Method for synthesizing dihydric alcohol single vinyl ether and double vinyl ether

A technology of alcohol monovinyl ether and divinyl ether, which is used in the synthesis field of vinyl ether compounds to achieve the effect of improving catalytic activity

Active Publication Date: 2011-09-07
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] For above-mentioned shortcoming, the object of the present invention is to provide a kind of under the situation that reaction temperature is not high, carry out normal pressure reaction to prepare vinyl ether, and can improve the synthetic method of dibasic alcohol monovinyl ether and divinyl ether of catalytic activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] Example 1 (comparative example)

[0023] Preparation of potassium alkoxide solution: Add 1,4-butanediol (BDO) 80g, industrial grade KOH 6.5g, polyethylene glycol dimethyl ether (M =300) 120 g, conduct heating reaction and carry out vacuum distillation at a vacuum degree above 0.090 MPa, and keep at 100-120 ℃ for 1-2 h to obtain potassium alcoholate solution;

[0024]First pass nitrogen to drive away the air in the system, then introduce acetylene into the reaction kettle through a safety bottle and a flow meter, observe the tail gas bubbles, so that the acetylene is slightly excessive during the reaction process, react at 140°C for 6 h, and then reduce the reaction solution to Press distillation, obtain cut 85.1g, measure component by gas chromatography and micromoisture analyzer, the result is as follows:

[0025] components

[0026] The conversion rate of BDO is 48.1%.

example 2

[0028] The preparation of potassium alkoxide is the same as in Example 1; 1.6 g of zinc oxide is added to the reaction solution composed of self-made 1,4-butanediol potassium alkoxide solution and polyethylene glycol dimethyl ether (M=300), and nitrogen gas is used to drive it away The air in the system, then introduce acetylene into the reaction kettle through the safety bottle and flow meter, observe the tail gas bubbles, so that the acetylene is slightly excessive during the reaction process, react at 140 ℃ for 6 h, and then distill the reaction solution under reduced pressure to obtain the fraction 77.4 g, measure components by gas chromatography and trace moisture meter, the results are as follows:

[0029] components

[0030] The conversion rate of BDO is 52.5%.

example 3

[0032] The preparation of potassium alkoxide is the same as that in Example 1. Add 1.6 g of triphenylphosphine to the reaction solution composed of self-made potassium alkoxide solution of 1,4-butanediol and polyethylene glycol dimethyl ether (M=300), and pass nitrogen gas first. Drive away the air in the system, then introduce acetylene into the reaction kettle through a safety bottle and a flow meter, observe the tail gas bubbles, so that the acetylene is slightly excessive during the reaction process, react at 140 °C for 6 h, and then distill the reaction solution under reduced pressure, Obtain cut 85.8 g, measure component by gas chromatography and micromoisture analyzer, the result is as follows:

[0033] components

[0034] The conversion rate of BDO is 47%.

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PUM

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Abstract

The invention relates to a method for synthesizing dihydric alcohol single vinyl ether and double vinyl ether. The method comprises the following steps of: preparing alcohol potassium solution from mixed liquid consisting of dihydric alcohol, potassium hydroxide and polyethylene glycol dimethyl ether; adding zinc oxide, triphenylphosphine or a mixture of the zinc oxide and the triphenylphosphine into the prepared alcohol potassium solution to prepare a reaction mixture; heating the reaction mixed liquid to 80 to 200 DEG C; introducing ethyne to react; after the reaction is finished, distilling the product under reduced pressure of below 2 kPa; and collecting fractions with the kettle temperature of below 180 DEG C to obtain a crude product of the dihydric alcohol single vinyl ether and double vinyl ether. The method has the advantages of preparing vinyl ether by reacting under normal pressure and low reaction temperature and improving catalytic activity.

Description

technical field [0001] The invention relates to a method for synthesizing vinyl ether compounds, in particular to a method for synthesizing glycol monovinyl ether and divinyl ether. Background technique [0002] The general formula of vinyl ether compounds: CH 2 =CHOROR 1 (where: R=(CH 2 )n, n=2-6; R 1 =H or CH=CH 2 base). Its structure is that the ether bond is directly connected to the vinyl double bond, and the double bond is an electron-rich double bond due to the influence of the adjacent oxygen atom, thus showing higher activity. Vinyl ethers with functional groups such as hydroxyalkyl vinyl ethers have good water solubility due to their hydroxyl groups, and can react with a series of resins, so they have a wide range of uses. These compounds are important organic synthesis intermediates and polymer monomers, and their homopolymers and copolymers are widely used in coatings, adhesives, printing inks, lubricants, plasticizers, elastomers, Foams, insecticides and...

Claims

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Application Information

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IPC IPC(8): C07C43/16C07C43/178C07C41/08
Inventor 朱新宝彭春睿刘准
Owner NANJING FORESTRY UNIV
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