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Method for separating ethyl ether, ethyl alcohol and acid water by combining rectifying and azeotropic distilling

A technology of azeotropic distillation and ethanol, applied in the separation/purification of hydroxyl compounds, separation/purification of carboxylic acid compounds, ether separation/purification, etc., can solve the problems of high energy consumption, incomplete separation, and difficulty in recycling

Inactive Publication Date: 2008-02-27
NANJING NORMAL UNIVERSITY
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Problems solved by technology

Ethanol+ether+acid-water separation in the current industrial production is generally separated by gap rectification, etc., to remove ether first, then distill ethanol, adopt this method to separate ethanol and ether, and the purity of separated ether and ethanol is generally about 94% and 91%, and The first-time yield is only about 87% and 80%, and the separation is not complete, which will cause difficulty in the recycling process and high energy consumption
At the same time, the acid water contains a certain amount of ethanol and ether, which will easily cause problems to the environment.

Method used

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  • Method for separating ethyl ether, ethyl alcohol and acid water by combining rectifying and azeotropic distilling

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Embodiment Construction

[0021] With reference to the technique shown in Figure 1 and the parameters shown in Table 2, the raw material (F1) is ether+ethanol+acid water mixed solution, the mass content (Xf1, Xf2, Xf3) are 2%, 93%, 5% respectively, pH=1~2, flow rate is 110Kg / h, through preheating to 33 ℃, precision rectifying tower T-1 top, low temperature are respectively 34.5 ℃ and 78- At 81°C, the top and low flows are 2.24Kg / h and 107.76Kg / h respectively, the pH values ​​are 5-6 and 1-2 respectively, and the reflux ratio (R1) at the top of the precision distillation column is controlled at 2-3. Bottom composition (x Di , x wi )x D1 =0.9810,x D2 =0.0055,x D3 =0.0135,x w1 = 0.0000, x w2 =0.9485,x w3 =0.0515; the tower bottom components are sent to the deacidification rectification unit T-2 for treatment, the top reflux ratio (R2) is controlled at 3 to 4, and 95.12% ethanol can be obtained at the top of the rectification tower, and the pH value is 5 to 6. The bottom is rich in acid aqueous sol...

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Abstract

The extraction and azeotropy combining process of separating ethyl ether, ethyl alcohol and acid water includes the following steps: the first separating the mixed solution of ethyl ether, ethyl alcohol and acid water inside a rectification apparatus with cyclohexane as azeotrpic agent to obtain ethyl ether in the tower top and ethyl alcohol and acid water in the tower bottom; deacidifying rectification to separate ethyl ether from acid water in a deacidifying rectification tower to obtain ethyl alcohol plus water in the tower top and acid water in the tower bottom to be neutralized; and final azeotrpic rectification of ethyl alcohol plus water in a azeotrpic rectification apparatus to with cyclohexane as azeotrpic agent to obtain ethyl alcohol with water content lower than 0.2 %, with the cyclohexane being used circularly and ethyl alcohol being used as material. The separating apparatus has optimized technological conditions, and the separated ethyl ether and ethyl alcohol has water content lowered to below 1.5% and 0.2% separately.

Description

technical field [0001] The invention relates to a chemical separation process, in particular to a separation method combining rectification and azeotropic distillation of ether, ethanol and acid water. technical background [0002] With the rapid development of my country's economic construction, the demand for ethanol as a solvent continues to increase. It is estimated that the current annual demand is about 4 million tons, while the domestic annual output is only 2 to 3 million tons, which is far from meeting the market demand. Some imports are still required. Ethanol is generally used as a solvent in many synthetic processes of pharmaceutical, chemical and pesticide intermediates, especially in the presence of acid (solid acid or inorganic acid) catalysts, ethanol is easy to produce ether, so it is easy to form ethanol, ether and acidic aqueous solution, ethanol , ether and water can form an azeotrope, and the azeotrope and composition of the azeotrope are shown in Table ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/34C07C43/06C07C29/76C07C31/08C07C51/43
Inventor 顾正桂
Owner NANJING NORMAL UNIVERSITY
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