造纸黑液磺化改性及改性产物性能研究  

Sulphonation of Black Liquor and Properties of the Modified Product

作　　者：季栋[1] 马宏明[1] 何明[1] 史以俊[1] 罗振扬[1] 

机构地区：[1]南京林业大学理学院,江苏南京210037

出　　处：《林产化学与工业》2013年第1期85-90,共6页Chemistry and Industry of Forest Products

基　　金：国家自然科学基金资助项目(50903043;51005123);江苏省生物质能源与材料重点实验室项目(201001)

摘　　要：采取了先提木质素再将木质素磺化的方案进行造纸黑液的磺化,由分段正交试验(先羟甲基化再磺化)确定最佳磺化工艺,制备出磺化木质素。利用红外光谱表征产物,并测定了产物的磺化度、净浆流动度和重均分子质量(MW)。最佳磺化工艺:酸析木质素4 g,水40 g,甲醛溶液5 g,pH值11,75℃下反应2 h,再调pH值为7,加亚硫酸钠2 g于140℃下反应4 h,所得磺化木质素的净浆流动度为232 mm。红外分析表明磺化木质素中引入了较多的磺酸基;磺化木质素的磺化度为0.821 mmol/g,MW为22.97 ku,均优于市售木质素磺酸钠,从而导致水灰比值0.35时其净浆流动度亦优于同掺量下的木钠。The lignin in black liquor was firstly extracted first and then sulphonated in present study. The optimum sulphonation conditions were determined by staged orthogonal design （hydroxymethylation first, then sulphonation）. The sulphonated lignin （SL） was prepared. The product was characterized by FT-IR. Its sulphonation degree, paste fluidity, and weight-average molecular weight were measured respectively. After 4 g acid precipitated lignin in 40 g water reacted with 5 g formaldehyde at 75 ℃ for 2 h under the pH 11 environment, the pH of the system was adjusted to 7 and then 2 g sodium sulphite was added and reacted for another 4 h at 140 %. The optimal sulfonated lignin was obtained. FT-IR spectra showed that considerable sulphonic groups were introduced onto sulphonated lignin. The sulphonation degree and molecular weight of sulphonated lignin are 0.821 mmol/g and 22.97 ku, respectively. It was better than that of commercially available sodium lignosulphonate （SIS）. This indicated that the paste fluidity of sulphonated lignin was also greater at water-cement ratio of 0.35 and identical dosage.

关 键 词：造纸黑液 磺化 正交试验 重均分子质量 

分 类 号：TQ35[化学工程] O636.2[理学—高分子化学]