混合醇醚化DMDHEU工艺研究

Research on the Process of Etherifying DMDHEU Resin with Mixed Alcohols

采用混合醇醚化DMDHEU树脂合成超低甲醛树脂.探讨了混合醇组成、混合醇用量、邻苯二甲酸酐用量、反应时间、反应温度和pH值对醚化后DMDHEU树脂性能的影响.通过测定和分析树脂中羟甲基含量、游离甲醛含量以及整理后织物的释放甲醛量、折皱回复角、撕破强力等,确定了较佳的混合醇醚化工艺：混合醇由66%二甘醇、17%乙二醇、17%甲醇组成,用量为DMDHEU用量的36%,邻苯二甲酸酐用量为混合醇用量的0.5%,反应温度70～72℃,反应时间4 h,pH值3.1~3.3,醚化后树脂的游离甲醛量低于0.4%,整理后织物上的释放甲醛量为37.6 mg/kg,折皱回复角较原布提高了100°以上,经向撕破强力保留率高于50%,综合性能优于用二甘醇醚化的DMDHEU树脂.

The process of synthesizing ultra-low formaldehyde resin by etherifying DMDHEU resin with mixed alco- hols is introduced. The effect of factors including the amount of varied alchols and phthalic anhydride, the reactive time, the reactive temperature and pH value on the etherified DMDHEU resin are discussed. The optimized process is determined by testing and analysing the hydroxymethyl contents, the free-formaldehyde contents of the resin, and the released formaldehyde contents, the wrinkle recovery angle and warp-wise strength preservation value of the fabric. The optimum condition of etherifying process is presented as follows ： Mixed alcohols are composed by 66% diethylene glycol, 17% glycol and 17% methanol, the amount of which is 36% to DMDHEU. The amount of the phthalic anhy- dride/total alcohols is 0.5% and the reactive temperature is 70-72 ~C, while the reactive time is 4 hours and pH value is 3.1~3.3. The free-formaldehyde of etherified resin is lower than 0.4%.The released formaldehyde of the finished fabric is reduced to 37.63 mg-kg-~,while the crease recovery angle improves more than 100°compared with original cloth and the warp-wise tearing strength retention is above 50%. The comprehensive performance of DMDHEU resin etherified with mixed alcohols is better than that of etherifying DMDHEU resin with diethylene glycol.