Separation method of difficult separation system containing triethylamine
A separation method and technology of triethylamine, applied in chemical instruments and methods, purification/separation of amino compounds, preparation of organic compounds, etc., can solve the difficulty of recycling triethylamine and isopropanol and the difficulty of selecting extraction agents , product purity is difficult to guarantee and other issues, to achieve the effect of limited evaporation, saving investment costs, and controllable energy consumption
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Embodiment 1
[0038]In this embodiment, water is used as the extractant (containing 0.02% caustic soda), and continuous extraction is used to separate triethylamine and isopropanol. The mass composition of triethylamine-isopropanol mixture (raw material liquid) is triethylamine 45%, isopropanol 50%, water 5%, and raw material liquid is sent into the bottom of continuous rotary disk extraction tower with the speed of 1kg / hour, and extractant water At a rate of 6kg / hour, it is sent to the top of the rotary disk extraction tower, and the operating temperature of the rotary disk extraction tower is 50-60°C. After continuous extraction, the extract phase is obtained at the top of the rotary disk extraction tower, and its content is 97% of triethylamine, 2.5% of water, and 0.5% of isopropanol; the heavy phase at the bottom is the raffinate phase, and its composition is 88% of water, isopropanol 8-10%, triethylamine 2-4%.
Embodiment 2
[0040] In this embodiment, water is used as the extractant (remove the salt or alkali), the extraction temperature is 60° C., and triethylamine and isopropanol are separated by a three-stage batch extraction process. The mass composition is 45% of triethylamine, 50% of isopropanol, 200g of triethylamine-isopropanol mixture (raw material solution) of 5% of water is added in a 1L Erlenmeyer flask, 400g of water is added, fully shaken and mixed, and allowed to stand 30min; separate the upper extract phase, add 400g water for a second extraction, mix well and let stand for 30min; continue to separate the upper extract phase, and repeat the extraction operation again. After three stages of intermittent extraction, the composition of the extraction phase is 96% of triethylamine, 3% of water and 1.0% of isopropanol. The raffinate phases obtained by the three-stage extraction were mixed to obtain a raffinate phase to be treated, which was composed of 88% water, 9% isopropanol and 3% t...
Embodiment 3
[0042] The heavy phase (about 88% of water, 8-10% of isopropanol, 3-4% of triethylamine) obtained by continuous extraction of embodiment 2 can separate triethylamine, isopropanol and triethylamine in water by simple rectification (distillation) distillation propanol. This unit obtains four stocks of materials: a) triethylamine containing a small amount of isopropanol and water (87% of triethylamine, 10% of water, 3% of isopropanol), removed from the triethylamine refining unit; b) containing a small amount of triethylamine , the mixed material of water and isopropanol (triethylamine 15%, water 30%, isopropanol 55%), return the fine (distillation) distillation of this section; c) the mixture of isopropanol and water (isopropanol 89% %, water 11%), sent to isopropanol refining for further processing; d) the residue in the tower kettle, the recovery of extractant water, can be sent to the continuous extraction unit for recycling.
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