| Through N-alkylation reaction using p-Aminophenyl-β-sulfatoethylsulfone(Para-ester)and 3-chloropropene as raw materials, a new temporary water-soluble polymerizable monomer of para-ester series was prepared, which can be used to prepare temporary water-soluble polymer taken off sulfonic esters. The influence of solvent,deacid reagent,pH,raw material molar ratio,reaction temperature,reaction time on raw material para-ester’s N-alkylation rate and product’s solubility in water was studied.The content of Cl- in water was measured by Mohr methord and IC to calculate raw material para-ester’s N-alkylation rate.And the content of carbon-carbon double bond of monomers was measured by Bromine method. The results showed that when water is uesd as solvent,the material proportion of3-chloropropene and para-ester is 2:1,the temperature of reaction is 60 ℃,the pH is controled at 7,the reaction time is 8h,raw material para-ester’s N-alkylation rate reached 98.40 % and the product’s solubility in water is very well. The Thin Layer Chromatography was used to find out the best developing agent before Column Chromatography which could isolate pure products.Through 14 kinds of solvents from 4 kinds,with uniform design method, single factor experiment method and orthogonal experiment method, a set of expanding agent system was optimized:V(methyl alcohol):V(1,2-dichloroethane):V(chloroform)=1:1:1.This method could reach a good substitute of N- alkylation And separate the pure product through the column chromatography.The structure of the raw materials and product was characterized by FT-IR, HPLC-MS and IC. The results of Infrared spectra〠MS spectra and IC spectra showed that the product’s structure is consistent with the expected results and the product’s solubility in water maintained well.Study on the stability of sulfate groups and the method of alkali sulfate removal of temporary water-soluble polymerizable monomer of para-ester series.Synthetic good water dispersible resin of the ester series.In the wake of the global warming and the ozone layer’s being destroyed, the requirement of industrial environmental protection in the world has become increasingly strict.Organic volatile matter(VOC),which is used in the coating process,has a negative effect on climate warming.For automotive coatings industry,the use of VOC in the coatingprocess has been strictly required.Among them,the most effective way to reduce VOC is water solubility.In this paper,for the first time the 3-chloropropene and para ester was used as raw material,water was used as reaction mediumthe reaction medium to prepare the polymer monomer with water soluble property. At present,there is no report on the synthesis and application of water soluble polymer monomers in coatings industry.If the forecast preparation process of its application in automotive finishes,emissions of VOC can be greatly reduced.And because of the removal of temporary water soluble functional groups of sulfate,it will lose water solubility,can make up for the lack of water-based paint performance,which could give topcoat more excellent performance. |
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