南京林业大学学报（自然科学版）
南京林業大學學報（自然科學版）
남경임업대학학보（자연과학판）
JOURNAL OF NANJING FORESTRY UNIVERSITY(NATURAL SCIENCE EDITION)
2015年
3期
113-118
,共6页
李韵卒%杨益琴%杨勤武%顾俐慧%王志国
李韻卒%楊益琴%楊勤武%顧俐慧%王誌國
리운졸%양익금%양근무%고리혜%왕지국
纤维素%己内酯%开环聚合%接枝%钛酸正丁酯
纖維素%己內酯%開環聚閤%接枝%鈦痠正丁酯
섬유소%기내지%개배취합%접지%태산정정지
cellulose%caprolactone ( CL)%ring-opening polymerization%graft%Ti( O-n-Bu) 4
以棉浆粕为原料，通过钛酸正丁酯（ Ti（ O－n－Bu）4）催化己内酯开环聚合接枝纤维素制备纤维素聚己内酯。通过单因素实验和正交试验研究了反应温度、反应时间、催化剂用量及己内酯用量对纤维素接枝率和己内酯转化率的影响。结果表明：反应温度是影响接枝率的主要因素，其次是己内酯用量，反应时间的影响最小。当反应温度为130℃、己内酯与纤维素的质量比为30、催化剂质量分数为2％（聚己内酯理论聚合度为37）、反应时间25 h时，己内酯的转化率和纤维素－聚己内酯的接枝率最高，分别为97．46％、70．44％。采用FTIR、1 H－NMR、XRD对产物进行了结构和性能表征，红外光谱分析表明，纤维素与聚己内酯发生了接枝共聚反应；1 H－NMR分析表明，己内酯已基本转化为聚己内酯，根据计算可知己内酯转化率与重量法测定结果一致；X－射线衍射图谱显示纤维素共聚物中纤维素的结晶结构特征减弱，出现了聚己内酯的结晶特征峰。
以棉漿粕為原料，通過鈦痠正丁酯（ Ti（ O－n－Bu）4）催化己內酯開環聚閤接枝纖維素製備纖維素聚己內酯。通過單因素實驗和正交試驗研究瞭反應溫度、反應時間、催化劑用量及己內酯用量對纖維素接枝率和己內酯轉化率的影響。結果錶明：反應溫度是影響接枝率的主要因素，其次是己內酯用量，反應時間的影響最小。噹反應溫度為130℃、己內酯與纖維素的質量比為30、催化劑質量分數為2％（聚己內酯理論聚閤度為37）、反應時間25 h時，己內酯的轉化率和纖維素－聚己內酯的接枝率最高，分彆為97．46％、70．44％。採用FTIR、1 H－NMR、XRD對產物進行瞭結構和性能錶徵，紅外光譜分析錶明，纖維素與聚己內酯髮生瞭接枝共聚反應；1 H－NMR分析錶明，己內酯已基本轉化為聚己內酯，根據計算可知己內酯轉化率與重量法測定結果一緻；X－射線衍射圖譜顯示纖維素共聚物中纖維素的結晶結構特徵減弱，齣現瞭聚己內酯的結晶特徵峰。
이면장박위원료，통과태산정정지（ Ti（ O－n－Bu）4）최화기내지개배취합접지섬유소제비섬유소취기내지。통과단인소실험화정교시험연구료반응온도、반응시간、최화제용량급기내지용량대섬유소접지솔화기내지전화솔적영향。결과표명：반응온도시영향접지솔적주요인소，기차시기내지용량，반응시간적영향최소。당반응온도위130℃、기내지여섬유소적질량비위30、최화제질량분수위2％（취기내지이론취합도위37）、반응시간25 h시，기내지적전화솔화섬유소－취기내지적접지솔최고，분별위97．46％、70．44％。채용FTIR、1 H－NMR、XRD대산물진행료결구화성능표정，홍외광보분석표명，섬유소여취기내지발생료접지공취반응；1 H－NMR분석표명，기내지이기본전화위취기내지，근거계산가지기내지전화솔여중량법측정결과일치；X－사선연사도보현시섬유소공취물중섬유소적결정결구특정감약，출현료취기내지적결정특정봉。
Cellulose polycaprolactone was prepared by grafting of cotton linter pulp with caprolactone ( CL) catalyzed by Ti( O-n-Bu) 4 via ring?opening polymerization. Effects of reaction temperature, reaction time, Ti( O-n-Bu) 4 amount, and caprolactone ( CL) on monomer conversion and graft rate were investigated through single factor experiments and or?thogonal test. The results showed that the significance sequence of the factors affecting the grafting rate was reaction tem?perature, mass ratio of CL to cellulose, and reaction time. The optimal reaction conditions were as follows:the amount of catalyst was 2% ( PCL theory degree of polymerization was 37) , the mass ratio of CL to cellulose was 30, and the graft polymerization was carried out at 130 ℃for 25 h. At aforesaid conditions, conversion of CL reached 97. 46% and graft rate of cellulose was 70.44%. Structure and properties were characterized by FTIR, 1 H-NMR, XRD. The FTIR result confirmed cellulose has been grafted with PCL. The 1 H-NMR analysis showed that most of the CL had transformed into PCL, and the calculated CL conversion according to 1 H-NMR was consistent with the result of weight measurement method. The XRD results showed that cellulose crystalline structure in cellulose?PCL has decreased, instead crystalline characteristic peaks of PCL was appeared.
