One, at present, the synthesis method of isoeugenol all exists the problem that production process is comparatively complicated, production cost is high, or reaction waste liquid pollutes environment, or cis-isoeugenol content is too high. CN201410100405.2 provides a synthetic method of isoeugenol, aiming to solve the complex production process and high production cost of the current synthetic method of isoeugenol, or the reaction waste liquid pollutes the environment, or the content of cis-isoeugenol is too high high question. Include the following steps:
(1) Add clove powder to 1mol/L potassium hydroxide solution and ethanol, place it at 100-130 °C for 1-2 hours under the condition of ultrasonic waves, and obtain a decomposition liquid; wherein, the clove powder, potassium hydroxide solution and ethanol The mass-to-volume ratio is (20-30) kg: (5-10) L: (5-10) L;
(2) Stir and mix the decomposed liquid with toluene, then heat and distill in a vacuum state, control the temperature of the distillation heating place to be 50-90°C, control the temperature of the volatilization outlet of the distillation gas to be 35-45°C, and condense the distillation gas with a condenser After collection, low-boiling impurities are obtained; wherein, the volume ratio of the decomposition liquid to toluene is (5-10): (3-4);
(3) Continue to distill the remaining filtrate after removing low-boiling impurities in the step (2), control the temperature of the distillation heating place to be 100°C-120°C, control the temperature of the distillation gas volatilization outlet to be 90-105°C, and use the distillation gas to The isoeugenol is obtained after condensation and collection in the condenser.
In the present invention, the amount of lye required is greatly reduced, and the liquid in the reaction process can be directly used for distillation without extraction and separation, and the operation is simpler; in addition, the reagents and test devices used in the present invention are all More commonly used, the production cost is very low; more importantly, the content of trans isoeugenol obtained in the present invention in isoeugenol can reach more than 95%.
2. CN201410811548.4 provides a method for preparing isoeugenol by catalytic pyrolysis of biomass using ruthenium or rhodium catalysts. According to the method provided by the invention, using biomass as raw material, the biomass and ruthenium or rhodium catalysts are mechanically mixed according to the mass ratio of (10:1) to (1:3), and then under anaerobic conditions at 250 Rapid pyrolysis at ~400°C, and the liquid product rich in isoeugenol can be obtained after the pyrolysis gas is condensed. The ruthenium-based or rhodium-based catalysts used in the present invention can greatly promote the formation of isoeugenol in the biomass pyrolysis process of Pinaceae, Sequoia, Cupressaceae or Araucariaceae, while inhibiting the pyrolysis of cellulose and hemicellulose Formation of volatile organic products and inhibition of lignin pyrolysis to form other phenolic products. Therefore the liquid product that obtains has relatively simple composition, and the purity of isoeugenol is higher, greatly simplifying its follow-up separation and purification process. Secondly, the performance of the catalyst is stable, and it can be separated from the pyrolysis residue by mechanical means to achieve recycling. In addition, the present invention controls the pyrolysis temperature at 250-400°C, and there are fewer pyrolysis products at a lower pyrolysis temperature, which is not only beneficial to control the product composition and further improve the selectivity to isoeugenol, but also has great impact on equipment and reaction conditions. The requirements are lower, which is conducive to reducing production costs.
