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Synthesis?Structure Characterization And Properties Of Dehydroabietic Acid Sulphonate Bola Surfactants

Posted on:2014-12-21Degree:MasterType:Thesis
Country:ChinaCandidate:X J MaoFull Text:PDF
GTID:2311330485494979Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
This paper studied the preparation of a series of dehydroabietic acid sulphonate Bola surfactants, which were synthesized with disproportionated rosin as the main materials, and optimized the synthetic process conditions, characterized the products structures; the physicochemical properties and application performance of the products were also studied. The results were as follows:1. Dehydroabietic acid was separated and purified by ethanol amine amination in multiple crystallization, used the disproportionated rosin as the main materials. The products were characterized by IR, UV, GC, and also measured its melting point, acid value.2. Dehydroabietic acid fat glycol diesters were preparation with the esterification reaction by dehydroabietic acid and fat glycol. According to the results of single factor experiments, reacting conditions were optimized by the orthogonal experimentation and the response surface software. And got the optimum process conditions:n (dehydroabietic acid):n (ethylene glycol)= 2.4:1, temperature 250 ?,time 7 h, p-toluene sulfonic acid as the catalyst, its dosage was as the dehydroabietic acid amount 5%. The prepared products were confirmed by analysis of FT-IR.3. Using concentrated sulfuric acid and chlorosulfonic acid as sulfonation reagent with dehydroabietic acid fat glycol diesters to prepare dehydroabietic acid fat glycol diesters double sulfonate. According to the results of single factor experiments, orthogonal experimentation and the response surface software, the sulfonation reacting conditions were separately optimized, and got the optimum process conditions:Concentrated sulfuric acid as sulfonation reagent:the material proportion n (concentrated sulfuric acid):n (dehydroabietic acid ethylene glycol diesters)= 45:1, temperature 36 ?, time 7 h, solvent (CH2CI2) 15.0 mL.Chlorosulfonic acid as sulfonation reagent:the material proportion n (chlorosulfonic acid):n (dehydroabietic acid ethylene glycol diesters)= 5:1, temperature 15 ?, time 70 min, solvent (CH2C12) 15.0 mL.4. The structure of target products was confirmed by FT-IR, HPLC and13C NMR.5. The chemical and physical properties were studied of the critical mice concentration (cmc) values, the surface tension at their cmc (?Cmc) values, saturated extent of adsorption(??), Bola molecule cross-sectional area (A), characteristic conductivity, krafft point (KP), HLB values,nature of the particle size distribution, Micellar aggregation behavior, Ionic strength effect,and slso the application performances were measuredjust as emulsifying power (EP), foaming power (FP), lime soap dispersing power (LDSP) and calcium ion stability (CIS), anionic surfactant and cationic surfactant compatibility test.Results showed that these Bola surfactants have high surface activities, the ?cmc was the range of 42-47 mN·m-1, the first Ccmc value was 10"5 mol-L"1, and the second Ccmcwas 10-4 mol·L-1;the ?? is increaseed with the carbon chain growth, and the A is reduced accordingly; good water solubility and low Krafft point. The solution properties of surfactant solution were founded that as concentration increases, the micelle size increases gradually, from a single dispersed micelle structure to form chains, tubular structure of organized assemblies. The surface performance experimental data also showed that this kind of surfactants with strong emulsifying power, good foam stability and decentralization capacity of calcium soap bubble ability.
Keywords/Search Tags:dehydroabietic acid, diesters, sulphonation, Bola surfactants, propertie
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