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A process for regenerating ionic compound

A technology of ionic compounds and chlorides, applied in separation methods, hydrocarbons, hydrocarbons, etc., can solve problems such as low energy efficiency, inability to reuse/recycle, and major equipment expenditures

Inactive Publication Date: 2015-12-23
RELIANCE INDUSTRIES LIMITED
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is difficult to recover and recycle aluminum trichloride
[0014] Disadvantages associated with prior art methods are that the recovered / regenerated catalyst has poor purity and cannot be reused / recycled after a certain limit
Additionally, some methods require special equipment, resulting in significant equipment expenditures
Furthermore, in some prior art methods the conditions used are harsh and thus energy inefficient

Method used

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  • A process for regenerating ionic compound
  • A process for regenerating ionic compound
  • A process for regenerating ionic compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] In this experiment, chloroaluminate-based ionic compounds were prepared, deactivated by repeated use in alkylation reactions, and then the deactivated ionic compounds were regenerated by the disclosed method.

[0072] Step i: Preparation of chloroaluminate ionic compound from 1-butyl-3-methylimidazolium bromide [BMIM]Br

[0073] The apparatus consisted of a 5 L three necked round bottom flask equipped with an overhead stirrer and placed in an ice bath at 0-5 °C. The flask was clamped to provide stability while stirring. Keep the whole assembly under nitrogen atmosphere. Weigh 680 g of [BMIM]Br and carefully fill the flask through the funnel. Weigh 830gAlCl 3 , and slowly added to the flask under constant stirring. AlCl 3 The loading of is completed within 1.5 hours. The mixture was further stirred for 2 hours to properly mix the ingredients. The final catalyst was kept under nitrogen.

[0074] Step ii: Inactivation of the ionic compound prepared in step (i) by r...

Embodiment 2

[0080] Example 2: Recovery of [BMIM]Br from fresh catalyst by neutralization with triethylamine

[0081]In this experiment, the ionic compound prepared in step (i) of Experiment 1 was directly regenerated without deactivation to investigate the efficiency of the disclosed method.

[0082] 10.0 g of fresh catalyst obtained from step (i) of Experiment 1 were charged together with 50 ml of ethyl acetate into a 250 ml round bottom flask equipped with an overhead stirrer maintained at 29°C. 12.6 g of triethylamine were slowly added over a period of 1 hour and stirred for 30 minutes. The resulting mixture was filtered and ethyl acetate was separated. The resulting solid was washed in batches with 200 ml of dichloromethane to extract [BMIM]Br from the solid mixture. The dichloromethane layer thus obtained was distilled off to obtain 4 g of [BMIM]Br salt. The yield obtained was 88%.

Embodiment 3

[0083] Example 3: Regeneration of the Ionic Compound [BMIM]Br Using Sodium Carbonate Using the Disclosed Method

[0084] The method used in this experiment was the same as that described in step (iii) of Experiment 1, except that sodium carbonate solution was used instead of triethylamine.

[0085] 100 g of the deactivated catalyst obtained in step (ii) of Experiment 1 was charged into a 500 ml Erlenmeyer flask. By mixing 133.3gNa 2 CO 3 and 350ml of water to prepare Na 2 CO 3 solution, and set aside. Na will be produced 2 CO 3 The solution was slowly added to the Erlenmeyer flask containing the deactivated catalyst. Once the addition was complete, 100 ml of ethyl acetate was added to the flask and stirred for 1 hour and allowed to stand for 1 hour. The water and ethyl acetate layers were separated, and the aqueous layer was subjected to distillation to obtain a solid mixture. The solid mixture was washed with 75 ml of dichloromethane to extract [BMIM]Br, and the resu...

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Abstract

The present disclosure provides a process for regenerating the deactivated ionic compound. The process involves mixing a deactivated ionic compound with at least one solvent such as ethyl acetate and neutralizing with at least one base such as triethylamine and tert-butyl amine to obtain a precipitate. The obtained precipitate is filtered to obtain a residue which is then washed with a solvent such as dichloromethane to obtain the ionic compound.

Description

technical field [0001] The present disclosure relates to a method for regenerating ionic compounds. In particular, the present disclosure relates to a method for regenerating metal halide-based ionic compounds. Background technique [0002] Ionic compounds are compounds made up of ions (ie, cations and anions). Ionic compounds are suitable as catalysts and as solvents in alkylation reactions, polymerization reactions, dimerization reactions, oligomerization reactions, acetylation reactions, metathesis reactions and copolymerization reactions. [0003] The most common ionic compounds are compounds made from organic-based cations and inorganic or organic anions. Pyridinium and imidazolium are commonly used cations, while anions such as BF4 - 、PF6 - , haloaluminate (such as Al 2 Cl 7 - and Al 2 Br 7 — ), [(CF 3 SO 2 ) 2 N)] - , Alkylsulfonate (RSO 3 - ) and carboxylate (RCO 2 - ). Ionic compounds of catalytic interest are those derived from ammonium halides a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/34
CPCB01J31/0282B01J31/26B01J31/40B01J2231/323C07C2/66C07C2527/125Y02P20/584B01J31/0284C07D213/06C07D233/58C07C15/107Y02P20/52
Inventor 帕凡库玛·阿杜里帕拉苏·维拉·阿帕拉维斯瓦纳·科特马哥什·萨克哈尔卡韦布提·杜克哈德维韦克·普拉巴卡尔·拉吉
Owner RELIANCE INDUSTRIES LIMITED
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