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Study On Synthesis Technology Of Ambergris-Like Perfume From Citral

Posted on:2010-07-09Degree:MasterType:Thesis
Country:ChinaCandidate:Y BaiFull Text:PDF
GTID:2121360275980877Subject:Forest Chemical Processing Engineering
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Ambergris from the sperm whale is known as one of the world's four major animal spices.Because of its complex and balanced flavor with each other and lasting fragrance emanated capacity.included healing tonic,aphrodisiac,anti-inflammatory.analgesic and other medical effects,it gets more and more attention.In recent years,as a result of endangered sperm whales,ambergris fragrance in the world market has become the "gray gold".Pseudoionone is synthesized with citral and acetone based on aldol reaction.Then the compound,ambergris-like perfume,which have the ambergris octalin structure are synthesized from pseudoionone by multi-step reaction.What's more.the new synthetic routes are put forw ard and preliminarily confirmed.Through systematic analysis of main factors such as the kind and the dosage of the catalyst. temperature,time,mixture ratio of the materials,manner of feeding,the traditional synthesis was improved.In this dissertation,those expensive reagents were replaced by the cheap,common and easy processing ones.The environmentally friendly reagents were instead of strong corrosive catalyst.Then some unimportant post treatments are omitted for cost saving.These enabled the industrial production of the response are easily reduced the post-treatment processes.Solid sodium hydroxide used as a catalyst in synthetic pseudoionone reactions,the best conditions like these:reaction temperature is 65℃.reaction time is 1.5h,the molar ratio of acetone and citral is 1:3, the yield of pseudoionone is 90.96%:reaction products by a vacuum distillation,distillate pseudoionone materials content was 88%.The catalyst was low-cost,easy to get and used less.Lewis acid catalyst aluminum chloride is firstly used in synthesis of ionone,and the best conditions are:at 0℃,the weight ratio of the catalyst and raw materials is 3:4,reaction time is 3 hours under the conditions,β-ionone yield is 45.54%,2dihydro-α-ionone yield is 43.55%.the total conversion rate of pseudoionone is 96.00%.In addition,the catalyst can be reused,clean elections,with the characteristics of green synthesis.The optimized reaction conditions of accessing to synthetic ambergris-like perfume scent technology:reaction temperature is 28℃,reaction time is 6 h,ether andβ-ionone volume ratio is 1:1, the reactant molar ratio is 5:1.4%ethanol solution of sodium hydroxide as catalyst,the product of ambergris fragrance flavor yield is 82.75%.This reaction conditions are mild,the post-processing is very convenient.The total yield of ambergris-like perfume relatived citral was 30.17%by three steps.And GC or GC-MS test proved the resulted substances the pseudo-ionone,β-ionone,dihydro-α-ionone and tricyclicoxalactone(Benzo[e]isobenzofuran-1.4-dione,1,3.4,5,5a,6,7,8,9.9a-decahydro-6,6.9a-trimethy) are the desired products.
Keywords/Search Tags:Ambergris-like perfume, pseudoionone, β-ionone, dihydro-α-ionone, citral
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