etc., and achieves production costs Low, low extraction efficiency, good use strength effect

Active Publication Date: 2013-08-28
河北利江生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the following defects still exist in the existing synthesis process: 1) The amine functional group is introduced through a chemical reaction on the highly cross-linked phenolic skeleton, and the highly cross-linked structure has a large steric hindrance effect, which limits The improvement of the reaction efficiency of the amine functional group; 2) The phenolic resin skeleton is a highly cross-linked skeleton structure obtained by forming a cross-linked bridge through the Mannich reaction of the ortho- and para-positions of the phenolic phenolic hydroxyl group, but the functional group of the amine group During the reaction, the Mannich reaction was also used at the ortho- and para-reaction sites of the phenolic hydroxyl group, which brought about a great contradiction in the synthesis process, that is, in order to maintain the highly cross-linked skeleton structure of the resin, sufficient occupation of formaldehyde is required. The phenolic hydroxyl group is in the ortho and para positions, which makes the subsequent amination reaction lack the necessary reaction sites; 3) Since the amine functional group is introduced through the Mannich reaction after the polymerization is completed, the resin synthesis steps are relatively complicated, and in The amination reaction requires a large amount of organic solvent to swell the phenolic resin skeleton
Therefore, the content of amino functional groups introduced in the phenolic resin skeleton is limited, and the synthesis cost is greatly increased

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method with the phenolic resin of cross-linked amino structure, the steps are as follows:

[0022] 1) Dissolve 20 g of phenol, 7.66 g of paraformaldehyde and 0.26 g of sodium hydroxide in 17.66 g of ethylene glycol in a 500 mL three-necked flask equipped with electric stirring, temperature control device, and reflux condenser, and heat to 90 ℃, keep warm for 2.5 h, then add 3.83 g paraformaldehyde and 3.83 g ethylenediamine into the reaction bottle, keep warm for 30 min, adjust the pH to 1.0 with a hydrochloric acid solution with a mass percent concentration of 36%, and obtain the reaction phase;

[0023] 2) Prepare a turbine oil containing Tween 80 mass percent with a concentration of 1% in a beaker as the dispersed phase;

[0024] 3) Mix the above-mentioned dispersed phase with the reaction phase for polymerization reaction, the mass ratio of the reaction phase and the dispersed phase is 1:2, stir the mixed solution and adjust the stirring speed ...

Embodiment 2

[0031] A kind of preparation method with the phenolic resin of cross-linked amino structure, the steps are as follows:

[0032] 1) Dissolve 30 g of phenol, 11.48 g of paraformaldehyde and 0.39 g of sodium hydroxide in 60.63 g of ethylene glycol in a 1000 mL three-neck flask equipped with electric stirring, temperature control device, and reflux condenser, and heat to 85 ℃, keep warm for 3 h, then add 9.57 g of paraformaldehyde and 9.57 g of ethylenediamine into the reaction flask, react at 80 °C for 30 min, adjust the pH to 1.5 with a hydrochloric acid solution with a mass percent concentration of 36%, and obtain the reaction phase;

[0033] 2) Prepare a turbine oil containing Tween 80 mass percent with a concentration of 1% in a beaker as the dispersed phase;

[0034] 3) Mix the above-mentioned dispersed phase with the reaction phase for polymerization reaction. The mass ratio of the reaction phase and the dispersed phase is 1:3. Stir the mixed solution and adjust the stirrin...

Embodiment 3

[0041] A kind of preparation method with the phenolic resin of cross-linked amino structure, the steps are as follows:

[0042] 1) Dissolve 30 g of phenol, 11.48 g of paraformaldehyde and 0.39 g of sodium hydroxide in 102.45 g of ethylene glycol in a 1000 mL three-necked flask equipped with electric stirring, temperature control device, and reflux condenser, and heat to 95°C Insulate for 2 hours, then add 9.57g of paraformaldehyde and 16.44g of diethylenetriamine into the reaction flask, react at 80°C for 30 minutes, adjust the pH to 1.5 with a hydrochloric acid solution with a concentration of 36% by mass, and obtain the reaction phase;

[0043] 2) Prepare a turbine oil containing Tween 80 mass percent with a concentration of 1% in a beaker as the dispersed phase;

[0044] 3) Mix the above-mentioned dispersed phase with the reaction phase for polymerization reaction, the mass ratio of the reaction phase and the dispersed phase is 1:2, stir the mixed solution and adjust the st...

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Abstract

The invention discloses a preparation method of phenolic resin with a cross-linked amino structure, which comprises the following steps of: 1) dissolving phenol, paraformaldehyde and sodium hydroxide in ethylene glycol, heating and preserving heat, and adding paraformaldehyde and a polyamine compound to obtain a reaction phase; 2) preparing Tween80-containing turbine oil with mass concentration of 1% as a dispersion phase; and 3) mixing the dispersion phase and the reaction phase for polymerization reaction, and performing filtration, washing and extraction to obtain the target object. The prepared phenolic resin with a cross-linked amino structure is used for extracting a high-purity curcumin compound from turmeric. The method disclosed by the invention has the advantages that the phenolic resin has good strength in use, and the polarity of resin is improved due to the existence of phenolic hydroxyl; under the hydrogen bond effect of the phenolic resin, a high-purity turmeric extract can be obtained through a simple one-step technology of 'adsorption-elution'; and moreover, the production cost is low, the extraction efficiency is high, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a highly selective adsorption resin for extracting natural curcumin, in particular to a preparation method of a phenolic resin with a cross-linked amine structure and its application. Background technique [0002] Curcumin is an active ingredient of turmeric, a plant of the Zingiberaceae family. It has various pharmacological activities, such as anti-inflammatory, anti-oxidation, hypolipidemic and anti-cancer activities. At the same time, curcumin has strong coloring ability and bright color, and the coloring ability is 3-4 times that of lemon yellow. times, is generally recognized at home and abroad as a natural pigment with high practicability. In recent years, a lot of fruitful work has been carried out on the extraction and purification of curcumin at home and abroad. The existing extraction methods include organic solvent extraction, lye extraction, enzymatic extraction, supercritical CO 2 fluid e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/073B01J20/26B01J20/30B01D11/02B01D15/00C07C49/255C07C45/79
Inventor 王春红巴晶施荣富
Owner 河北利江生物科技有限公司
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