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Preparation method of epsilon-caprolactam-tetraalkyl ammonium halide-SO2-H2O hydrido complex

A technology of -SO2-H2O and tetraalkylammonium halides, which is applied in chemical instruments and methods, separation methods, and separation of dispersed particles, can solve the problems of high viscosity, high regeneration energy consumption, and high cost, and achieve high yield, The preparation method is simple and the effect of efficient absorption

Inactive Publication Date: 2013-10-09
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Many experts at home and abroad have used guanidine and imidazole ionic liquids or ionic liquid membranes as absorbents to remove acid gases (CO 2 , SO 2 、H 2 S, etc.), achieved ideal results, but most ionic liquids have limitations such as high production costs and high viscosity, and have not considered their degradability in the environment
The Chinese patents whose publication numbers are CN101601961A and CN201010269494.5 respectively disclose the use of caprolactam-tetraalkylammonium halide ionic liquids to absorb SO 2 and H 2 The method of S gas, its absorption mode is physical absorption, ionic liquid and SO 2 Regeneration energy consumption is high, and the regenerated SO 2 The production of sulfuric acid by catalysis is low and the cost is high, so there are certain difficulties in the industrial application of this process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Weigh 0.421 mol of ε-caprolactam and 0.165 mol of tetrapropylammonium bromide into a round-bottomed flask equipped with a rotor, stir and heat in a constant temperature water bath at 75°C for 2 hours to obtain ε-caprolactam-tetrapropyl bromide ammonium chloride ionic liquid.

[0022] b. Dissolve the ε-caprolactam-tetrapropylammonium bromide ionic liquid obtained in step a with distilled water at a molar concentration of 2 mol / L, and mix uniformly to obtain an aqueous solution of ε-caprolactam-tetrapropylammonium bromide ionic liquid.

[0023] c. Mix the ε-caprolactam-tetrapropylammonium bromide ionic liquid aqueous solution obtained in step b with 1.00mol of SO 2 Gas reaction for 1h, phase separation, the lower layer is ε-caprolactam-tetrapropylammonium bromide-SO 2 -H 2 O hydrogenation complex, productive rate 95% (mass ratio).

Embodiment 2

[0025] a. Weigh 0.390 mol of ε-caprolactam and 0.223 mol of tetraethylammonium bromide into a round bottom flask equipped with a rotor, stir and heat in a constant temperature water bath at 75°C for 2 hours to obtain ε-caprolactam-tetraethyl bromide ammonium chloride ionic liquid.

[0026] b. Dissolve the ε-caprolactam-tetraethylammonium bromide ionic liquid obtained in step a with distilled water at a molar concentration of 1 mol / L, and mix uniformly to obtain an aqueous solution of ε-caprolactam-tetraethylammonium bromide ionic liquid.

[0027] c. the ε-caprolactam-tetraethylammonium bromide ionic liquid aqueous solution obtained in step b and 0.50mol of SO 2 Reaction for 1h, phase separation, the lower layer is ε-caprolactam-tetraethylammonium bromide-SO 2 -H 2 O hydrogenation complex, yield 93% (mass ratio).

Embodiment 3

[0029] a. Weigh 0.318mol of ε-caprolactam and 0.373mol of tetramethylammonium bromide into a round-bottomed flask equipped with a rotor, stir and heat in a constant temperature water bath at 75°C for 2 hours to obtain ε-caprolactam-tetramethylbromide ammonium chloride ionic liquid.

[0030] b. Dissolve the ε-caprolactam-tetramethylammonium bromide ionic liquid obtained in step a with distilled water at a molar concentration of 0.1 mol / L, and mix uniformly to obtain an aqueous solution of ε-caprolactam-tetramethylammonium bromide ionic liquid.

[0031] c. the ε-caprolactam-tetramethylammonium bromide ionic liquid aqueous solution that step b obtains in the SO with 0.12mol 2 Gas reaction for 1h, phase separation, the lower layer is ε-caprolactam-tetramethylammonium bromide-SO 2 -H 2 O hydrogenation complex, productive rate 90% (mass ratio).

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Abstract

The invention relates to a preparation method of an epsilon-caprolactam-tetraalkyl ammonium halide-SO2-H2O hydrido complex. The method comprises the following steps of: weighing epsilon-caprolactam and tetraalkyl ammonium halide in a certain molar weight according to proportion; stirring for 2 hours at 75 DEG C to obtain an epsilon-caprolactam-tetraalkyl ammonium halide ionic liquid; preparing the liquid to an aqueous liquor in certain concentration; and reacting with SO2 gas and layering phase, wherein the lower layer is the epsilon-caprolactam-tetraalkyl ammonium halide-SO2-H2O hydrido complex. The epsilon-caprolactam-tetraalkyl ammonium halide ionic liquid aqueous liquor and SO2 form the hydrido complex through hydrogen bonds. The hydrido complex provided by the invention can efficiently absorb hydrogen sulfide exhaust gas, so that sulphur single substance can be efficiently recovered with low cost, and SO2 exhaust gas can be absorbed to be regenerated.

Description

technical field [0001] The present invention relates to a kind of by epsilon-caprolactam-tetraalkylammonium halide ionic liquid aqueous solution and SO 2 Preparation of ε-caprolactam-tetraalkylammonium halide-SO 2 -H 2 O Hydrogenation complex method. Background technique [0002] In recent years, acid gas removal technology is a key technology related to energy efficient utilization, clean production and circular economy. It has great social and economic significance and has become a global research topic. At present, the removal methods of acid gas mainly include chemical absorption method, physical adsorption method, low temperature separation method, membrane separation method, etc. Among them, the method of chemical absorption method, especially the method of using organic amine solution as absorbent, is the commonly used method at present, and there are also existing methods. A more mature process. However, the volatility of organic amines makes the traditional orga...

Claims

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Application Information

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IPC IPC(8): B01D53/78B01D53/52
Inventor 段二红宋玉杨昆王坤坤张鹏孟薇郭斌
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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