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Tetramethyl hexaalkyl triethylene tetraammonium salt, and preparation method and application thereof

A technology of tetramethylhexaalkyltriethylene and tetraammonium salt, which is applied in the field of fine chemical industry and solvent extraction, can solve the problems of small extraction saturation capacity, long and short phase separation time, and achieve easy recovery and separation The effect of short phase time and no corrosion of equipment

Active Publication Date: 2016-04-20
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at a series of shortcomings such as few types of quaternary ammonium salt extractants available in existing hydrometallurgy, small extraction saturation capacity, and long phase separation time, the first purpose of the present invention is to provide a quaternary ammonium salt extractant with a new structure. Ammonium salt extractant tetramethylhexaalkyltriethylene tetraammonium salt; the quaternary ammonium salt compound has the property of ionic liquid, and as a metal anion extractant, it has the characteristics of short phase separation time and large capacity, and it does not corrode equipment and has low toxicity , to meet the industrial application requirements of extractants

Method used

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  • Tetramethyl hexaalkyl triethylene tetraammonium salt, and preparation method and application thereof
  • Tetramethyl hexaalkyl triethylene tetraammonium salt, and preparation method and application thereof
  • Tetramethyl hexaalkyl triethylene tetraammonium salt, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Add 0.5 mol of anhydrous sodium carbonate, 50 mL of absolute ethanol and 0.1 mol of triethylenetetramine into a three-necked bottle with a capacity of 500 mL, put the three-necked bottle on the stirrer, start the stirrer at the same time, and heat the water bath to 75 °C, slowly dropwise add 0.9 mol of n-bromohexane and 50 mL of anhydrous ethanol mixture therein, and the dropwise addition is completed within 4 hours. After the dropwise addition was completed and reacted for 24 hours, 0.9 mol of sodium hydroxide solid was added thereto. After reacting for 3 hours, the stirring was stopped, cooled, and filtered. The organic phase obtained by filtration was subjected to vacuum distillation, and the obtained substance was separated into two layers. The upper layer is light red liquid, and the lower layer is brown-black opaque liquid. Add 200mL of 10% sodium carbonate solution to the distilled product to wash the product, wash three times, and after standing, separate the o...

Embodiment 2

[0040] Add 0.5 mol of anhydrous potassium carbonate, 50 mL of absolute ethanol and 0.1 mol of triethylenetetramine into a three-necked bottle with a capacity of 500 mL, put the three-necked bottle on the stirrer, start the stirrer at the same time, and heat the oil bath to At 120°C, slowly add 0.9 mol of n-octane bromide and 50 mL of absolute ethanol dropwise therein, and the dropwise addition is completed within 4 hours. After the dropwise addition was completed and reacted for 10 h, 0.9 mol of sodium hydroxide solid was added thereto, and after reacting for 4 h, the stirring was stopped, cooled, and filtered. The organic phase obtained by filtration was subjected to vacuum distillation, and the obtained substance was separated into two layers. The upper layer is light red liquid, and the lower layer is brown-black opaque liquid. Add 200 mL of potassium carbonate solution with a mass fraction of 10% to the distilled product to wash the product three times, and after standing...

Embodiment 3

[0043] Add 0.5 mol of anhydrous potassium carbonate, 50 mL of absolute ethanol and 0.1 mol of triethylenetetramine into a three-necked bottle with a capacity of 500 mL, put the three-necked bottle on the stirrer, start the stirrer at the same time, and heat the oil bath to At 100°C, slowly add 0.9 mol of n-octane bromide and 50 mL of absolute ethanol dropwise therein, and the dropwise addition is completed within 4 hours. After the dropwise addition was completed and reacted for 14 hours, 0.9 mol of sodium hydroxide solid was added thereto, and after reacting for 6 hours, the stirring was stopped, cooled, and filtered. The organic phase obtained by filtration was subjected to vacuum distillation, and the obtained substance was separated into two layers. The upper layer is light red liquid, and the lower layer is brown-black opaque liquid. Add 200 mL of potassium carbonate solution with a mass fraction of 10% to the distilled product to wash the product three times, and after ...

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Abstract

The invention discloses a tetramethyl hexaalkyl triethylene tetraammonium salt, and a preparation method and application thereof. The preparation method comprises the following steps: slowly adding monobromoalkane into an ethanol solution containing sodium carbonate and / or potassium carbonate and triethylene tetraammonium drop by drop so as to obtain hexaalkyl triethylene tetra-tert-ammonium; and reacting hexaalkyl triethylene tetra-tert-ammonium and a methanol solution of dimethyl carbonate at high temperature and high pressure so as to obtain the tetramethyl hexaalkyl triethylene tetraammonium salt. A series of tetramethyl hexaalkyl triethylene tetraammonium salts with ionic liquid properties are obtained by subjecting the tetramethyl hexaalkyl triethylene tetraammonium salt and compounds including NO<3->, SO4<2->, Cl<-> and the like to an ion exchange reaction. The series of quaternary ammonium salts are applied to selective extraction and separation of anions like tungsten, molybdenum and vanadium in aqueous solutions, realizes separation of the anions like tungsten, molybdenum and vanadium from impurity ions like sulfur and phosphorus and can be extensively applied to fields like wet metallurgy and sewage treatment.

Description

technical field [0001] The invention relates to a novel tetramethylhexaalkyltriethylene tetraammonium salt extractant, a preparation method thereof and an application in extracting metal ions in aqueous solution, belonging to the technical fields of fine chemical industry and solvent extraction. Background technique [0002] With the increasing development of cemented carbide, electronics, national defense and other industries, people's demand for tungsten, molybdenum and vanadium is increasing day by day. The current tungsten, molybdenum and vanadium are mainly smelted and extracted from ores and extracted and recovered from waste solutions containing tungsten, molybdenum and vanadium. With the reduction of ore resources and the improvement of environmental protection requirements, efficient extraction and separation of tungsten, molybdenum and vanadium has become the current main process. The solvent extraction method for extracting and separating tungsten, molybdenum and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/12C07C211/63C22B3/26C22B34/34C22B34/36C22B34/22
CPCC07C209/12C07C211/63C22B34/22C22B34/34C22B34/36C22B3/288Y02P10/20
Inventor 曹佐英邓海碧肖连生张贵清关文娟李青刚曾理
Owner CENT SOUTH UNIV