湖北大学学报(自然科学版)
湖北大學學報(自然科學版)
호북대학학보(자연과학판)
2009年
4期
393-397
,共5页
刘清云%陈怀侠%聂敬忠%杨龙%文章%徐振辉
劉清雲%陳懷俠%聶敬忠%楊龍%文章%徐振輝
류청운%진부협%섭경충%양룡%문장%서진휘
凝胶色谱%紫外图谱解析%磺甲基化酚醛树脂%分离%分子量%质量控制
凝膠色譜%紫外圖譜解析%磺甲基化酚醛樹脂%分離%分子量%質量控製
응효색보%자외도보해석%광갑기화분철수지%분리%분자량%질량공제
gel permeation chromatography(GPC)%ultraviolet spectrum analysis%SMP%separation%molecular quantity%quality control
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.
應用凝膠色譜-紫外檢測法對SMP聚閤生產過程中的原料單體、反應過程中生成的小分子、低聚物及最終產品進行瞭凝膠色譜分離與紫外圖譜解析,研究建立瞭凝膠色譜用于磺甲基酚醛樹脂生產控製的方法.研究錶明,使用Sephadex G-10色譜柱,在0.01 mol/L的NaOH溶液為流動相、柱溫35℃、流速1.0 mL/min等色譜條件下,大小分子的齣峰時間分彆為8.2 min與13.4 min,大小分子物質的分離比較徹底.利用凝膠色譜-紫外檢測法分析苯酚類小分子凝膠色譜峰的位置變化和彊度可以準確鑑控SMP生產中反應進行情況,小分子峰消失即為反應終點.該方法用于生產控製準確可靠,可以避免生產過程中過度磺化縮聚造成的分子量過高而水溶性降低或者反應不夠充分造成的分子量過低、羥甲基含量高易熱聚交聯等現象,對于磺甲基化酚醛樹脂工業化產品的質量控製具有重要意義.
응용응효색보-자외검측법대SMP취합생산과정중적원료단체、반응과정중생성적소분자、저취물급최종산품진행료응효색보분리여자외도보해석,연구건립료응효색보용우광갑기분철수지생산공제적방법.연구표명,사용Sephadex G-10색보주,재0.01 mol/L적NaOH용액위류동상、주온35℃、류속1.0 mL/min등색보조건하,대소분자적출봉시간분별위8.2 min여13.4 min,대소분자물질적분리비교철저.이용응효색보-자외검측법분석분분류소분자응효색보봉적위치변화화강도가이준학감공SMP생산중반응진행정황,소분자봉소실즉위반응종점.해방법용우생산공제준학가고,가이피면생산과정중과도광화축취조성적분자량과고이수용성강저혹자반응불구충분조성적분자량과저、간갑기함량고역열취교련등현상,대우광갑기화분철수지공업화산품적질량공제구유중요의의.
A gel permeation chromatography method was developed for the production controlling of sulfomethylated phenolic resin(SMP).The raw material monomers,sinail 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 1 3.4 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.