Study On The Technology Of Synthesizing Perillartine Through Catalyzing And Transforming β-pinene

Perillartine is a new kind of food additive with high sweetness andlow caloricity. It is stable in character, heat-proof, poison-proof,avirulence and etch-proof, and could be used in the business lines oftobacco, daily chemical, food, etc. Perillartine has been being researchedand developed only since the later 80s of 20th century, but it has abroadening usage. Therefore, researching and studying perillartine willput great significance to the essence and spice industry, and we assurethat it will welcome a bright market prospect. In our experiment,Perillartine has been synthesized through usingβ-pinene from ourabundant turpentine oil as raw material by 4-step reactions: epoxidation,isomerization, oxidation and oximation. The method takes short synthesissteps, needs moderate experiment condition, and gives high yield.Following are the 3 conclusions:1. Set down peracetic acid titration system and titrated theconcentration of the peracetic acid by various proportion between H₂O₂and acetic acid, then studied its influence onβ-pinene epoxidation,confirm the best proportion: with 3% Sulfuric acid as the catalyst, 50%H₂O₂, n(H₂O₂):n(HOAc)=1:1.3—1.5 to make about 26% peracetic acid,using which to epoxidizeβ-pinene synthesize 2,10-epoxypinane with high selective and transformation rate, and researched the experimentaltemperature.2. The product distribution and reaction mechanism of2,10-epoxypinane by nitrate catalysts are studied, researched theinfluence on the product distribution by catalysts and reaction condition.Based on the past research achievement, through the analysis on theproduction parameter and results, discover that solvent purity inisomerization reaction is the key factor to influence the yield of perillylalcohol. Promoted the technology process of purify solvent throughanalysis the impurity in the recycled solvent. Choose the petroleum aetheras extractant to extract twice, and then the purity of nitromethane wasenhanced up to 98%, terpene≤1%. Solvent purification has got itssuccess in industry process and gained similar results as in experiment.3. Reaction regulations of synthesizing perillaldehyde throughsupported oxidant selectively oxidizing Perillyl alcohol are studied. Wealso investigated the influence on perillaldehyde yield rate by usingvarious dosages of supported oxidant and reaction condition.Perillaldehyde yield rate shall be up 80% in optimized reaction condition.The reaction mechanism is promoted after analyzing the mutual influencebetween the oxidant and the carrier. The proper condition of synthesizingperillartine with 60% perillaldehyde as stuff is: perillaldehyde:hydroxylamine hcl: sodium carbonate=1.0: 1.4: 0.7(mol), reaction temperature 40℃, reaction time 4h. In this way, the yield of perillartinereaches 78.5%.