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Method for synthesizing ionic liquid

A technology of ionic liquid and decompression separation, which is applied in organic chemistry and other fields, can solve the problems of increasing energy consumption and reducing efficiency, and achieves the effects of high production efficiency, low production cost and strong operability

Inactive Publication Date: 2010-05-19
CHTC HELON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The initial reaction rate of ionic liquid synthesis is high. As the yield increases, the ionic liquid gradually becomes a solvent, the raw material becomes a solute, and the reaction rate drops sharply. Generally, prolonging the reaction time increases the yield of the ionic liquid, and then purifies the raw material. Separation, which greatly increases energy consumption and reduces efficiency

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  • Method for synthesizing ionic liquid
  • Method for synthesizing ionic liquid

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Experimental program
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Embodiment 1

[0018] Take 2.05kg of n-chlorobutane and 1.63kg of N-methylimidazole (the molar ratio of n-chlorobutane to N-methylimidazole is 1.11:1), put them into an 8L glass reactor, and the temperature of the jacket of the glass reactor is The control is 72±1°C, the temperature of the condenser above the glass reactor is controlled at ≤20°C, the stirring rate is 260-280r / min, and the reaction is 10 hours to obtain a light yellow liquid reaction product; the liquid reaction product is introduced into the decompression separation tower, Separation and recovery of unreacted chlorobutane 0.48kg; then add the light yellow liquid after removing chlorobutane and extractant ethyl acetate 4.2kg in the centrifugal extractor to realize the separation of ethyl acetate phase and ionic liquid phase Separated to obtain 2.98kg of pure ionic liquid (85% conversion rate); the ethyl acetate phase enters the decompression separation tower to realize the separation of ethyl acetate and N-methylimidazole, and...

Embodiment 2

[0020] Take 3.00kg of chlorobutane and 2.60kg of N-methylimidazole (the molar ratio of chlorobutane to N-methylimidazole is 1.02:1), add it to an 8L glass reactor, and the temperature of the glass reactor jacket is Control 80±1°C, control the temperature of the condenser above the glass reactor to ≤20°C, stir at a rate of 300-320r / min, react for 8 hours, and obtain a light yellow liquid reaction product; import the liquid reaction product into a decompression separation tower, and separate Recover 0.30 kg of unreacted chlorobutane; then add the light yellow liquid after removing chlorobutane and 5.0 kg of ethyl acetate into the centrifugal extractor to realize the separation of ethyl acetate phase and ionic liquid phase , obtain pure ionic liquid 4.87kg (transformation rate is 87%); Ethyl acetate phase enters decompression separation column and realizes the separation of ethyl acetate and N-methylimidazole, reclaims and obtains N-methylimidazole 0.21kg. The separated and recov...

Embodiment 3

[0022] Take 3.06kg of n-chlorobutane and 2.26kg of N-methylimidazole (the molar ratio of n-chlorobutane to N-methylimidazole is 1.2:1), add it to an 8L glass reactor, and the temperature of the jacket of the glass reactor is Control 85±1°C, control the temperature of the condenser above the glass reactor ≤20°C, stir at 280-300r / min, react for 6 hours, and obtain a light yellow liquid reaction product; import the liquid reaction product into a decompression separation tower, and separate Recover 0.52kg of unreacted n-chlorobutane; add the light yellow liquid after removing n-chlorobutane and 5.2kg of extractant ethyl acetate into the centrifugal extractor to realize the separation of ethyl acetate phase and ionic liquid phase , obtain pure ionic liquid 4.73kg (conversion rate is 89%); Ethyl acetate phase enters decompression separation column and realizes the separation of ethyl acetate and N-methylimidazole, reclaims and obtains N-methylimidazole 0.18kg. The separated and reco...

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Abstract

The invention discloses a method for synthesizing ionic liquid, comprising the following process steps of: (1) synthesis step: mixing n-chlorobutane and N-methylimidazole according to a mol ratio of 1:(1-1.2):1, reacting for 4-10 hours in a reflux stirring state with the reaction temperature of 70-90 DEG C to obtain a reaction product; and (2) extraction and separation steps: adding an extracting agent of ethyl acetate in the obtained reaction product, and separating an ethyl acetate phase from an ionic liquid phrase by extraction to obtain the ionic liquid. The invention has simple process, strong operability, high production efficiency and over 85 percent of conversion rate of the ionic liquid, fully utilizes raw materials, reduces the production cost and improves the purity of the ionic liquid.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis and preparation method of ionic liquid 1-butyl-3-methylimidazolium chloride. Background technique [0002] Ionic liquid is an emerging solvent and reaction medium that has attracted much attention in the 21st century. Since ionic liquids have low vapor pressure, are non-volatile, and are easy to recycle, replacing volatile organic solvents with ionic liquids has potentially huge economic value and extensive humanistic connotations, both in terms of reducing production costs and being environmentally friendly. . As a green solvent, ionic liquids are widely used in the fields of electrochemistry, organic synthesis, catalysis and separation, and are also good solvents for many polymer polymerization reactions and processing. At present, the transition of ionic liquids from the laboratory to industrial applications is not mainly a matter of technical feasibility, but a...

Claims

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Application Information

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IPC IPC(8): C07D233/58
Inventor 田素峰刘建华马君志姜明亮吴亚红
Owner CHTC HELON