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Method for purifying ethyl acetate

A technology of ethyl acetate and crude ethyl acetate, which is applied in the field of ethyl acetate, can solve the problems of non-recyclable, high energy consumption, and complicated operation, so as to reduce purification energy consumption, low energy consumption, and reduce purification cost Effect

Active Publication Date: 2021-03-16
宁波大膜科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method obtains ethyl acetate with higher purity, the operation is complicated. The strongly acidic ion exchange resin and 4A molecular sieve introduced in the drying process cannot be recycled after absorbing water impurities on the one hand, and need to be filtered after absorbing water impurities on the other hand. Molecular sieves often cause 4A molecular sieves to remain after filtration. Therefore, ultrafiltration treatment is required after extraction and rectification, which requires high energy consumption and high cost.

Method used

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  • Method for purifying ethyl acetate
  • Method for purifying ethyl acetate
  • Method for purifying ethyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The crude ethyl acetate is composed of ethyl acetate, water, and ethanol solvent. According to mass percentage, ethyl acetate accounts for 94wt%, water accounts for 3.5wt%, and ethanol accounts for 2.5wt%.

[0045] The acid-resistant permeable membrane is a silica membrane.

[0046] 100kg of crude ethyl acetate was separated and dehydrated through an acid-resistant permeable membrane at a flow rate of 5kg / h. After dehydration, the water content on the crude ethyl acetate side was 0.5wt%, and the water content on the permeate side of the membrane was 99.4wt%. Then, ethanol was removed from the dehydrated crude ethyl acetate through rectification, the temperature at the top of the rectification column was 76.8°C, and purified ethyl acetate was obtained from the bottom of the column according to the reflux ratio of 20:1.

[0047] In this example, the yield of ethyl acetate was 86.5%, and the purity was 99.93%.

Embodiment 2

[0049] Crude ethyl acetate is composed of ethyl acetate, water, ethanol, and toluene solvent. According to mass percentage, ethyl acetate accounts for 94wt%, water accounts for 3.5wt%, ethanol accounts for 2wt%, and toluene accounts for 0.5wt%.

[0050] The acid-resistant permeable membrane is T / NaY zeolite molecular sieve composite membrane. Porous α-Al 2 o 3 A hollow ceramic fiber tube is used as a support carrier, with a diameter of 12 mm and an average pore diameter of 2 μm. The T / NaY zeolite molecular sieve composite membrane is prepared on the porous carrier.

[0051] The preparation method mainly includes two parts: firstly, a continuous NaY zeolite molecular sieve coating is prepared on a porous carrier to obtain a NaY zeolite molecular sieve coating modified carrier; then a T-type zeolite is prepared on the NaY zeolite molecular sieve coating modified carrier by a hydrothermal method. Molecular sieve membrane. Specifically include the following steps:

[0052] (1...

Embodiment 3

[0072] The crude ethyl acetate is composed of ethyl acetate, water, and ethanol solvent. According to mass percentage, ethyl acetate accounts for 94.5wt%, water accounts for 3.5wt%, and ethanol accounts for 2wt%.

[0073] The acid-resistant permeable membrane is a silicone membrane.

[0074] 100kg of crude ethyl acetate was separated and dehydrated through an acid-resistant permeable membrane at a flow rate of 160kg / h. After dehydration, the water content on the crude ethyl acetate side was 0.6wt%, and the water content on the permeate side of the membrane was 99.3wt%. Then, the dehydrated crude ethyl acetate was removed by rectification to remove ethanol. The temperature at the top of the rectification tower was 76.8°C, and purified ethyl acetate was obtained from the bottom of the tower according to the reflux ratio of 20:1.

[0075] In this example, the yield of ethyl acetate was 85.3%, and the purity was 99.99%.

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Abstract

The invention provides a method for purifying ethyl acetate. The method comprises the following steps: dehydrating crude ethyl acetate to be treated through an acid-resistant permeable membrane, and removing other impurities through a rectification technique. Compared with a single rectification process, the method has the advantages that water in ethyl acetate is removed in advance through an acid-resistant permeable membrane dehydration technology, so that a ternary or higher azeotropic system formed by ethyl acetate, water, ethanol and the like is broken through, the efficiency of removingother impurities through the rectification technology is remarkably improved, and the yield of ethyl acetate is increased; besides, moisture in the crude ethyl acetate solvent can be effectively removed by the crude ethyl acetate through the acid-resistant permeable membrane, other substances do not need to be added, new pollution is not generated, subsequent additional treatment is not needed, the permeable membrane can be continuously operated, the dehydration efficiency is high, the energy consumption is low, the ethyl acetate purification energy consumption is greatly reduced, and the purification cost is reduced.

Description

technical field [0001] The invention relates to the technical field of ethyl acetate, in particular to a method for purifying ethyl acetate. Background technique [0002] Ethyl acetate is a colorless and transparent liquid with a fruity aroma, volatile, sensitive to air, capable of absorbing water, which can decompose slowly and become acidic; miscible with chloroform, ethanol, acetone and acetaldehyde, soluble in Water; can dissolve certain metal salts (zinc chloride, ferric chloride, etc.); relative density is 0.902, melting point is -83°C, boiling point is 77°C; irritating, median lethal dose (rat, oral) 11.3mol / kg, can be used as extractant. [0003] As an important chemical raw material, ethyl acetate is widely used. For example, it can be used as a standard substance for calibrating thermometers when separating sugars. Determination of tin, gold, iron, mercury, oxidizing agents and platinum. Determination of tin, boron, gold, iron, aluminum, clamp and potassium. F...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C67/54C07C69/14B01D71/02B01D69/02B01D67/00B01D69/12
CPCC07C67/48C07C67/54B01D71/028B01D69/02B01D69/12B01D67/0051B01D67/0041B01D2325/30C07C69/14Y02P20/10
Inventor 孔春龙黄添浩应湖昕金鹏郑凯杰
Owner 宁波大膜科技有限公司
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