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Method for synthesizing APE by using allyl alcohol as accelerator

Date  2020-07-04 22:22:54 Shenzhen Prechem New Materials Co., Ltd Views

Etherization reaction is a reaction in which pentaerythritol and dipentaerythritol are added to alkali metal hydroxide solution to dissolve in temperature, and then allyl alcohol accelerator is added to adjust the reaction temperature at 80~120℃ under normal pressure. For better performance, propylene chloride can also be added under pressure, and the reaction temperature must be maintained at 80~120℃. When the reaction time is lower than 80℃, the reaction time is longer than 120℃, and the fertility rate of side reaction is lower. The reaction is best carried out under reflux conditions, and the water in the system is best slowly removed near the rapid reaction stage. It is better to add the required alkali metal aqueous solution to the rapid reaction section and then add some more. The addition amount of propylene chloride can be freely selected according to the composition of allyl ether. However, the amount of alkali metal hydroxide should be 1~1.2 times that of propylene chloride. For alkali metal hydroxides, sodium hydroxide and calcium hydroxide are preferred. Industrialization, choose sodium hydroxide advantageous. As for the concentration of alkali, the requirement of fast reaction is high concentration, usually choose 30~60% range is more appropriate. Generally, it is convenient to use the market mass concentration of 50% directly. If the concentration of base is lower than 30%, the reaction speed will be slower, while if the concentration is above 60%, the solubility of pentaerythritol and dipentaerythritol will be reduced. This creates a balance problem.

When allyl alcohol was added into the system as a reaction accelerator, the ratio of 2~15% of pentaerythritol and dipentaerythritol in 100 parts (weight) was appropriate. Under 2%, the promotion effect is not obvious, higher than 15% will produce a lot of diallyl ether by-products.