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Preparation method and application of ionic liquid-sodium (mono-/di-)hydrogen phosphate buffer aqueous two-phase system

A two-phase system and ionic liquid technology, applied in the direction of organic chemistry, can solve the problems that liquid-liquid extraction cannot meet the separation requirements, and achieve the effect of strong practical value, easy phase separation, and high enrichment degree

Inactive Publication Date: 2018-04-06
李辉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] With the continuous improvement of environmental protection requirements and the extensive development of high-tech separation technology research work, the traditional liquid-liquid extraction can no longer meet the separation requirements, so a new type of liquid-liquid separation technology - two-aqueous phase extraction (ATPE) Came into being

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Preparation of nicotine-modified ionic liquid: Add 0.5 mmol polyethylene glycol-6000 bridged imidazole and 0.5 Mmol nicotine-nornicotine-neonicotine mixture (molar ratio 6:2:1), heated and stirred in a water bath at 80°C, and reacted for 40 h. After rinsing, add 100mL chloroform and 0.2mmol NaB (C 6 h 5 ) 4 , react at room temperature for 40 hours, then add 2.0 mmol ethylenediamine, and reflux for 10 hours to obtain a variety of nicotine-modified polyethylene glycol-6000 ionic liquids;

[0016] (2) Preparation of two-phase aqueous system: Add 10g of polyethylene glycol-6000 ionic liquid into 2.6mL of acetone solvent, and sonicate for 5min to obtain solution A; add 28g of deionized water to another beaker, and then add 4.8g of phosphoric acid Sodium hydrogen disodium-sodium dihydrogen phosphate mixture (molar ratio 2:1) to obtain solution B; put the container containing 20mL A in a 47°C water bath, slowly add 16mL solution B while stirring, and let stand;

[0017...

Embodiment 2

[0019] (1) Preparation of nicotine-modified ionic liquid: Add 0.5 mmol polyethylene glycol-6000 bridged imidazole and 0.5 Mmol nicotine-nornicotine-neonicotine mixture (molar ratio 18:2:1), heated and stirred in a water bath at 80°C, and reacted for 40 h. After rinsing, add 100mL chloroform and 0.2mmol NaB (C 6 h 5 ) 4 , react at room temperature for 40 hours, then add 2.0 mmol ethylenediamine, and reflux for 10 hours to obtain a variety of nicotine-modified polyethylene glycol-6000 ionic liquids;

[0020] (2) Preparation of two-phase aqueous system: Add 5.3g of polyethylene glycol-6000 ionic liquid to 4.8mL of acetone solvent, sonicate for 5 minutes to obtain solution A; add 16mL of deionized water to another beaker, and then add 7.9g Disodium hydrogen phosphate-sodium dihydrogen phosphate mixture (molar ratio 2:1) to obtain solution B; put the container containing 20mL of A in a 35°C water bath, slowly add 27mL of solution B while stirring, and let stand;

[0021] (3) Ad...

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Abstract

The invention discloses a method for extracting a tobacco alkaloid by a novel nicotine modified ionic liquid-sodium (mono- / di-)hydrogen phosphate buffer aqueous two-phase system. The method comprises(1) preparing a nicotine modified ionic liquid; (2) preparing the aqueous two-phase system; and (3) in the aqueous two-phase solution, adding a solution of a tobacco crude extract to be extracted, performing shaking for 3-7 min, placing the mixture in a water bath pot of 30-50 DEG C, allowing the mixture to be stand, after layering is stable, and separating out the upper phase, so as to obtain 85%or more of the tobacco alkaloid in an initial tobacco extract through once extraction. According to the technical scheme, the aqueous two-phase system of the ionic liquid and the sodium (mono- / di-)hydrogen phosphate buffer is adopted to separate the nicotine, the technological conditions of the aqueous two-phase extraction are selected and optimized, and the method has the advantages of pH-control phase separation, low price, high efficiency and mild extraction, no toxicity, small loss of activity of the extract and the like, and is a green process. At the same time, the aqueous two-phase system of the method has high selectivity and high enrichment degree on the nicotine, and has high practical value.

Description

technical field [0001] The invention relates to a preparation method of an ionic liquid-sodium hydrogen phosphate buffer two-phase system and a method for extracting tobacco alkaloids using the two-phase system. Background technique [0002] Nicotine is a natural alkaloid that mainly exists in tobacco leaves, and its content accounts for about 0.50-10.0% of the dry weight of tobacco. Nicotine is used as an additive to improve the quality of cigarettes and enhance the use value of tobacco leaves. Nicotine series pesticides belong to plant insecticides, which have the characteristics of steam fumigation, stomach poisoning, contact killing and rapid degradation without residue. In agriculture, tobacco base is often used in the manufacture of pesticides to control crop pests such as aphids in field crop production. It is widely used as an insecticide for crops such as grain, oilseeds, vegetables, fruits, pastures, etc. It is an ideal high-efficiency green insecticide and biologi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
Inventor 李辉龚梦婷黄信慧宋俊杰
Owner 李辉
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