A kind of functionalized post-crosslinking resin and its preparation method and application

A technology of cross-linking resin and functional group is applied in the field of cross-linking resin after functionalization and its preparation, which can solve the problems of high content of impurities, sensitive chemical structure and physical properties of DHA, difficulty in separation and extraction, etc., so as to improve the polarity effect with selectivity, broad use, optimized adsorption performance

Active Publication Date: 2022-04-22
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the problems that the fermentation liquid system has complex impurities, high content of impurities, sensitive chemical structure and physical properties of DHA itself, and difficult separation and extraction, and provides an adsorption resin with high efficiency and high selectivity for adsorption and separation of DHA

Method used

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  • A kind of functionalized post-crosslinking resin and its preparation method and application
  • A kind of functionalized post-crosslinking resin and its preparation method and application
  • A kind of functionalized post-crosslinking resin and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0029] Embodiment 1: Preparation of post-crosslinking resin

[0030] Add 100mL of nitrobenzene and 10g of chlorine balls to a 250mL three-necked flask equipped with a stirrer and a thermometer, and swell at room temperature for 12 hours; add 1.2g of anhydrous aluminum chloride, and mix the system under mechanical stirring at room temperature. The temperature of the system was raised to 135°C, and the timer was started. After reacting for 4 hours, the reaction was stopped; the resin was filtered out and rinsed with industrial ethanol and pure water. Then use industrial ethanol and pure water to wash 4 times under ultrasonic (each time 30min). After cleaning, the resin was moved into a blast drying oven at 70°C and dried for 12 hours to obtain a post-crosslinked resin.

[0031] The reaction equation is as follows:

[0032]

specific Embodiment approach 2

[0033] Embodiment 2: Preparation of oxygen-containing functional group resin

[0034] Step 1: Add 50mL of nitrobenzene and 6g of chlorine balls to a 100mL three-necked bottle equipped with a stirrer and a thermometer, and swell for 12 hours at room temperature; add 1.2g of anhydrous aluminum chloride, and mix the system under mechanical stirring at room temperature. uniform. The temperature of the system was raised to 60°C, and the timer was started. After reacting for 4 hours, the reaction was stopped; the resin was filtered out and rinsed with industrial ethanol and pure water. Then use industrial ethanol and pure water to wash 4 times under ultrasonic (each time 30min). After cleaning, the resin was moved into a blast drying oven at 70°C and dried for 12 hours to obtain a post-crosslinked resin.

[0035]Step 2: Take 5g of post-crosslinking resin and 50mL of N,N-dimethylformamide in a 100mL three-necked flask, and swell for 12h; then add 2.5g of 2,3,4-trihydroxybenzoic ac...

specific Embodiment approach 3

[0038] Embodiment 3: Preparation of nitrogen-containing functional base resin

[0039] Step 1: Add 50mL of nitrobenzene and 6g of chlorine balls to a 100mL three-necked bottle equipped with a stirrer and a thermometer, and swell for 12 hours at room temperature; add 1.2g of anhydrous aluminum chloride, and mix the system under mechanical stirring at room temperature. uniform. The temperature of the system was raised to 60°C, and the timer was started. After reacting for 4 hours, the reaction was stopped; the resin was filtered out and rinsed with industrial ethanol and pure water. Then use industrial ethanol and pure water to wash 4 times under ultrasonic (each time 30min). After cleaning, the resin was moved into a blast drying oven at 70°C and dried for 12 hours to obtain a post-crosslinked resin.

[0040] Step 2: Take 5g of post-crosslinking resin and 50mL of N,N-dimethylformamide in a 100mL three-necked flask, and swell for 12h; control the temperature of the system at ...

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Abstract

The invention discloses a functionalized post-crosslinking resin, a preparation method and application thereof, and belongs to the technical field of resin synthesis and application thereof. The invention aims at the problems that the fermented liquid system has complex impurities, high content of impurities, sensitive chemical structure and physical properties of DHA itself, and difficult separation and extraction. The present invention is based on the chemical structure characteristics of DHA with small molecular size, large polarity, one ketone carbonyl group and two hydroxyl groups, using polystyrene resin as raw material, and adopting Friedel-Crafts alkylation reaction to regulate post-crosslinking reaction through Lewis acid catalysis, endowing post- The cross-linked resin has a higher specific surface area and smaller pore size, and then improves the polarity and selectivity of the resin by introducing functional groups containing nitrogen, oxygen, boron, etc., optimizes the adsorption performance of the resin to DHA, and is equipped with high-efficiency desorption crystallization Process for preparing DHA products. The invention realizes selective adsorption and separation of DHA by relying on the high-efficiency functional base resin, effectively reduces the purification cost of DHA in the fermentation liquid, and at the same time reduces the loss of DHA.

Description

technical field [0001] The invention relates to a functionalized post-crosslinking resin and its preparation method and application, belonging to the technical field of resin synthesis and application. Background technique [0002] DHA (1,3-dihydroxyacetone) is a simple ketose, white powder crystal with sweet taste, easily soluble in water and organic solvents such as ethanol, acetone and ether, with a molecular weight of 90.08. DHA has the characteristics of thermal sensitivity and viscosity increase as the concentration increases, which makes it impossible to directly crystallize and purify it, and the solubility of DHA and the existence of a large number of impurities will affect the crystallization of DHA, and the high temperature conditions in the concentration process will also cause DHA. Massive degradation. [0003] Existing methods for separating and extracting DHA include thin film evaporation, solvent extraction, membrane separation, alcohol precipitation evapora...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/42C08F8/32C08F8/10C08F8/26C08F212/08B01J20/26B01J20/28B01J20/30B01D15/34
CPCC08F8/42C08F8/32C08F8/10C08F8/26B01J20/267B01J20/28066B01J20/2808B01D15/34C08F212/08
Inventor 姜龙徐超咸漠靳超刘耀杰柳林杰
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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