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Two selective ionic liquids and synthesis method thereof

An ionic liquid and selective technology, which is applied in the preparation of test samples, instruments, and analysis materials, etc., can solve problems affecting the development of male reproductive system, girls' breast development, premature puberty, and reproductive system deformity, etc., and achieves a simple and controllable preparation process , the reaction process is stable, and the effect of protecting the environment

Inactive Publication Date: 2014-07-16
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"Environmental Health Perspectives" and other important international academic journals reported that the main plasticizer phthalates can cause allergic symptoms in children, cause endocrine disorders and premature breast development in girls, affect the development of the male reproductive system and even cause reproductive system deformities And metabolic dysfunction, etc., which seriously endanger human health

Method used

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  • Two selective ionic liquids and synthesis method thereof
  • Two selective ionic liquids and synthesis method thereof
  • Two selective ionic liquids and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0016] 1-Acetoxymethyl-3-methylimidazolium bistrifluoromethylsulfonimide salt ([CH 2 COOCH 3 MIM] NTf 2 )

[0017] in N 2 Under protection, use 25ml of acetonitrile as a solvent, add 7.9mL (0.1mol) of N-methylimidazole to the reaction vessel, slowly add 9.3mL (0.1mol) methyl bromoacetate dropwise to the reaction vessel, and make it react with bromoacetic acid The molar ratio of methyl ester is 1:1~1.5. First, stir continuously at room temperature to fully mix the two. Use DF-101S collector type constant temperature heating magnetic stirrer to heat to 55°C for reflux reaction for 12 hours to obtain methyl bromide 1-acetate Ester-3-methylimidazole ionic liquid crude product, after cooling, wash the crude product several times with ethyl acetate, distill off the solvent and ethyl acetate under reduced pressure, and dry in vacuo to obtain a white solid, which is the purified ionic liquid intermediate Product 1-Acetoxymethyl-3-methylimidazolium bromide. Dissolve lithium bistri...

Embodiment 2

[0019] 1-methylbenzoate-3-methylimidazolium bistrifluoromethylsulfonimide salt ([CH 2 C 6 h 4 COOCH 3 MIM] NTf 2 )

[0020] in N 2Under protection, use 30ml of acetonitrile as a solvent, add 22.9g (0.1mol) of methyl p-bromomethylbenzoate to the reaction vessel, slowly add 7.9mL (0.1mol) of N-methylimidazole dropwise to the reaction vessel, first Stir continuously at room temperature to fully mix the two, use DF-101S collector type constant temperature heating magnetic stirrer to heat to 55 ° C for reflux reaction for 12 hours, wait for the reaction to be cooled, wash with ethyl acetate several times, and distill under reduced pressure to remove the solvent and Ethyl acetate was dried in vacuo to obtain a white solid, namely the purified ionic liquid intermediate 1-p-methylbenzoate-3-methylimidazolium bromide. Dissolve the lithium bistrifluoromethanesulfonimide and the purified 1-p-methylbenzoic acid methyl-3-methylimidazolium bromide separately with an appropriate amount...

Embodiment 3

[0033] Weigh 15 mg of 1-methyl-acetate-3-methylimidazole bistrifluoromethanesulfonimide salt and apply it on 100 mg of acid-washed 102 white support, and use passive sampling to enrich the volatile and semi- volatile organic compounds.

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Abstract

The invention discloses two selective ionic liquids and a synthesis method thereof, and belongs to the technical field of ionic liquids. The ionic liquids are a 1-methyl acetate-3-methylimidazole bistrifluoromethanesulfonimide salt and a 1-methyl p-toluate-3-methylimidazole bistrifluoromethanesulfonimide salt. The synthesis method comprises the preparation process: under the protection of N2, adding N-methylimidazole and halogenated hydrocarbon into a reaction vessel according to the molar ratio of 1:1-1.5, adding acetonitrile, stirring uniformly at the room temperature, heating to 55 DEG C, refluxing for 12 h, allowing the system to be divided into an upper phase and a lower phase, after cooling, separating to obtain a lower-layer halogen ionic liquid crude product, washing with ethyl acetate, and drying to obtain a purified ionic liquid intermediate; and adding an anionic salt aqueous solution into the ionic liquid intermediate, stirring for 12 h at the room temperature, after finishing a reaction, allowing the solution to be divided into two layers, discarding the upper-layer aqueous phase, washing with distilled water for a plurality of times until the water layer is neutral, and drying to obtain the product. The preparation process is simple and can be manipulated, the whole reaction process is stable, and thus the preparation method can be considered to be applied in industrialized production.

Description

technical field [0001] The present invention relates to two kinds of synthetic methods of novel imidazole-based ionic liquids based on the selectivity of SVOCs in indoor air, in particular to using N-methylimidazole and halogenated hydrocarbon derivatives with specific functional groups as raw materials to synthesize two kinds of 1, 3-disubstituted imidazolium cation and NTf 2 The novel selective ionic liquid which is an anion is intended to be used for the extraction and enrichment of trace pollutants SVOCs in indoor air and the subsequent instrument-linked determination, and belongs to the technical field of ionic liquids. Background technique [0002] Semi-volatile organic pollutants (SVOCs) refer to organic compounds with a boiling point in the range of 240-400 °C. Although the saturated vapor pressure is low, they have strong adsorption properties. Compared with VOCs, SVOCs are more stable in the environment and are not easy to degrade , can exist in the indoor environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/56C07C311/48C07C303/40G01N1/40
CPCC07D233/56G01N1/4044
Inventor 刘潮清王小逸任海荣陈慧敏
Owner BEIJING UNIV OF TECH
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