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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

Active Publication Date: 2019-04-16
杭州九清科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, azeotropic distillation has its own limitations: in terms of energy consumption, the cost is higher than other methods; in terms of equipment investment, it is often larger than other methods, and the product purity is difficult to guarantee
However, the cost of using ionic liquid is high, and a third organic component is introduced, which makes it difficult to recycle the separated triethylamine and isopropanol in the original process
Extractive distillation In the process of industrial production, it is very difficult to select the extractant. It is necessary to use a conventional extractant and ensure an efficient extraction effect; there are still problems to be solved in terms of energy consumption in the process of separation and reuse of the extractant

Method used

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  • Separation method of difficult separation system containing triethylamine
  • Separation method of difficult separation system containing triethylamine

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Experimental program
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Effect test

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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Abstract

The invention discloses a separation method of a triethylamine-containing system difficult to separate. According to the technical scheme, water, alkaline water or brine is adopted as an extractant, acontinuous or intermittent extraction process is adopted to separate triethylamine and a second component without introduction of new impurities, and the water can be recycled with no production of wastewater; then rectification is performed so as to remove residual triethylamine and second component in a raffinate phase, the relative volatility of the triethylamine and second component in the raffinate phase can be changed greatly, and high-content triethylamine and second component can be recovered efficiently from the raffinate phase containing low content of triethylamine and second component; and the operation in the distillation step can be completed by using a simple rectification unit, the evaporation amount is limited, and the energy consumption is controllable; therefore, extraction and rectification are coupled in the process so as to realize separation of triethylamine and the second component, and since water, alkaline water or brine is adopted as the extractant in the whole process with no introduction of other impurities, and addition of the alkali or salts is beneficial to separation of the triethylamine and the second component, the process has the advantages of simple equipment, investment cost saving, simple operation and operation cost saving, and the advantages are innovation points of the process.

Description

technical field [0001] The invention relates to the fields of pharmaceutical solvent recovery and industrial wastewater or waste liquid treatment, in particular to a separation method for a difficult-to-separate system containing triethylamine. Background technique [0002] Triethylamine (molecular formula: N(CH 2 CH 3 ) 3 ) is an amine organic compound, a colorless to pale yellow transparent liquid with a strong ammonia odor, slightly fumes in the air, slightly soluble in water, soluble in ethanol and ether, and its aqueous solution is alkaline It is an organic base, catalyst, solvent and raw material commonly used in drug synthesis. [0003] Triethylamine and isopropanol are widely used in petrochemical, pharmaceutical and chemical fields. Especially triethylamine, because its price is high, consider from production cost and reduce pollution, triethylamine recycling has higher practical significance. The recovery rate and recovery quality of triethylamine directly aff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/86C07C211/05C07C29/86C07C29/80C07C31/12
CPCC07C29/80C07C29/86C07C209/86C07C211/05C07C31/12
Inventor 彭明兴
Owner 杭州九清科技有限公司
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