Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification

A technology of ethyl isobutyrate and extractive distillation, which is applied in extractive distillation, purification/separation/stabilization of organic compounds, preparation of carboxylate, etc. Low cost, low process energy consumption, and small equipment investment

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

Chinese patent CN101028986, the method for extracting and rectifying the separation of benzene, the selected extractant is pure organic solvents such as alcohols, and there are certain defects in the stability performance
Due to the existence of azeotropy, common separation methods are difficult to achieve. If it is not recycled, it will not o...

Method used

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  • Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification

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Experimental program
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Effect test

Embodiment 1

[0013] Using a batch extraction and rectification device, put 500L of isobutanol-ethyl isobutyrate mixture into the heating kettle (52% of isobutanol and 48% of ethyl isobutyrate, both are mass fractions), the selected extractant in the experiment It is 90wt% ethylene glycol and 10wt% [Emim][OAc]. Turn on the heat source of the heating kettle and the cold source of the condenser. The feeding position is close to the top of the tower, the extraction agent addition rate is controlled to 550L / h, and the total reflux operation is performed. When the temperature at the top of the extractive distillation tower is 109~110°C, the content of ethyl isobutyrate in the distillate is ≥99%. Start discharging, the reflux ratio is 9:1, and the discharging speed is 200L / h. When the temperature at the top of the extractive distillation column drops to 107~109°C, take out the transition section of isobutanol-ethyl isobutyrate, and stop adding the extractant. The reflux ratio is 10:1. When t...

Embodiment 2

[0015] Using a batch rectification extraction device, put 500L isobutanol-ethyl isobutyrate mixture into the heating tank (50% isobutanol, 50% ethyl isobutyrate, both are mass fractions), and the extractant is 85wt% ethyl alcohol Diol and 15wt%[Emim][OAc], turn on the heat source of the heating kettle and the cold source of the condenser, after a period of reflux at the top of the extractive distillation column, wait for the temperature at the top of the tower to stabilize, add the extractant, and the extraction feed position is near At the top of the tower, control the addition rate of the extractant to 800L / h, and operate under total reflux. When the temperature at the top of the extractive distillation tower is 109~110°C, the content of ethyl isobutyrate in the distillate is ≥99%. The ratio is 12:1, the discharge rate is 300L / h, when the temperature at the top of the extractive distillation column drops to 107~109°C, the transition section of isobutanol-ethyl isobutyra...

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Abstract

The invention relates to a separation method of an isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification, which comprises the following steps: ethylene glycol and an ionic liquid 1-ethyl-3-methylimidazolyl acetate are used as extractants; under normal pressure or reduced pressure, the mass ratio of the extractants entering an extraction rectification tower to the overhead is (1.8-5):1; the charging temperature of the extractants is 20-40 DEG C, and a qualified transition section I of ethyl isobutyrate, ethyl isobutyrate and isobutanol and a transition section II of isobutanol, isobutanol and ethylene glycol are sequentially produced from the tower top; and when the components of the extractants at the tower bottom satisfy the requirements, the tower is shut down for cooling, and the extractants are pumped into a higher-position storage tank for use of the next batch of material. The extraction rectification device used by the method comprises an extraction rectification tower, a heating kettle, a condenser, a higher-position storage tank, a receiving tank, a product tank and a vacuum pump.

Description

technical field [0001] The invention relates to a separation method for intermittent extraction and rectification of isobutanol-ethyl isobutyrate azeotrope, which belongs to the special rectification separation technology of isobutanol-ethyl isobutyrate azeotrope. Background technique [0002] Extractive distillation is a kind of special distillation separation technology, which is suitable for separating azeotropic systems that are difficult to separate by ordinary distillation. It increases the relative volatility of two or more components in the original azeotropic mixture by adding an extractant (solvent), 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 azeotropic or near-boiling syste...

Claims

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Application Information

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IPC IPC(8): C07C27/32C07C31/12C07C29/84C07C69/24C07C67/54C07B63/00B01D3/40
CPCC07C29/84B01D3/40C07C67/54C07C31/12C07C69/24
Inventor 姜占坤刘顺江孙国新
Owner UNIV OF JINAN
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