Preparation Of 1,3-dioleoyl-2-palmitoylglycerol By Transesterification And Its Process Enlargement

Human milk is the golden standard of infant formula.1,3-dioleoyl-2-palmitoylglycerol(OPO),which is designed as the human milk substitute,is used wildly in high-end infant formula.In this study,we found a process to prepare the 1,3-dioleoyl-2-palmitoylglycerol and use packed bed reactor to enlarge this process.Finally use molecular distillation to separate the product.The contents are as followed:1.First,use palmitic acid and glycerol in the molar ratio in 1:2.8 as raw material and use sulfuric acid as catalyzer.Under vacuum condition,The reaction react at 130? for 2 hours and then react at 160? for 6 hours.The raw product is washed by hot salt water to get purified PPP.PPP is mixed with ethyl oleate at a molar ratio of 1:7 as substrate.Substrate use 4A molecular sieve to remove water.The product was catalyzed by Novoozym(?)40086 with a mass of 10%PPP in the substrate and reacted in a shaker at 55? for 12 hours at 200 rpm.The total proportion of OPO in triglyceride(TAG)was 44.67%.2.Secondly,the process of the interesterification is applied and optimized in stirred reactor,rotating packed bed reactor and packed bed reactor,and compare the result of the reaction in different kind of reactors.The comparing factor include the account for OPO in TAG in one batch product,and the average account for OPO in TAG in all product and the life-span of the lipase.Through compare,the most applicable reactor is packed bed reactor,and the account for OPO in TAG in one batch product is 46.53%.Lipase can react in packed bed reactor for 7 times.3.Then establish a continuous fed-batch process to keep the substrate stability flow in lower temperature.In the first step,the water-removed substrate,which is mixture of PPP and ethyl oleate with the ratio of 1:14,pump into the packed bed reactor,which is filled 5.4 g Novozym(?)40086.The reactor temperature is 50?.The residence time of reaction is 28.1 min.When the reactor runs 96 hours,the half lipase become inactive.The account for OPO in TAG in first-step product is 35.44%.In the second step,add PPP in first-step product to make the ratio of TAG to ethyl fatty acid in 1:7.The substrate pump into the packed bed reactor,which is filled 5.4 g Novozym(?)40086.The reactor temperature is 55?.The residence time of reaction is 28.1 min.When the reactor runs 72 hours,the half lipase become inactive.The account for OPO in TAG in first-step product is 43.59%.4.Finally,heat the product and filter to remove trace free lipase and micro-insoluble particles.And use and compare molecular distillation with vacuum distillation to separate TAG from product.And the best way to separate is using molecular distillation.The product is pump into molecular distillation in 60 mL/min.The rotating rate of scraper is 250 rpm.And the temperature of the evaporating surface is 180? and condensing surface is 30?.TAG accounted for 92.11%of the total base material,while OPO accounted for 40.31%of the total product.