The Study On Preparation Of Polyamide Polyamine Epichlorohydrin Grafting Funcrional Monomer And Its Application

Firstly, triethylenetetramine, tetraethylenepentamine or the polyethylene polyamine was used as the raw material to prepare the polyamide polyamine epichlorohydrin (PAE), and then, the fluorinated acrylate monomer was grafted onto PAE initiated by microwave radiation. By this way, the PAE-PFA was obtained. In this paper, the synthesis process for PAE and PAE-PFA, and the results were shown as followings,(1) The optimum conditions for preparing polyamide polyamine by adipate reacting with triethylenetetramine, tetraethylenepentamine or the polyethylene polyamine to was discussed. The results shows that the mole ratio of polyethylene polyamine and adipate was1:1at130-135℃for30min, and then it was moved to Condensate backflow at design temperature for2h. The extent for condensation polymerization could reach95%. The condensation polymerization was used as intermediate reacted at optimum condition, the viscidity was600-800cP, which is the good for polyamide polyamine epichlorohydrin resin.(2) The results for preparation of PAE was indicaded that the stability of the products was unstable at the mole rate of PPC and EPI below1.2, and the it could achieve the ideal effect at1.8. The experiments showed that the wet strength would decreased with the rate value of EPI and PPC increasing, and the rate value of EPI and PPC was1:3to be the optimum. The orthogonal analysis suggested that the temperature was the most influential condition; the reaction time was less, and rate for reactant and temperature rising were the least ones. Considering the stable and wet strength of PAE, the condition is EPI/PPC=1.3, the rate of temperature rising0.5℃/min, reaction temperature50℃, reaction time40min, and the viscidity of the products was40-46cP with solid content20%.(3) Via method of microwave radiation emulsion polymerization, the sizing agent, PAE-PFA, was obtained. The results shows:(a) it could be obtained the high yield at3%emulsifier; the yield of products could achieve90%at the power50W reacting4.5min; the15%of functional monomer was the optimal dosage.(b) the PDI would increase with the more emulsifier used and the increase of power of microwave radiation, but it decreased at200W.(c) the wrapping angle will be the maximum at4%emulsifier,10%functional monomer and50W for4.5min.The kinetic study on the synthesis of PAE-PFA by microwave was discussed. By univariate analysis, dosages of emulsifier, fluorine monomer and initiator were investigated, and the synthesis mechanism of PAE-PFA was studied. It was shown that the relation beyond reaction rate, emulsifier, fluorine monomer and initiator was follows the equation Rp∝[E]0.5525[I]0.4559[F]0.505, which indicaded the reaction conform to Smith-Ewart theory.FTIR and NMR were used, and it proved the functional group and structure of the product. The molecular weight and molecular weight distribution was analyzed by GPC. The molecular weight was48550and molecular weight distribution reached1.36, when conversion percent was97.1%. The linearity between In([M]0/[M]) and t showed that the ATRP reaction process is better controlled. glass transition temperature suggested the product was pure.The silicon material also has good oil-repellent, water-repellent and antifouling properties, so a novel silicon-containing fluorine anti-oil moisturizing strength agent could be prepared by the silicon and fluorine monomer reacted with PAE. The contant was as followings.(1) In this experiment, the new fluorine anti-oil containing humidifier strength agent was prepared by using the non-ionic emulsifier OP-10, ionic emulsifiers SDS, fluorinated emulsifier S200as the complex emulsifier, and the azobis isoheptyloxy nitrile as an initiator, methacrylic dodecafluoroheptanoyl ester (G04) as the fluorine-containing monomer, silicone macromolecules as silicon-containing monomers. The optimal process was3%PAE,1%azobis isoheptyloxy nitrile, fluorine-containing monomers/PAE1.5, and silicon-containing monomers/PAE2reacting6h at50℃. The wet strength of the product could reach to, and oil rating could be8.(2) The product, which wet strength and oil rating could reach20%and8, was used for coating paper. The coating paper, preparing at120℃for20min, with2.86g/m2～6.29g/m2of the product could meet the requirements of food packaging for anti-oil.