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Multi-sulfonic-acid-group acidic functionalized ionic liquid and preparation method thereof

A technology of polysulfonic acid and ionic liquid, which is applied in the preparation of sulfonic acid, sulfonate, and peroxy compound, etc., can solve problems such as single structure

Active Publication Date: 2016-07-06
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] One of the purposes of the present invention is to provide a novel polysulfonic acid-based functionalized ionic liquid and a preparation method thereof in order to overcome the relatively single structure of the current sulfonic acid-type ionic liquid. This type of ionic liquid has good surface activity; The preparation method has the characteristics of simple operation, high product yield, and easy industrial implementation.

Method used

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  • Multi-sulfonic-acid-group acidic functionalized ionic liquid and preparation method thereof
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  • Multi-sulfonic-acid-group acidic functionalized ionic liquid and preparation method thereof

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preparation example Construction

[0059] Combine below figure 1 , describe the preparation method of above-mentioned ionic liquid in detail, specifically comprise the following steps:

[0060] Ionic liquid (1), ionic liquid [N 2 (SO 3 h) 2 ]2HSO 4 The synthesis of includes the following steps:

[0061] Step S101: Add tetraethylenediamine and 1,4-butane sultone or propane sultone sequentially into a reaction flask equipped with mechanical stirring, and stir at room temperature for more than 4 hours until the system changes from a liquid phase to a solid phase. phase, the crude product was fully washed with ethyl acetate and then suction filtered, and the filter cake was vacuum-dried at 75-85°C for more than 8 hours to obtain the intermediate amphoteric salt, tetramethylethylenediamine and 1,4-butanesulfone The molar ratio of ester or propane sultone is 1:2.05~2.50;

[0062] Step S102: dissolving the intermediate amphoteric salt obtained in the above step S101 in deionized water and placing it in an ice-wate...

Embodiment 1

[0081] Ionic liquid [N 2 (SO 3 h) 2 ]2HSO 4 Synthesis

[0082] Step S101: Add 1 mol of tetraethylenediamine and 2.05 mol of 1,4-butane sultone in sequence to a reaction flask equipped with mechanical stirring, and stir at room temperature for 4 hours until the system changes from a liquid phase to a solid phase; the crude The product was fully washed with ethyl acetate and then suction-filtered, and the filter cake was vacuum-dried at 75°C for 8 hours to obtain the intermediate amphoteric salt with a yield of ≥95%;

[0083] Step S102: Dissolve the amphoteric salt in deionized water and place it in an ice-water bath, slowly add sulfuric acid dropwise, the molar ratio of sulfuric acid to the intermediate amphoteric salt is 1:2, transfer to an oil bath after adding, and heat up to 80°C After reacting for 8 hours, the target ionic liquid was obtained. The appearance of the ionic liquid was a viscous liquid, and the yield was ≥96%.

Embodiment 2

[0085] Ionic liquid [N 2 (SO 3 h) 2 ]2HSO 4 Most of the synthesis is the same as in Example 1;

[0086] The difference from Example 101 is:

[0087] S101: Add 1 mol of tetraethylenediamine and 2.15 mol of 1,4-butane sultone in sequence, stir at room temperature for 5 hours, and vacuum-dry the filter cake at 80°C for 10 hours;

[0088] S102: Raise the temperature to 83°C and react for 10 hours.

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Abstract

The invention provides multi-sulfonic-acid-group acidic functionalized ionic liquid, a preparation method thereof and a method of utilizing the ionic liquid to prepare organic peroxide.Each cation of the ionic liquid has two or three alkyl sulfonic acid side chains with 3 or 3 carbon atoms, a matched anion is hydrogen sulfate radical, and the ionic liquid is of an open straight chain structure.The preparation method of the organic peroxide includes: sequentially adding the ionic liquid and hydrogen peroxide into a reaction kettle, fully stirring at room temperature to homogeneous phase, adding cyclohexanone or methyl ethyl ketone, and finishing after reaction at room temperature for 3-8 h; separating a product out of a reaction system obtained through suction filtering or phase separation, sequentially performing water washing or saline washing to obtain water-phase liquid and a crude product, and drying the crude product under vacuum condition to obtain the organic peroxide.The preparation method has the advantages of mild reaction condition, high yield, high product purity and easiness in product separation.

Description

technical field [0001] The invention relates to chemical products and preparation technology thereof, in particular to a polysulfonic Brönsted acidic functionalized ionic liquid and a preparation method thereof. This type of ionic liquid can be used as a catalytic system to prepare organic peroxides such as cyclohexanone peroxide, methyl ethyl ketone peroxide, benzoyl peroxide, and acetylacetone peroxide. Organic peroxides such as cyclohexanone peroxide and methyl ethyl ketone peroxide are used as room temperature curing agents for unsaturated polyester resins, and are widely used in the production fields of polyester buttons, artificial agate, glass fiber reinforced plastic products, and artificial marble. Background technique [0002] The unsaturated polyester resin room temperature curing agent refers to the initiator added when the unsaturated polyester resin is cured at room temperature, which is usually an organic peroxide, such as cyclohexanone peroxide, methyl ethyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/02C07C309/14B01J31/02C07C407/00C07C409/18C07C409/16C07C409/34
CPCB01J31/0279B01J2231/70C07C303/02C07C303/32C07C309/14C07C407/00C07C409/18C07C409/16C07C409/34
Inventor 李心忠李政周沂
Owner MINJIANG UNIV
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