Refining method of vinyl ethyl ether

Abstract

The invention discloses a refining method of vinyl ethyl ether, and belongs to the technical field of fine chemical engineering. The preparation method comprises the following steps: adding industrial-grade vinyl ethyl ether into deionized water, stirring, heating, and standing to separate water; the purity of the high-purity vinyl ethyl ether is greater than or equal to 99.5%, the water content is less than or equal to 0.1%, and the single impurity content is less than or equal to 0.1%. The method is simple in route operation, stable in quality and suitable for industrial production, and the product meets the downstream polymerization requirement of vinyl ether.

Description

Technical Field

[0001] The invention relates to a method for refining vinyl ethyl ether, belonging to the technical field of fine chemical industry. Background Art

[0002] Ethyl vinyl ether, anesthetizes the central nervous system, and its anesthetic effect is stronger than that of ether. It is used as an anesthetic and sedative in medicine, and is also used as a pharmaceutical chemical intermediate. It can also be used in the production of drugs such as sulfadiazine, glutaraldehyde, polymers, and coatings. It is often used as a monomer for homopolymers / copolymers. In the process of synthesizing ethyl vinyl ether, impurities such as acetylene, ethanol, acetaldehyde, vinyl propyl ether, vinyl isobutyl ether, 1,1-diethoxyethane, and water are produced; these impurities affect the polymerization of ethyl vinyl ether, and high molecular weight polyvinyl ethyl ether cannot be obtained.

[0003] The existing production method of vinyl ethyl ether is to react acetylene with ethanol and then wash it with water to obtain it. Impurities such as acetylene and ethanol remain in it, making the content less than 99.2%, which affects its application in the field of polymerization and coatings. Summary of the invention

[0004] In order to overcome the shortcomings of the prior art, the present invention provides a method for producing high-purity vinyl ethyl ether. The method proposes to further remove ethanol by water washing; remove acetaldehyde, vinyl propyl ether, vinyl isobutyl ether, and 1,1-diethoxyethane by vaporization; and remove acetylene by heating. Vinyl ethyl ether with a purity of ≥99.5%, a moisture content of ≤0.1%, and a single impurity of ≤0.1% is obtained.

[0005] The invention discloses a method for refining vinyl ethyl ether, comprising the following operations: adding deionized water to industrial-grade vinyl ethyl ether, stirring and heating, and then standing to separate water; adding a stabilizer, vaporizing and condensing, and obtaining high-purity vinyl ethyl ether with a purity of ≥99.5%, a water content of ≤0.1%, and a single impurity of ≤0.1%.

[0006] Furthermore, in the above technical solution, the industrial grade vinyl ethyl ether has a purity of 95-98% and a water content of >0.2%.

[0007] Furthermore, in the above technical solution, the deionized water has a conductivity of ≤20 μs / cm and is added in an amount of 50%.

[0008] Furthermore, in the above technical solution, the stirring time is 2 to 5 hours, the standing time is 30 to 60 minutes, and the temperature is 20 to 40°C.

[0009] Furthermore, in the above technical solution, the stabilizer is potassium hydroxide or sodium hydroxide, and the added amount is 1 to 2‰.

[0010] Furthermore, in the above technical solution, the vaporization temperature is 30-50°C.

[0011] Furthermore, in the above technical solution, product purity and individual impurity tests are determined by GC.

[0012] Furthermore, in the above technical solution, the moisture test adopts KF determination.

[0013] Advantageous Effects of the Invention

[0014] The invention adopts industrial-grade vinyl ethyl ether for purification, adopts water washing to remove ethanol, removes acetaldehyde, vinyl propyl ether, vinyl isobutyl ether and 1,1-diethoxyethane by vaporization, removes acetylene by heating, and obtains a product with a GC purity of ≥99.5%, impurities of ≤0.1% and water content of ≤0.1%.

[0015] The route of the invention is simple to operate and has stable quality, is suitable for industrial production, and the product meets the requirements of downstream polymerization of vinyl ether. DETAILED DESCRIPTION

[0016] Embodiment 1:

[0017] Add 400g of vinyl ethyl ether (GC purity 98.1%, water 0.3%) to the reaction bottle, add 200g of deionized water, heat to 25°C, stir for 3 hours, stand for 30 minutes to separate water; add 0.4g of potassium hydroxide, heat to 40°C, collect the condensed product, and obtain 380g of product vinyl ethyl ether. After testing, the GC purity is 99.54% and the water content is 0.06%.

[0018] Example 2

[0019] Add 400g of vinyl ethyl ether (GC purity 97.8%, water 0.4%) to the reaction bottle, add 180g of deionized water, heat to 25°C, stir for 3 hours, stand for 30 minutes to separate water; add 0.7g of potassium hydroxide, heat to 45°C, collect the condensed product, and obtain 382g of product vinyl ethyl ether. After testing, the GC purity is 99.61% and the water content is 0.07%.

[0020] Example 3

[0021] Add 400g of vinyl ethyl ether (GC purity 98.2%, water 0.4%) to the reaction bottle, add 240g of deionized water, heat to 25°C, stir for 3 hours, stand for 30 minutes to separate water; add 0.6g of potassium hydroxide, heat to 40°C, collect the condensed product, and obtain 385g of product vinyl ethyl ether. After testing, the GC purity is 99.62%, and the water content is 0.05%.

[0022] Example 4

[0023] Add 400g of vinyl ethyl ether (GC purity 98.4%, water 0.5%) to the reaction bottle, add 200g of deionized water, heat to 25°C, stir for 3 hours, stand for 30 minutes to separate water; add 0.8g of potassium hydroxide, heat to 40°C, collect the condensed product, and obtain 387g of product vinyl ethyl ether. After testing, the GC purity is 99.59% and the water content is 0.05%.

[0024] The above are only preferred specific implementation modes of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solutions and inventive concepts of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for refining vinyl ethyl ether, characterized in that: The method comprises the following operations: adding deionized water to industrial-grade vinyl ether, stirring and heating, and then standing to separate the water; adding a stabilizer, vaporizing and condensing to obtain high-purity vinyl ether with a purity of ≥99.5%, a water content of ≤0.1%, and a single impurity of ≤0.1%.

2. The method for refining vinyl ether according to claim 1, characterized in that: The industrial grade vinyl ethyl ether has a purity of 95-98% and a water content of more than 0.2%.

3. The method for refining vinyl ether according to claim 1, characterized in that: The deionized water has a conductivity of ≤20 μs / cm and is added in an amount of 50%.

4. The method for refining vinyl ethyl ether according to claim 1, characterized in that: The stirring time is 2 to 5 hours, the standing time is 30 to 60 minutes, and the temperature is 20 to 40°C.

5. The method for refining vinyl ethyl ether according to claim 1, characterized in that: The stabilizer is potassium hydroxide or sodium hydroxide, and the added amount is 1-2‰.

6. The method for refining vinyl ether according to claim 1, characterized in that: The vaporization temperature is 30-50℃.

7. The method for refining vinyl ethyl ether according to claim 1, characterized in that: Product purity and individual impurity tests are determined by GC.

8. The method for refining vinyl ethyl ether according to claim 1, characterized in that: The moisture content is measured by KF test.