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Microwave Synthesis Of Eructopropylpropyl Hydroxysulfonic Acid Betaine And Its Application Study

Posted on:2017-05-31Degree:MasterType:Thesis
Country:ChinaCandidate:M S LiFull Text:PDF
GTID:2351330485496579Subject:Chemical engineering
Abstract/Summary:PDF Full Text Request
Containing a plurality of hydrophilic groups and the long carbon chain, betaine,which will have good application prospects in the fabric industry, is a green surfactant with superior function of softness and wettability. Under microwave radiation, Erucic acid, 3-dimethylamino propylamine, epichlorohydrin ECH and sodium bisulfite as the reaction material to synthesis of Erucoylamidopropyl hydroxysulfobetaine(EHSB).It needs three steps: ring opening reactions, amidation reaction and quaternization reaction. Respectively on the Intermediate 3-Chloro-2-Hydroxy propyl sulfonic acid sodium CHPS-Na and erucic acid amide propyl dimethyl amine EAPDMA and product EHSB purified.After that, identified the structure of the intermediate and final product by FTIR and 1HNMR analysis. Under microwave reaction conditions, this study focused on amidation reaction and quaternization reaction in order to select the best process conditions by single factor and orthogonal experiments. The results compared with the traditional method.This paper examines the basic performance of aqueous solution EHSB: Surface active, Emulsifying properties, solubilising properties, biodegradability ect. Moreover, EHSB and emulsifier 1305 are formulated into an emulsion. Through the single factor experiment to investigated the effects of the individual components of the emulsion stability so as to select the best conditions.Formulated a series of concentrations of the emulsion to deal with lycra and cotton cloth. Tested softness, yellowing resistance, wetting properties of the fabric,and compared with D1821, commercially available of the organic silicon and LHSB. By SEM to Observed before and after processing of the surface of textile fibers morphologies. The results are as follows:1. Ring opening reaction under microwave irradiation process conditions :n(NaHSO3):n(ECH)=1.1:1, water content is 1.3 times of the total mass of reactants.Temperature 70 ?, time 30 min, microwave power 500 W. The yield of Intermediate CHPS-Na is 85%. Comparing with the traditional method, the results show thatuponreaching the same 85% yield, microwave synthesis consumes only 16.7% of the time of traditional methods.2. Under microwave irradiation, optimum reaction conditions of amidation reaction: Nitrogen protection, n(Erucic acid): n(3-dimethylamino propylamine)=1:1.1,Temperature 169 ?, time 90 min, microwave power 400 W. The conversion rate of Erucic acid is 75.5%. Under the same conditions, using traditional method to synthesis, The conversion rate of Erucic acid is 45.6%. Extended reaction times,When both conversion rate reach 90%. Compared with traditional method, the time of synthesis EAPDMA is only 33.33%.3. Under microwave irradiation, the optimum reaction conditions of quaternization reaction: Nitrogen protection, n(EAPDMA): n(CHPS-Na)=0.9:1,Temperature 90?, Solvent VIsopropanol:Vwater=1:2. time 40 min, microwave power500 W. The Tertiary amines of conversion rate is 80.2%. Under the same conditions,using traditional method to synthesis, Tertiary amines of conversion rate is 15.1%.Extended reaction times, When the two conversion rate reached 90%. Compared with traditional method, the time of synthesis EHSB was only 21.25%.4. Properties of EHSB aqueous solution: Krafft point below 0 ?. The CMC was1.38 × 10-4mol/L, surface tension was 16.0 mN/m. EHBS has good solubilization,foam stability and biodegradability. In kerosene-water system and Tetrachlorethylene-water system, EHSB has good Emulsifying properties. But its Foaming properties was poor.5. EHSB emulsion optimized conditions: example for formulating 100 g EHSB emulsion A(20%wt), acetic acid 10% of EHSB mass, 1305 20% of EHSB mass, The stability of the emulsion was well of high temperature resistance, salt performance,and alkali resistance. After 1 month at normal temperature, it was remained stable.EHSB in the range of 20%-50% of emulsion A remained had good stability.6. Application performance of EHSB Emulsion: fabric softness was well,hydrophilicity was quite well, resistance to yellowing just so so. Comparing withorganic silicon, D1821, LHSB, softness:organic silicon>EHSB>D1821>LHSB.resistance to yellowing: LHSB>D1821>EHSB>organic silicon. Hydrophilicity:LHSB > D1821 > EHSB > organic silicon. By SEM to observed fibers of the surfacemorphology, the results showed that had deal with the EHSB emulsion of the fibers, it would be more and more smooth than had no treated. Having treated 5 times,the smooth of fibers was outstanding.
Keywords/Search Tags:Hydroxyl sulfobetaine, Microwave systhesis, Erucic acid, Softener, Biodegradability, Hydrophilicity
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