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Synthesis And Characterization Of Sodium2-Hydroxy-3-Chloro Propanesuifate Under Microwave Irradiation

Posted on:2013-03-01Degree:MasterType:Thesis
Country:ChinaCandidate:W WangFull Text:PDF
GTID:2251330401450861Subject:Chemical Engineering and Technology
Abstract/Summary:PDF Full Text Request
Microwave chemistry,as a green chemistry, which not only can dramaticallyreduce reaction time but also make a “new” reaction possible, has been widely used inorganic synthesis. Nowadays microwave-heating is becoming a widespreadtechnology in the fields of organic chemistry. With the development of our nationaleconomy and a corresponding growth of research funds, microwave chemical reactoris playing an increasingly important role in organic laboratory.Sodium2-hydroxy-3-chloro propanesulfate(CHPS),is a kind of chloridecontaining hydroxide and sulfonate, in which both halogen and hydroxyl group havehigh activity and sulfonate is hydrophilic as well. For these reasons, CHPS is widelyapplied to synthesis of key functional monomer in polymers fields and also becomes asignificant fine intermediate. Thus, it can be used as organic chemical intermediatesfor the preparation of better anion surfactant, amylum, water loss control agents in saltdrilling fluid, functional monomer for polymers and etc. At present, the research onmicrowave synthesis,characteristics and application of CHPS has not been reported.Therefore, the research in this paper has great significance to the theory and practiceof further study on objective product.In this paper, CHPS was synthesized from sodium hydrogensulfite andepichlorohydrin(ECH)with Tetrabutylammonium bromide (TBAB) as the phasetransfer catalyst under normal condition and microwaves irradiation, respectively. Theproducts were characterized by IR, elementary analysis, melting point testing and itsphysicochemical property, thus some characteristics of the products are obtained inthis paper. The effect of reaction temperature, microwave radiation time, radiationpower, molar ratio of reactants, catalyst dosage, and the amount of solvent on productyield was investigated. The optimized reaction conditions under microwavesirradiation were that molar ratio of sodium hydrogensulfite to epichlorohydrin(ECH)was1:1.4, reaction temperature85℃, addition time25min, the time of reflux reaction10min,microwave power500W, and the yield reaches over85%.The optimal conditions for the synthesis of CHPS were investigated with TBABas catalyst on the basis of orthogonal design5factors and4levels under normalcondition and microwaves irradiation, respectively. Then, the optimum operationconditions have been further evaluated and the results are summarized and discussed.And then,3-allyoxy-2-hydroxy-1-propanesulfonic acid salt was synthesized from the objective product CHPS and reaction conditions were optimized as well.Finally, lauric acid-2-hydroxy-3-Allyloxy-1-propanesulfonic acid salt, a novel geminisurfactant, which was widely applied to the fields such as biology,chemicalengineering, pharmacy,food additive and etc, was prepared from the above-mentionedproduct and lauric acid.
Keywords/Search Tags:Microwave field, Sodium2-hydroxy-3-chloro propanesulfate, Epichlorohydrin, Tetrabutylammonium bromide, Synthesis
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