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Process for recovering dimethyl formyl amine from waste water using ion liquid extracting process

A technology of dimethylformamide and ionic liquid, which is applied in extraction water/sewage treatment, carboxylic acid amide separation/purification, organic chemistry, etc., can solve the problems of organic solvent loss, low recovery rate, secondary pollution, etc. Achieve the effects of reduced loss, no secondary environmental pollution, and short equilibrium time

Inactive Publication Date: 2007-07-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome defects such as high energy consumption, low recovery rate, organic solvent loss, and secondary pollution in the prior art and provide a method for recovering dimethylformamide from waste water by using an ionic liquid extraction method

Method used

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  • Process for recovering dimethyl formyl amine from waste water using ion liquid extracting process
  • Process for recovering dimethyl formyl amine from waste water using ion liquid extracting process
  • Process for recovering dimethyl formyl amine from waste water using ion liquid extracting process

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: the synthesis of hydrophobic ionic liquid

[0026] Two-step method for synthesizing ionic liquids, first synthesizing 1-methyl-3-propyl methyl ether imidazolium ions, respectively redistilling methyl imidazole and 3-chloropropyl methyl ether before the reaction, and then making the molar ratio 1: Mix the ratio of 1 in a three-necked flask, stir well, heat and reflux in a water bath at 80°C for 24 hours under the protection of nitrogen, wash with ether after cooling to remove unreacted methylimidazole and 3-chloropropyl methyl ether, at 70°C Rotary evaporation 1h obtains 1-methyl-3-propyl methyl ether imidazolium ion; KPF 6 Mix it with the newly synthesized 1-methyl-3-propyl methyl ether imidazolium ion in a molar ratio of 1:1, then carry out the metathesis reaction in a water bath at 80°C for 12 hours, wash with deionized water and dry with anhydrous magnesium sulfate. The impurity was removed by rotary evaporation at 80°C for 10 h, and the desired ionic ...

Embodiment 2

[0027] Example 2: Effect of time on extraction balance

[0028] Using the ionic liquid prepared in Example 1 to extract DMF in the DMF aqueous solution, the specific process is as follows. Accurately measure the DMF aqueous solution that concentration is 8wt%, 30wt%, 50wt%, 70wt% and each 100ml of the ionic liquid made by embodiment 1, the ratio of both by volume 1: 1 or 1: 5, simultaneously once Add it into a mixing tank with stirring (equivalent to single-stage extraction), turn on the stirring to fully mix the two phases, and control the temperature at 20-30°C. Stir for 1, 3, 5, 7, 10, 20, and 30 minutes respectively, then stop stirring, pour into a graduated cylinder, and let stand to separate the phases. After the interface between the two phases is clear, measure the volumes of the aqueous phase and the ionic liquid phase, take the upper aqueous phase with a pipette, and analyze the concentration of DMF contained therein by spectrophotometry. According to the mass bala...

Embodiment 3

[0030] Accurately measure concentration is the DMF aqueous solution of 8wt% and each 100ml of the ionic liquid that is made by embodiment 1, the ratio that both are 1: 1 is added in the mixing tank with agitation (equivalent to single Grade extraction), prepare 3 parts of such extraction systems and mark them as A, B, and C respectively. Slowly add 10wt% H in extraction system B 2 SO 4 , the control pH is 1.0. Add 2 g of NaCl solid to the extraction system C. Start stirring for each extraction system to fully mix the two phases, and control the temperature at 20-30°C. After stirring for 20 minutes, stop stirring, pour into a graduated cylinder, and let stand to separate phases. After the interface between the two phases is clear, measure the volumes of the aqueous phase and the ionic liquid phase, and use a pipette to take the light phase aqueous phase and analyze the concentration of DMF contained therein by spectrophotometry. According to the mass balance of DMF in the ...

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Abstract

This invention relates to a method of using hydrophobicity ionic liquid as extractant to recycle dimethylformamide (DMF) in waste water. This ionic liquid can mix intensively with low density DMF(1-10wt%) at arbitrarily volume ratio'make DMF enriching in ionic liquid phase from water; And the extraction phase ion liquid through reduction vaporization to steam out the DMF. The ion liquid is recycling. The extraction method of distribution ratio is greater than 2, when the two-phase volume ratio of 1:1, an extraction rate of more than 60%, also can use multi-cascade extraction to enhance the extraction rate. Ionic liquids difficult volatile, stable, the extraction process will basically wear and tear. In addition, the method is simple, non-emulsifying through extraction, stillness stratified fast, extraction process rapidly and significantly superior to the traditional method of solvent recover.

Description

technical field [0001] The invention relates to the fields of liquid-liquid extraction and solvent recovery, in particular to a method for recovering dimethylformamide from waste water by using an ionic liquid extraction method. technical background [0002] N, N-dimethylformamide referred to as DMF, is an excellent industrial solvent and organic synthetic material, widely used in a variety of industries, including: 1) polyacrylonitrile fiber spinning solvent; 2) in petroleum As a gas absorbent in chemical industry; 3) as a solvent in the production of artificial leather. These application processes correspondingly produce a large amount of wastewater containing DMF. If the DMF waste liquid is directly discharged into the external environment, it will not only cause economic losses, but also cause serious environmental pollution. How to economically and effectively recover the DMF and treat the accompanying Waste water is very important for improving the overall economic an...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C233/03C02F1/26
Inventor 杨明德吴玉龙党杰胡湖生陈镇杨桂成
Owner TSINGHUA UNIV
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