Separation method for batch extractive distillation of methanol-propyl formate azeotrope

A technology of propyl formate and extractive rectification, which is used in extractive distillation, purification/separation/stabilization of organic compounds, preparation of carboxylate and other directions, can solve the requirement that ordinary separation methods are difficult to meet the requirements of purification, and there is no information and pollution. environment and other issues, to achieve the effect of low cost, simple and flexible operation, and small equipment investment

Inactive Publication Date: 2015-02-25
UNIV OF JINAN
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Problems solved by technology

Both have broad application prospects in industry, but due to the azeotropic existence of the two, ordinary separation methods are difficult to meet the requirements of refining, thus limiting the application of the two, if not recycled, it will not only pollute the environment, but also c...

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  • Separation method for batch extractive distillation of methanol-propyl formate azeotrope

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Using a batch extraction and rectification device, 500L of methanol-propyl formate azeotrope (51% of methanol and 49% of propyl formate, both in mass fraction) was put into the heating kettle. The extraction agent selected in the experiment was 90wt% ethylene glycol and 10wt%[Emim][BF 4 ] ionic liquid, turn on the heat source of the heating kettle and the cold source of the condenser, after the top of the extractive distillation tower is refluxed for a period of time, and the temperature of the top of the tower is stable, add the extractant, the feed position of the extractant is near the top of the tower, and the extraction agent is controlled The addition rate is 500L / h, total reflux operation, when the top temperature of the extractive distillation tower is 64~65°C, the methanol content in the distillate is ≥99% and the material starts to be discharged, the reflux ratio is 5:1, and the discharge speed is 200L / h. When the temperature at the top of the extractive dis...

Embodiment 2

[0015] Using a batch rectification extraction device, put 500L of methanol-propyl formate azeotropic mixture (50% of methanol and 50% of propyl formate, both in mass fraction) into the heating kettle, and the extraction agent selected in the experiment is 86wt% N-formazol Basepyrrolidone and 14wt% [Emim] [BF 4 ] Ionic liquid, turn on the heat source of the heating kettle and the cold source of the condenser, after the top of the extractive distillation tower is refluxed for a period of time, and the temperature of the top of the tower is stable, add the extractant, the extraction feed position is near the top of the tower, control the addition of the extractant The speed is 800L / h, total reflux operation, when the temperature at the top of the extractive distillation tower is 64~65℃, the propyl formate content in the distillate is ≥99% and the material starts to be discharged, the reflux ratio is 7:1, and the material discharge speed is 300L / h, when the temperature at the top...

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Abstract

The invention discloses a separation method for batch extractive distillation of a methanol-propyl formate azeotrope. The method comprises the following steps: at atmospheric pressure or reduced pressure, by using ethylene glycol or N-methyl pyrrolidinone and an ionic liquid namely 1-ethyl-3-methyl tetrafluoroborate [Emim][BF4] as extracting agents, sequentially extracting qualified methanol and isobutanol from a tower top, pumping the extracting agents into an overhead storage tank when compositions of the extracting agents of a heating kettle meet the requirements, and feeding to perform the next batch of batch extractive distillation separation. The separation method disclosed by the invention has the advantages that a methanol-propyl formate azeotropic system can be damaged by using the ionic liquid and commonly-used solvents as the extracting agents, and methanol and propyl formate products with high purity can be obtained.

Description

technical field [0001] The invention relates to a separation method for intermittent extraction and rectification of methanol-propyl formate azeotrope, which belongs to the special rectification and separation technology of methanol-propyl formate azeotrope. Background technique [0002] Extractive distillation is a kind of special distillation separation technology, and it is mainly used for systems that have azeotropic phenomena in industrial production but cannot be separated by ordinary separation methods. It increases the relative volatility of two or more components in the original azeotropic mixture by adding a third component, so as to achieve the purpose of separation. Interstitial extractive distillation combines the advantages of both batch distillation and extractive distillation. The equipment is flexible in operation, and multiple components can be separated through one tower. The investment in equipment is small, and it is suitable for small batches of azeotro...

Claims

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Application Information

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IPC IPC(8): C07C27/32C07C31/04C07C29/84C07C69/06C07C67/54C07B63/00B01D3/40
CPCB01D3/40C07C29/84C07C67/54C07C31/04C07C69/06Y02P20/54
Inventor 姜占坤刘顺江孙国新
Owner UNIV OF JINAN
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