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Preparation method of ionic liquid monomer with homopolymer having UCST property

An ionic liquid, homopolymer technology, applied in organic chemistry and other directions, can solve problems such as inconvenience

Inactive Publication Date: 2020-04-17
WEIFANG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, it has not been found in the prior art that homopolymers prepared from ionic liquid monomers have UCST properties
[0006] In summary, there are obviously inconveniences and defects in the actual use of the existing technology, so it is necessary to improve

Method used

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  • Preparation method of ionic liquid monomer with homopolymer having UCST property
  • Preparation method of ionic liquid monomer with homopolymer having UCST property
  • Preparation method of ionic liquid monomer with homopolymer having UCST property

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preparation example Construction

[0031] The invention provides a method for preparing an ionic liquid monomer whose homopolymer has UCST properties, comprising the steps of:

[0032] step one

[0033] At room temperature, dissolve hexylimidazole in ethyl acetate and stir for 15-30 minutes; then slowly add benzyl chloride methyl styrene for quaternization reaction to obtain intermediate product 1;

[0034] In the present invention, the reaction time of the quaternization reaction is 8-12 hours. The ethyl acetate and benzyl chloride methyl styrene used in the present invention are analytically pure.

[0035] The mass ratio of hexylimidazole to ethyl acetate is 1:1; the molar ratio of hexylimidazole to benzyl chloride methyl styrene is 1:0.89~0.99.

[0036] The method of slowly adding benzyl chloride methyl styrene is to add drop by drop or add in 10-20 times; this operation can always keep the concentration of hexylimidazole greater than that of benzyl chloride methyl styrene, increase the reaction rate and r...

Embodiment 1

[0055] Weigh 30.45g of hexylimidazole, dissolve it in 35.00mL of ethyl acetate and stir for 1h; then add 30.21g of benzylchloromethylstyrene dropwise into the above reaction solution, and react at room temperature for 8h to obtain intermediate product 1.

[0056] Pour the above-mentioned intermediate product 1 into a container, then add 50.00 mL of deionized water, stir for 15 minutes, then let it stand for stratification, continue to add the same volume of deionized water, repeat the operation three times, and collect the lower layer of intermediate product 2.

[0057] Add 200mL of deionized water and accurately weighed 43.95g of sodium fluoroborate into the container, and stir for 30 minutes until the sodium fluoroborate solid is completely dissolved to obtain a sodium fluoroborate solution; add the above-mentioned intermediate product 2 to the sodium fluoroborate solution dropwise, Stir while adding dropwise, carry out counter ion exchange reaction, the reaction time is 120m...

Embodiment 2

[0061] Weigh 30.45g of hexylimidazole, dissolve it in 35.00mL of ethyl acetate and stir for 1h; then add 28.70g of benzylchloromethylstyrene dropwise into the above reaction solution, and react at room temperature for 8h to obtain intermediate product 1.

[0062] Pour the above-mentioned intermediate product 1 into a container, then add 50.00 mL of deionized water, stir for 15 minutes, then let it stand for stratification, continue to add the same volume of deionized water, repeat the operation three times, and collect the lower layer of intermediate product 2.

[0063] Add 200mL of deionized water and accurately weighed 43.95g of sodium fluoroborate into the container, and stir for 30 minutes until the sodium fluoroborate solid is completely dissolved to obtain a sodium fluoroborate solution; add the above-mentioned intermediate product 2 to the sodium fluoroborate solution dropwise, Stir while adding dropwise, carry out counter ion exchange reaction, the reaction time is 120m...

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Abstract

The invention belongs to the technical field of ionic liquid preparation, and provides a preparation method of an ionic liquid monomer with a homopolymer having UCST property. The method comprises thefollowing steps: dissolving hexylimidazole in ethyl acetate, slowly adding benzyl chloromethyl styrene, carrying out a quaternization reaction, adding deionized water, extracting, washing, and collecting the lower-layer substance; and slowly adding the lower-layer substance into a sodium fluoborate solution, carrying out a counter ion replacement reaction, collecting a white powder solid, washing, and drying to obtain the ionic liquid monomer 1-hexyl-3-(4-vinylbenzyl)imidazole fluoborate. According to the invention, the prepared ionic liquid monomer is high in structural purity, and the homopolymer has typical UCST properties; the preparation process is simple, the reaction conditions are room temperature, the requirements on production equipment are low, and the production cost is saved;and the ethyl acetate and the sodium fluoborate solution in the reaction process can be recycled so as to avoid environmental pollution.

Description

technical field [0001] The invention relates to the technical field of ionic liquid preparation, in particular to a preparation method of an ionic liquid monomer whose homopolymer has UCST properties. Background technique [0002] UCST (upper critical solution temperature) is the abbreviation of the highest critical temperature, which means that a temperature-sensitive material will change from a dissolved (or swollen) state to an insoluble (or shrinkage) state when the temperature is lower than a certain temperature or temperature range. nature. UCST properties usually exist in homopolymers and copolymers with specific structures, which are related to the properties of the solvent. [0003] Ionic liquids are a class of organic salts composed of organic cations, inorganic or organic anions, and the organic salts are liquid when the boiling point is lower than 100°C. Organic cations are mainly composed of imidazole quaternary ammonium salts, pyridine quaternary ammonium sal...

Claims

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Application Information

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IPC IPC(8): C07D233/58
CPCC07D233/58
Inventor 杨永启刘光耀申亮亮邢仁卫宋继梅闫友军张军肖珍
Owner WEIFANG UNIV OF SCI & TECH
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