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Quaternary ammonium class ionic liquid compound containing hydroxy groups and preparation method thereof

A technology for ionic liquids and compounds, which is applied in the field of quaternary ammonium ionic liquid compounds and their preparation, can solve the problems of inability to separate components and poor economic efficiency, and achieve the effects of green and environmental protection in the synthesis process, improved separation ability, and wide application prospects

Inactive Publication Date: 2012-09-12
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Distillation is one of the most important methods for separating homogeneous liquid mixtures in industrial production, but for some systems with relatively small differences in volatility, conventional distillation operations are less economical, and for systems with azeotropic compositions, Conventional distillation cannot achieve the separation of components

Method used

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  • Quaternary ammonium class ionic liquid compound containing hydroxy groups and preparation method thereof
  • Quaternary ammonium class ionic liquid compound containing hydroxy groups and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix 44.57 grams (0.5 moles) of N,N-dimethylethanolamine and 91.08 grams (0.5 moles) of triethyl phosphate in a round-bottomed flask with a condenser, and raise the temperature to 150°C through a constant temperature bath while stirring. The reaction was maintained at a constant temperature for 10 hours, and a weak nitrogen flow was maintained as a protective gas during the entire reaction process. After the reaction was completed and cooled to room temperature, the crude product was washed several times with ether, and then dried in vacuum at 120°C for 24 hours to obtain ethyl (hydroxyethyl) dimethyl quaternary ammonium diethyl phosphate. The reaction yield (in N , N-dimethylethanolamine) was 91.1%.

[0025] The result of the nuclear magnetic resonance analysis of this product is: 1 HNMR(300mHz, DMSO-d6): δ 3.97(2H); 3.57(4H); 3.43(2H); 3.30(6H); 3.28(2H); The analysis result of mass spectrometry (MS) was: m / z 271.2. Elemental analysis (EA) results were: C: 44.51%; H...

Embodiment 2

[0027] Mix 52.22 grams (0.35 moles) of triethanolamine and 133.16 grams (0.5 moles) of tributyl phosphate in a round-bottomed flask with a condenser, raise the temperature to 130 ° C through a constant temperature bath while stirring, and keep the constant temperature for 16 hours. A weak nitrogen flow was maintained as a protective gas throughout the reaction. After the reaction was completed and cooled to room temperature, the crude product was washed several times with ether, and then vacuum-dried at 120°C for 6 hours, that is, butyl trihydroxyethyl quaternary ammonium dibutyl phosphate, and the reaction yield (calculated as triethanolamine) was 93.6 %.

[0028] The result of the nuclear magnetic resonance analysis of this product is: 1 HNMR(300mHz, DMSO-d6): δ 3.97(6H); 3.53(6H); 3.24(2H); 1.73(2H); 1.48(4H); 1.33(6H); 0.96(9H). The analysis result of mass spectrometry (MS) was: m / z 415.5. Elemental analysis (EA) results were: C: 52.25%; H: 10.31%; N: 3.30% (calculated:...

Embodiment 3

[0030] Mix 143.45 grams (0.75 moles) of triisopropanolamine and 77.1 grams (0.5 moles) of diethyl sulfate in a round-bottomed flask with a condenser, raise the temperature to 100°C through a constant temperature bath while stirring, and maintain a constant temperature reaction For 24 hours, a slight nitrogen flow was maintained as a protective gas throughout the reaction. After the reaction was finished and cooled to room temperature, the crude product was washed several times with ethanol, and then vacuum-dried at 80°C for 48 hours to obtain trihydroxyisopropyl ethyl quaternary ammonium ethyl sulfate. The reaction yield (in terms of isopropanolamine ) was 80.3%.

[0031] The result of the nuclear magnetic resonance analysis of this product is: 1 HNMR(300mHz, DMSO-d6): δ 4.02(3H); 3.57(2H); 3.39(6H); 3.28(2H); 1.39(3H); 1.25(3H); 1.21(9H). The analysis result of mass spectrometry (MS) was: m / z 345.5. Elemental analysis (EA) results were: C: 45.02%; H: 8.81%; N: 4.11% (calcu...

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Abstract

The invention discloses a quaternary ammonium class ionic liquid compound containing hydroxy groups, which is used for extracting and rectifying systems, such as normal hexane-benzene, cyclohexane-benzene, ethanol-water and the like. The invention also provides a preparation method of the quaternary ammonium class ionic liquid compound containing the hydroxy groups. The ionic liquid compound disclosed by the invention has the characteristics that ionic liquid is not volatilized and has a liquid state of positive and negative ions and the separation performance of a compound containing hydroxy groups is high. The quaternary ammonium class ionic liquid compound containing the hydroxy groups is also synthesized at one step by adopting a common chemical raw materials, so that the price is low.

Description

technical field [0001] The invention relates to an ionic liquid compound and a preparation method thereof, in particular to a hydroxyl-containing quaternary ammonium ionic liquid compound and a preparation method thereof. Background technique [0002] Distillation is one of the most important methods for separating homogeneous liquid mixtures in industrial production, but for some systems with relatively small differences in volatility, conventional distillation operations are less economical, and for systems with azeotropic compositions, Conventional distillation cannot achieve the separation of components. In view of this situation, researchers have developed a special distillation process, that is, to achieve separation by adding other components to the system to change their relative volatility. According to the different interaction principles between the added components and the original system, these special rectification methods can be divided into azeotropic rectif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11C07C305/08C07C303/24C07C215/40C07C213/08
Inventor 焦真王献伟杨前前
Owner SOUTHEAST UNIV
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