Synthesis Of Novel Tertiary Amine Salt Polymeric Decolorizing Flocculant And Application In Regeneration Of Waste Lubricating Oil

With the increase of global lubricating oil consumption，large amount of wastelubricating oil is produced consequently. Fortunately，waste lubricant can be recycled andregenerated as a useful resource，which attached much significant importance to the resourcesaving，environment protection，economic benefits and society merits. Polymeric flocculanthas been widely applied as a purification agent in waste water treatment and waste oilreclaiming pre-treatment stage owing to its small usage but high flocculation efficiency.Herein，a novel tertiary amine salt polymeric decolorizing flocculant was prepared via aneutralization modification of poly(N,N-Dimethylaminoethyl methacrylate)(PDMAEMA).The waste oil was regenerated by combining three main techniques: distillation-sulfuricrefining-flocculation refining. The flocculation refining was adopted to replace the traditionalclay refining，aimed at reducing the waste sludge yield and removing the secondary pollution.This study is divided into four parts as follows.Part one: the waste oil was treated by distillation with adding mixed bases. The effectsof factors such as the adding means，the concentration ratio and total mass concentration andquantity of the mixed bases(potassium hydroxide and sodium hydroxide) on the yield ratioand the properties of the distillation fractionations were investigated. An optimum operationcondition has been obtained. The chemical structures of the waste oil and the red distillationoil were characterized by Infrared spectroscopy (FT-IR).Part two: the red oil was treated with sulfuric refining and flocculating refiningcombined. The yield of acid sludge，the yield of acid oil，the color，acid number，lighttransmittance of the acid oil and the flocculating oil were proposed as refining indexes. Aninteraction orthogonal designing L2（7313）and single-factor experiments were used to examinethe effects of sulfuric refining operation variables such as sulfuric acid content，thetemperature，the stirred time and the sedimentation time on the indexes. An optimum sulfuricrefining condition related to flocculating refining technique has been achieved. The chemicalstructures of the red distillation oil，the acid oil and the waste oil were characterized byFT-IR.Part three: A homopolymer called poly(N,N-Dimethylaminoethyl methacrylate)(PDMAEMA) was prepared in a solution polymerization method with radicalpolymerization mechanism by using the N,N-Dimethylaminoethyl methacrylate(DMAEMA)as monomer，Azobisisobutyronitrile（AIBN）as indicator and the ethanol as solvent. Anorthogonal designing L16(45) and single-factor experiments were adopted to investigate theeffects of the homopolymerization factors including the indicator content，the monomer massconcentration，the reaction temperature and the reaction time on the compsitions andflocculating properties of the flocculant. An optimum condition to synthesize thehomopolymer has been determined according to its flocculating effect. The relationshipbetween the viscosity and concentration of PDMAEMA in ethanol solution was studied. Thechemical structure of the PDMAEMA was characterized by FT-IR and1H-NMR(NuclearMagnetic Resonance).Part four: the tertiary amine polymeric decolorizing flocculantpoly(N,N-Dimethylaminoethyl methacrylate-oleic acid) salt (PDMAEMA-Oleic acid) wassynthesized by using the oleic acid to neutralize the weak basic groups on the water solublehomopolymer chain and its applied operations were explored. The neutralization factorsincluding the neutralization time， the neutralization temperature，the neutralization degreen(oleic acid):n(DMAEMA) and the neutralization mass concentration on the structures andthe properties of the flocculant as well as the effects of the flocculant usage，the flocculantsolution concentration，the centrifugal speed，the centrifugal time and the base oil addictiveswere examined on the decolorizing and flocculating the acid oil. A comparison of theflocculating refining and the clay refining was conducted according to the process andproperties of both the base oil products. The optimum operation variables to prepare andapply the tertiary amine salt polymeric flocculant have been determined. The chemicalstructure of the PDMAEMA-Oleic acid was characterized by FT-IR and1H-NMR.