Diethanolamine was added to formalin at 35 ℃,and the mixture was warmed to 40~45 ℃ for 2 h. Whereafter,the water in the mixture was evaporated with vacuum distillation at 80~82 ℃ under 0.094MPa to obtain intermediate,3-(2-hydroxyethyl)-1,3-oxazole(HENH).
On these conditions, pressure is 4.0～6.5kPa, temperature is 160～170℃,the high purity native nicotine is taken by the vacuum distillation, the purity of the product is above 98%, the yield is above 68.7%.
In the first step, stearyl chloride is made by stearic acid and thionyl chloride , n(stearic)∶n(thionyl chloride)=1∶1.5 ,at the reaction temperature 80℃and the reaction time of 6 hours. Stearyl chloride is gotten by collecting the fraction from 170℃ to 200℃in the reduced pressure distillation.
The optimum conditions were below :diethylenetriamine:1,2-epoxypropane:sulfuric acid:water = 1∶0.6∶1∶4.5(mol proportion),reaction temperature is 30~35℃ and rection time is 6 hours,then neutralized,filtrated,distilled,[bis(2-aminothyl) amino]-2-propanol was finally obtained through decompression distillation under 160~164 ℃/1.3 kPa.
The method of segment decompression distillation was applied to separate the product and excessive methanol(MeOH) and ethylene diamine(EDA). Under the lower vacuum conditions(0.06MPa),98.1% of the recovery for both MeOH and EDA was achieved.
In the reaction,sodium methoxide acts as catalyst,the ratio of glyceryl triacetate,glycerin tripropionate and methly stearate is 11∶1∶1,2.5 h of decompression distillation,temperature 82～84℃,the product of this reaction triacylglycerol is smectic solid at normal atmospheric temperature.
At first, according to the characteristics of the physical properties of the component involved, cooling suction screening method is adopted to pass over the concerned steps of decompressed distillation and extraction, which reduces the quantity of the water added to half, and recycle the raw material unreacted in the reacting mixed-liquid.
Decompressed distillation was executed by recovered for 1-6 times mother-liquid as input material, the content of components was determined quantitatively. It could make us to understand the economic significance of micro-reactors being reclyed in synthesizing nano-particles.
3. The parameters of wet saponification for Samara oil were optimized by orthogonal experiment: the sample was saponified in boiled water for 1 hour in alkali hydrolyze conditions, then crude phytosterol was extracted as the proporation 3:1, dissolved in ethanol to saturate state under heat, then decompressed distillation on circumrotate evaporation instrument and crystallize out the content of phytosterol is 19.5%.