Study On Synthesis And Properties Of Rosin-based Phosphate

In this dissertation phosphate anionic surfactant was synthesized byphosphorylating polyoxyethylene abietate(PA). Phosphorylating agent was P2O5 there.PA was prepared from disproportionated rosin and ethylene oxide(EO). The structuresof phosphate polyoxyethylene abietate (PPA) was identified by IR.PA was first synthesized: Addition reaction of disproportionated rosin and EOwas performed in the condition of catalyst. Through the study of the influence ofreaction factors such as temperature, calalyst amount. The suitable syntheticconditions were as follow: reaction temperature was 180℃, calalyst amount was3.6%(based on total materials(mol)). Reaction between carboxyl of thedisproportionated rosin and EO had taken place, which was confirmed by IR. Therelations between physical properties of polyoxyethylene abietate(PA) andpolymerization degree of EO(n) were also studied. With the increasing ofpolymerization degree of EO, the color of the products be darken gradually; theviscosity was lowering first, then rising; The content of polyglycol was increasing; theyield of monoester and the hydroxyl value of products were dropping.PA was esterified by phosphorus pentoxide and created PPA under nitrogenatmosphere in this stage. Then water would be used to hydrolyze the reaction products.The effects on the ratio of raw materials, the reaction time and temperature, thefeeding way of phosphorus pentoxide were investigated respectively. The optimumesterifying conditions as below: PA/ P2O5 =2:1 (mol/mol); reaction temperature was80 ℃; reaction time was 6 h; P2O5 was feeded at batches. The optimum hydrolyticconditions also be determined: amount of adding water was 4 %(g/g); reactiontemperature was 60 ℃; reaction time was 3 h. The products PPA could be neutralizedby alkali according to vary demands.In this paper the contents of mono-, diester in phosphate products were measuredthrough potentiometric titration. The kinds and ratios of solvent, the solvent andconcentration of titrant along with the other additives were discussed respectrively.The optimum analytic conditions were obtained: 50 % ethanol as solvent, 0.25 mol?L-1NaOH(H2O) as titrant, dosage of 10 % CaCl2 and saturated NaCl solubtion were4～7 mL and 4～6 mL respectively. i王艳娜:松香基磷酸酯的合成及性能研究 2004 年 5 月The relations between surface physicochemical properties of the products andpolymerization degree of EO were studied. With the increasing of polymerizationdegree of EO(n), surface tension(δ) and emulsifying power(EP)went up; criticalmicelle concentration(CMC) and wetting power(WP) declined; foaming power(FP)changed a little; Karfft(KP) was below zero.Finally application experiments on emulsification and antiemusification of theproducts were also studied. It was found that PPA-15, PPA-20(n=15, 20) had betteremulsifying efficiency, and antimulsifying property of PPA-10(n=10) was better thanothers for higher ratio of dehydration.