林产化学与工业
林產化學與工業
림산화학여공업
CHEMISTRY AND INDUSTRY OF FOREST PRODUCTS
2015年
4期
48-52
,共5页
卢燕凤%吴耿烽%曾常伟%李涛%吕建华%陈燕丹%黄彪
盧燕鳳%吳耿烽%曾常偉%李濤%呂建華%陳燕丹%黃彪
로연봉%오경봉%증상위%리도%려건화%진연단%황표
炭基%磷钨酸%催化%纤维素水解%纳米纤维素晶体
炭基%燐鎢痠%催化%纖維素水解%納米纖維素晶體
탄기%린오산%최화%섬유소수해%납미섬유소정체
carbon-based%phosphotungstic acid%catalysis%cellulose hydrolysis%nanocrystalline cellulose
以杉木屑为原料,采用原位合成法制备炭基磷钨酸催化剂,以此催化剂催化水解微晶纤维素制备纳米纤维素( NCC),考察了液料浸渍比、炭化温度及炭化时间等催化剂的制备因素对NCC得率的影响。结果表明:液料浸渍比2.5∶1(mL∶g),炭化温度350℃,炭化时间1.5 h条件下制备得到的炭基磷钨酸的催化性能较好,NCC得率可达25.28%。采用傅里叶红外光谱仪、热重分析及扫描电镜对炭基磷钨酸催化剂进行了表征,结果表明:磷钨酸较好地负载在炭材料上,炭基磷钨酸的Keggin结构特征吸收峰并未发生明显变化,磷钨酸Keggin结构开始分解的温度是370℃。用透射电子显微镜和X射线衍射仪对NCC的形貌、晶体结构进行了分析,结果表明:NCC呈棒状,直径9~70 nm,长度130~830 nm,平均长径比为11.2∶1,结晶度为76.1%,平均晶粒尺寸6.9 nm。
以杉木屑為原料,採用原位閤成法製備炭基燐鎢痠催化劑,以此催化劑催化水解微晶纖維素製備納米纖維素( NCC),攷察瞭液料浸漬比、炭化溫度及炭化時間等催化劑的製備因素對NCC得率的影響。結果錶明:液料浸漬比2.5∶1(mL∶g),炭化溫度350℃,炭化時間1.5 h條件下製備得到的炭基燐鎢痠的催化性能較好,NCC得率可達25.28%。採用傅裏葉紅外光譜儀、熱重分析及掃描電鏡對炭基燐鎢痠催化劑進行瞭錶徵,結果錶明:燐鎢痠較好地負載在炭材料上,炭基燐鎢痠的Keggin結構特徵吸收峰併未髮生明顯變化,燐鎢痠Keggin結構開始分解的溫度是370℃。用透射電子顯微鏡和X射線衍射儀對NCC的形貌、晶體結構進行瞭分析,結果錶明:NCC呈棒狀,直徑9~70 nm,長度130~830 nm,平均長徑比為11.2∶1,結晶度為76.1%,平均晶粒呎吋6.9 nm。
이삼목설위원료,채용원위합성법제비탄기린오산최화제,이차최화제최화수해미정섬유소제비납미섬유소( NCC),고찰료액료침지비、탄화온도급탄화시간등최화제적제비인소대NCC득솔적영향。결과표명:액료침지비2.5∶1(mL∶g),탄화온도350℃,탄화시간1.5 h조건하제비득도적탄기린오산적최화성능교호,NCC득솔가체25.28%。채용부리협홍외광보의、열중분석급소묘전경대탄기린오산최화제진행료표정,결과표명:린오산교호지부재재탄재료상,탄기린오산적Keggin결구특정흡수봉병미발생명현변화,린오산Keggin결구개시분해적온도시370℃。용투사전자현미경화X사선연사의대NCC적형모、정체결구진행료분석,결과표명:NCC정봉상,직경9~70 nm,장도130~830 nm,평균장경비위11.2∶1,결정도위76.1%,평균정립척촌6.9 nm。
Carbon-based phosphotungstic acid ( H3 PW12 O40 ) catalyst was prepared from sawdust of Chinese fir by in-situ synthesis. Nanocrystalline cellulose ( NCC) from cellulose by catalytic hydrolysis was studied. The effects of impregnation ratio, carbonization temperature and carbonization time on the yield of NCC were also analyzed. The results showed that under the impregnation ratio of liquid to solid 2. 5∶1, thecarbonization temperature 350 ℃ and carbonization time 1. 5 h, a comparatively high yield of NCC was observed as 25. 28%. The catalysts were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, and scanning electron microscope. The results indicated that phosphotungstic acid was loaded on the carbon under good conditions, the keggin structure characteristic absorption peak of carbon-based phosphotungstic acid remains stable, and the initial decomposition temperature of keggin structure of phosphotungstic acid is 370 ℃. The morphological and crystal structures of NCC were carried out by Transmission electron microscopy and X-ray diffraction. The results showed that the NCC observed by TEM turned out to be rod-like, with the size of 9-70 nm in width and 130-830 nm in length and the average aspect ratio of 11. 2∶1. X-ray diffraction analysis revealed that the crystallinity of the NCC was 76. 1%, with the average particle size of 6. 9 nm.