A method for separating and purifying o-hydroxyl compounds

A technology for separation and purification of adjacent hydroxyl groups, which is applied in quinone separation/purification, chemical/physical processes, ion exchange, etc. It can solve the problems of difficult flotation to separate water-soluble targets, destroy biological activity, and low efficiency, and achieve a simple and convenient system and method of operation, high purity, and effect of large upper phase volume

Active Publication Date: 2018-10-09
JIANGSU UNIV
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  • Claims
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of traditional organic solvent extraction, two-phase extraction and solvent flotation techniques such as large material consumption, low efficiency, large pollution and destruction of biological activity, and solve the problem of difficult selective flotation separation of water-soluble extracts from natural product extraction feed liquids. To solve the problem of specific goals, provide a method for the separation and purification of ortho-hydroxyl compounds in a two-phase flotation system using a temperature-sensitive block polymer as a collector, and realize the flotation separation of the model compound water-soluble alizarin red

Method used

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  • A method for separating and purifying o-hydroxyl compounds

Examples

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Comparison scheme
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Embodiment 1

[0036] Example 1: Phenylboronic acid functionalized PEO 20 PPOs 60 PEOs 20 Synthesis

[0037] Add 0.12 g of m-carboxyphenylboronic acid into 17.50 mL of dichloromethane, fully dissolve it, add 124 μL of oxalyl chloride, and add 4 drops of N,N-dimethylformamide dropwise to initiate the reaction. The obtained solution was stirred and reacted at room temperature for 12 h, and then the solvent was removed by rotary distillation under reduced pressure to obtain 0.12 g of 3-formylchlorophenylboronic acid as a yellow liquid product. 0.12 g of product 3-formylchlorophenylboronic acid was dissolved in 17.50 mL of dichloromethane to obtain solution A; 0.50 g of PEO 20 PPOs 60 PEOs 20 Dissolve in 35.00 mL of dichloromethane, and add 150 μL of triethylamine to it to obtain solution B. Then, all 17.50 mL of solution A was dropped into 35.00 mL of solution B under cooling in an ice-water bath. After the dropwise addition was complete, the ice-water bath was removed, and the system wa...

Embodiment 2

[0042] Example 2: Separation and purification of o-hydroxyl compounds by two-phase flotation system

[0043] (1) Add 0.1 mg Alizarin Red and 8 g K to a 50 mL colorimetric tube 2 HPO 4 , then add

[0044] The phenylboronic acid functionalized PEO prepared in 0.05g embodiment 1 20 PPOs 60 PEOs 20 As a flotation collector and diluted to 50 mL with distilled water, the solution system was fully shaken to mix evenly. The resulting solution was left to stand for 15 min and then poured into a flotation column, followed by adding 5 mL of n-propanol, adjusting the gas flow to 5 mL / min and starting flotation. After 10 min, the system separated into two phases.

[0045] (2) After phase separation, record the volume of the upper phase as 2.9 mL, and measure the concentration of alizarin red as follows: Take 1.00 mL of the sample to be tested and mix it with 9.00 mL of citric acid-sodium citrate buffer solution (pH=4) at 10.00 mL plastic centrifuge tube, fully shake the solution to ...

Embodiment 3

[0046] Example 3: Separation and purification of o-hydroxy compounds by two-phase flotation system

[0047] (1) Add 1 mg Alizarin Red and 16 g K to a 50 mL colorimetric tube 2 HPO 4 , then add

[0048] The phenylboronic acid functionalized PEO prepared in 0.4 g embodiment 1 20 PPOs 60 PEOs 20 As a flotation collector and diluted to 50 mL with distilled water, the solution system was fully shaken to mix evenly. The resulting solution was left to stand for 15 min and then poured into a flotation column, followed by adding 5 mL of n-propanol, adjusting the gas flow to 25 mL / min and starting flotation. After 50 min, the system separated into two phases.

[0049] (2) After phase separation, record the volume of the upper phase as 4.1 mL, and measure the concentration of alizarin red as follows: Take 1.00 mL of the sample to be tested and mix it with 9.00 mL of citric acid-sodium citrate buffer solution (pH=4) at 10.00 mL plastic centrifuge tube, fully shake the solution to m...

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Abstract

The invention relates to a method for separating and purifying an o-hydroxyl compound, and belongs to the field of natural product separation and purification. The method comprises the steps that firstly, alizarin red and K2HPO4 are added into a colorimetric tube, then phenylboronic acid functionalized PEO20PPO60PEO20 is added, the solution is diluted with distilled water, full shaking is carried out, and the mixture is mixed to be uniform; the mixture is poured into a flotation column after still standing, then normal propyl alcohol is added, gas flowing speed is regulated, and flotation is started; after the system is divided into two phases, the volume of the upper phase is recorded, and the alizarin red concentration in the upper phase is measured. The double aqueous phase flotation system is set up for flotation separation of o-hydroxyl compound alizarin red; synthesized phenylboronic acid functionalized PEO20PPO60PEO20 is added to serve as a complementing agent and can be effectively combined with alizarin red, meanwhile, functionalized PEO20PPO60PEO20 can be effectively adsorbed on a hydrophobic bubble interface, and flotation separation of water-soluble alizarin red is achieved; obtained alizarin red is large in the enrichment factor and high in purity, and the yield of the product can be increased.

Description

technical field [0001] The invention relates to a method for separating and purifying o-hydroxy compounds, in particular to a method for separating and purifying o-hydroxy compounds based on a temperature-sensitive block polymer-based two-phase flotation system, and belongs to the field of separation and purification of natural products. Background technique [0002] As an important class of natural products, natural ortho-hydroxy compounds (such as polysaccharides, anthocyanins, proanthocyanidins, etc.) have attracted attention for their good anti-oxidation, anti-cancer and anti-aging properties, so they are widely used in the field of medicine and health care. The separation and purification method widely used in industrial production is organic solvent extraction. However, a large amount of organic solvents are used in the process of this method, which will inevitably lead to higher material consumption and serious environmental pollution. More importantly, the use of a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C46/10C07C50/34C08G65/48C08G65/337B01D15/08B01D11/04
CPCB01D11/04B01D15/08C07C46/10C08G65/337C08G65/48C08G65/485C07C50/34
Inventor 王赟韩娟李媛媛陈桐毛艳丽李春梅王蕾倪良
Owner JIANGSU UNIV
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