Method for preparing compound 4-hydroxy butyl vinyl ether

A technology of hydroxybutyl vinyl ether and compounds, which is applied in the field of preparation of vinyl ether compounds, and can solve problems such as increasing the contact time of acetylene gas, low vinyl ether content, and high cyclic acetal by-products

Inactive Publication Date: 2010-12-01
焦作新景科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] It can be seen from the above description that the German patent GB773331 also has shortcomings: the content of vinyl ether after the reaction is still not high, and the by-product of cyclic acetal is relatively high. This is because the acetylene reaction is a gas-liquid phase reaction, and GB773331 passed The reaction column is filled with ceramic fillers to increase the contact time between acetylene gas and glycols (compared with no ceramic fillers), but this method alone is not enough

Method used

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  • Method for preparing compound 4-hydroxy butyl vinyl ether
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  • Method for preparing compound 4-hydroxy butyl vinyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 2000g of 1,4-butanediol and 180g of potassium hydroxide into a 3000ml three-necked bottle, start stirring, heat the oil bath to 140°C, distill under 0.05MPa vacuum, and slip out about 200g of colorless transparent liquid to obtain about 1980g of brown Viscous liquid, add 400g dimethyl sulfoxide, stir well and set aside.

[0048] Such as figure 1 Shown: Weigh about 400g of the above raw materials and add them to the packing reaction tower 1. The packing reaction tower is 70cm high and 5cm in diameter (volume 0.9L, the actual volume after filling the ceramic ring is 0.6L), the packing is ceramic ring 2, open The heat supply control system 3 uses the heat transfer oil 9 oil bath to supply heat, and when the temperature reaches 170°C, open the acetylene gas valve 4 and the nitrogen gas valve 5, and pass the flowmeter, the acetylene gas: nitrogen = 60:40 (V / V) The ratio is passed into the tower, and the flow rate of the mixed gas is 15-20L / H. At the same time, the dropp...

Embodiment 2

[0050]Add 2000g of 1,4-butanediol and 180g of potassium hydroxide into a 3000ml three-necked bottle, start stirring, heat the oil bath to 140°C, distill under 0.05MPa vacuum, and slip out about 200g of colorless transparent liquid to obtain about 1980g of brown Viscous liquid, add 400g dimethyl sulfoxide and 10g octadecyltrimethylammonium chloride, stir well and set aside.

[0051] Such as figure 1 Shown: Weigh about 400g of the above raw materials and add them to the packing reaction tower 1. The packing reaction tower is 70cm high and 5cm in diameter (volume 0.9L, the actual volume after filling the ceramic ring is 0.6L), the packing is ceramic ring 2, open The heat supply control system 3 uses the heat transfer oil 9 oil bath to supply heat, and when the temperature reaches 170°C, open the acetylene gas valve 4 and the nitrogen gas valve 5, and pass the flowmeter, the acetylene gas: nitrogen = 60:40 (V / V) The ratio is passed into the tower, and the flow rate of the mixed g...

Embodiment 3

[0053] Add 2000g of 1,4-butanediol and 180g of potassium hydroxide into a 3000ml three-necked bottle, start stirring, heat the oil bath to 140°C, distill under 0.05MPa vacuum, and slip out about 200g of colorless transparent liquid to obtain about 1980g of brown Viscous liquid, add 300g dimethyl sulfoxide and 8g octadecyltrimethylammonium chloride, stir well and set aside.

[0054] Such as figure 1 Shown: Weigh about 400g of the above raw materials and add them to the packing reaction tower 1. The packing reaction tower is 70cm high and 5cm in diameter (volume 0.9L, the actual volume after filling the ceramic ring is 0.6L), the packing is ceramic ring 2, open The heat supply control system 3 uses the heat transfer oil 9 oil bath to supply heat, and when the temperature reaches 170°C, open the acetylene gas valve 4 and the nitrogen gas valve 5, and pass the flowmeter, the acetylene gas: nitrogen = 55:45 (V / V) The ratio is passed into the tower, and the flow rate of the mixed g...

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Abstract

The invention belongs to a method for preparing a vinyl ether compound, in particular to the method for preparing 4-hydroxy butyl vinyl ether. In the reaction of 1,4-butanediol and acetylene, dimethyl sulfoxide is added so that beneficial effects are achieved for the reaction, wherein the content of a 4-hydroxy butyl vinyl ether crude product is improved to 81 percent from 72 percent before adding; and a cyclic acetal byproduct is reduced to about 4 percent from 6 percent before adding. The content of the crude product can be further improved by 1 to 2 percent by adding a cationic surface active agent, namely octadecyl trimethyl ammonium chloride.

Description

technical field [0001] The invention belongs to a preparation method of vinyl ether compounds, in particular to a preparation method of 4-hydroxybutyl vinyl ether. Background technique [0002] Vinyl ether compounds are unsaturated ethers, which are very important organic synthesis intermediates and high polymer monomers. Its homopolymers and copolymers are widely used in adhesives, coatings, lubricants, Plasticizers, pesticides, and surface protection materials and many other fields. In recent years, it has developed rapidly as a vinyl ether reactive diluent for radiation-cured coatings, or modified epoxy resins with vinyl ethers into oligomers containing vinyl ether functions, and applied to UV-cured coatings. middle. For this reason, the application prospect of vinyl ether compounds is extremely broad. [0003] 4-Hydroxybutyl vinyl ether is an important kind of vinyl ether compounds. [0004] The industrial production of 4-hydroxybutyl vinyl ether is mainly the acetyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/178C07C41/08B01J31/26
Inventor 方钢阎璟琪项雄彪
Owner 焦作新景科技有限公司
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