凝胶色谱用于磺甲基酚醛树脂生产控制方法研究

Studies on the production control method of sulfomethylated phenolic resin by gel permetion chromatophy

应用凝胶色谱-紫外检测法对SMP聚合生产过程中的原料单体、反应过程中生成的小分子、低聚物及最终产品进行了凝胶色谱分离与紫外图谱解析,研究建立了凝胶色谱用于磺甲基酚醛树脂生产控制的方法.研究表明,使用Sephadex G-10色谱柱,在0.01 mol/L的NaOH溶液为流动相、柱温35℃、流速1.0 mL/min等色谱条件下,大小分子的出峰时间分别为8.2 min与13.4 min,大小分子物质的分离比较彻底.利用凝胶色谱-紫外检测法分析苯酚类小分子凝胶色谱峰的位置变化和强度可以准确监控SMP生产中反应进行情况,小分子峰消失即为反应终点.该方法用于生产控制准确可靠,可以避免生产过程中过度磺化缩聚造成的分子量过高而水溶性降低或者反应不够充分造成的分子量过低、羟甲基含量高易热聚交联等现象,对于磺甲基化酚醛树脂工业化产品的质量控制具有重要意义.

A gel permeation chromatography method was developed for the production controlling of sulfomethylated phenolic resin （SMP）. The raw material monomers, small molecules, oligomers and the products produced in the reaction procession were separated by gel permeation chromatography and analyzed by UV. The separation was carried out on a Waters symmetry column （Sephadex G-10） with 0. 01 mol/L NaOH aqueous solution as mobile phase. The flow rate was 1. 0 mL/min, the column temperature was at 35 ℃. The retention times of big molecules and small molecular were at 8.2 min and 13. 4 min, respectively, and they were separated completely. The change of retention time and the peak intension of the small phenol molecules can be used to judge the reaction procession. The disappearance of the peak of small molecules showed the termination of the reaction. The use of this exact and dependable method can avoid the excess sulfonation and converge which resulted in molecular quantity ascend, solubility descend and more hydroxymethyl cross-linking phenomenon. The application of the method is of great significance for the effective quality control SMP.