杉木屑干馏及干馏产物组成的研究
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摘要
以杉木屑为原料,采用干馏法制备杉木油,分别得到干馏油、木醋液、焦油和木炭,产率分别为4.0%、38.0%、14.3%、28.8%,除此之外还得到不凝性可燃气,产率为15.0%。对杉木屑干馏油、木醋液和不凝性气体的性质、组成进行研究,结果发现:杉木屑的固液产品总转化率达到了80%以上;杉木干馏油的主要组成为α-柏木烯29.36%、β-柏木烯11.87%、柏木醇12.10%等;木醋液的主要成分为1-甲基亚乙基环己烷24.07%、乙酸19.77%、4-乙基愈创木酚11.71%、糠醛8.06%等;不凝性可燃气主要由H_2、CO和CH_4组成。
Essential fir oil was prepared by destructive distillation using Chinese fir chips as raw material. The yields of destructive distillation oil,wood vinegar,tar and charcoal were 4. 0%,38. 0%,14. 3% and 28. 8%,respectively. Noncondensable flammable gas was also generated during destructive distillation,the yield of gas was 15. 0%. The property and composition of destructive distillation oil,wood vinegar and non-condensable gas were studied. The results showed that all of the fir chips were converted into products with conversion rate over 80%. The compositions of destructive distillation oil wereα-cedrene 29. 36%,β-cedrene 11. 87%,cedrol 12. 10%,etc. The main organic components of the vinegar were 1-methylethylidene-cyclohexane 24.07%,acetic acid 19.77%,4-ethylguaiacol 11.71%,furfural 8.06%,etc. Main components of noncondensable combustible gas were H_2,CO and CH_4.
Essential fir oil was prepared by destructive distillation using Chinese fir chips as raw material. The yields of destructive distillation oil,wood vinegar,tar and charcoal were 4. 0%,38. 0%,14. 3% and 28. 8%,respectively. Noncondensable flammable gas was also generated during destructive distillation,the yield of gas was 15. 0%. The property and composition of destructive distillation oil,wood vinegar and non-condensable gas were studied. The results showed that all of the fir chips were converted into products with conversion rate over 80%. The compositions of destructive distillation oil wereα-cedrene 29. 36%,β-cedrene 11. 87%,cedrol 12. 10%,etc. The main organic components of the vinegar were 1-methylethylidene-cyclohexane 24.07%,acetic acid 19.77%,4-ethylguaiacol 11.71%,furfural 8.06%,etc. Main components of noncondensable combustible gas were H_2,CO and CH_4.
引文
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[16]SELIM S A,ADAM M E,HASSAN S M,et al. Chemical composition,antimicrobial and antibiofilm activity of the essential oil and methanol extract of the Mediterranean cypress(Cupressus sempervirens L.)[J]. BMC Complementary&Alternative Medicine,2014,14(1):179.
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[18]孙凌峰,陈新,刘秀娟,等.杉木根精油化学成分研究[J].江西师范大学学报:自然科学版,2000,24(1):45-49.SUN L F,CHEN X,LIU X J,et al. Studies on chemical constituents of the essential oil from the root of Cunninghamia lanceolata[J]. Journal of Jiangxi Normal University:Natural Sciences Edition,2000,24(1):45-49.
[19]HUANG L H,QIN T F,TATSURO O. Studies on preparations and analysis of essential oil from Chinese fir[J]. Journal of Forestry Research,2004,15(1):80-82.
[20]朱凯,曹少元,陈科.杉木油的提取及干馏油的精制[J].农业工程学报,2012,28(9):282-286.ZHU K,CAO S Y,CHEN K. Extraction of Chinese fir wood oil and refinement of pyroligneous oil[J]. Transactions of the Chinese Society of Agricultural Engineering,2012,28(9):282-286.
[21]朱凯,陈科.杉木根的干馏及干馏可燃气的组成[J].农业工程学报,2011,27(S2):135-138.ZHU K,CHEN K. Fir root dry distillation and composition of combustible gases[J]. Transactions of the Chinese Society of Agricultural Engineering,2011,27(S2):135-138.
[22]马莉,陈君,朱凯,等.墨西哥柏精油的提取及成分分析[J].林业工程学报,2016,1(3):63-67.MA L,CHEN J,ZHU K,et al. Extraction and component analysis of Cupressus lusitanica essential oil[J]. Journal of Forestry Engineering,2016,1(3):63-67.
[23]KATO Y,ENOMOTO R,AKAZAWA M,et al. Characterization of Japanese cedar bio-oil produced using a bench-scale auger pyrolyzer[J/OL]. Springerplus,2016,5:1-11[2018-03-16].https:∥link.springer.com/content/pdf/10.1186%2Fs40064-016-1848-7.pdf.
[24]FLETCHER T L,HARRIS E E. Destructive distillation of Douglas fir lignin[J]. Journal of the American Chemical Society,1947,69(12):3144-3145.
[2]胡铁,谷政伟,钟雄,等.杉木屑精油提取工艺及成分分析[J].湖北农业科学,2014,53(14):3387-3390.HU T,GU Z W,ZHONG X,et al. Extraction and analyses of essential oil from sawdust of Cunninghamia lanceolata[J]. Hubei Agricultural Sciences,2014,53(14):3387-3390.
[3]沈琦,王敏,艾宁,等.农林废弃物成分分析及其综合利用前景展望[J].可再生能源,2009,27(1):58-61.SHEN Q,WANG M,AI N,et al. Component analysis and prospects for comprehensive utilization of agricultural and forestry wasters[J].Renewable Energy Resources,2009,27(1):58-61.
[4]HUBER D P W,PHILIPPE R N,GODARD K A,et al. Characterization of four terpene synthase c DNAs from methyl jasmonate-induced Douglas-fir,Pseudotsuga menziesii[J]. Phytochemistry,2005,66(12):1427-1439.
[5]朱凯.杉木废弃物提取精油及柏木系香料的合成[C]∥2013(第九届)中国日用化学工业论坛论文集.南京:南京林业大学,2013:42-49.ZHU K. Synthesis of essential oil from Chinese fir waste and cedar flavor[C]∥2013(9th)China Daily Chemical Industry Forum Proceedings.Nanjing:Nanjing Forestry University,2013:42-49.
[6]ADAMS R P. Cedar wood oil:Analyses and properties[J]. Modern Methods of Plant Analysis,1991,12(7):159-173.
[7]周文富,黄忠兴,徐芃,等.杉根精油分离及其化学成分测定[J].精细化工,2007,24(11):1095-1098.ZHOU W F,HUANG Z X,XU F,et al. Determination of chemical constituents of the essential oil from the root of Cunninghamia lanceolata[J].Fine Chemicals,2007,24(11):1095-1098.
[8]程健,曾韬,杨彦春.杉木根干馏油提取杉木精油及化学成分分析[J].林产化学与工业,2007,27(S1):65-68.CHENG J,ZENG T,YANG Y C. Analysis of Cunninghamia essential oil distillated from pyroligneous oil of Cunninghamia lanceolata(Lamb.)Hook[J]. Chemistry and Industry of Forest Products,2007,27(S1):65-68.
[9]马莉,吴光耀,陈君,等.二氧化硅负载磷钨酸催化罗汉柏木烯的异构反应[J].林业工程学报,2017,2(6):60-66.MA L,WU G Y,CHEN J,et al. Silica-supported phosphotungstic acids catalyze isomerization reaction of thujopsene[J]. Journal of Forestry Engineering,2017,2(6):60-66.
[10]黄克瀛,王美其.用柏木油合成柏木酮的研究[J].林产化工通讯,1996,30(2):10-11.HUANG K Y,WANG M Q. Study on synthesis of cedarin with cedar oil[J]. Chemical Communication of Forest Products,1996,30(2):10-11.
[11]陈华成.环氧柏木烷的合成研究[D].南京:南京林业大学硕士学位论文,2006.CHEN H C. Study on the synthesis ofα-epoxycedrane[D]. Nanjing:Master Degree Thesis of Nanjing Forestry University,2006.
[12]童娟,唐健.乙酸柏木酯的合成研究[J].化工技术与开发,2002,31(3):5-7.TONG J,TANG J. Study on synthesis of cedryl acetate[J]. Technology&Development of Chemical Industry,2002,31(3):5-7.
[13]曹双喜,杨兵.柏木油化学成分的分析研究[J].湖南化工,1998(5):43-44.CAO S X,YANG B. An investigation on the chemical composition for cedar wood oil[J]. Hunan Chemical Industry,1998(5):43-44.
[14]TUNALIER Z,KIRIMER N,KHC B. A potential new source of cedarwood oil:Juniperus foetidissima Willd.[J]. Journal of Essential Oil Research,2004,16(3):233-235.
[15]陈科.杉木根精油提取及深加工研究[D].南京:南京林业大学硕士学位论文,2010.CHEN K. Study on essential oil extracted from Chinese fir root and deep-processing[D]. Nanjing:Master Degree Thesis of Nanjing Forestry University,2010.
[16]SELIM S A,ADAM M E,HASSAN S M,et al. Chemical composition,antimicrobial and antibiofilm activity of the essential oil and methanol extract of the Mediterranean cypress(Cupressus sempervirens L.)[J]. BMC Complementary&Alternative Medicine,2014,14(1):179.
[17]王玉,王小东,黄慧.木醋液的研究进展[J].安徽林业科技,2015,41(5):12-15.WANG Y,WANG X D,HUANG H. Research progress on wood vinegar[J]. Anhui Forestry Science and Technology,2015,41(5):12-15.
[18]孙凌峰,陈新,刘秀娟,等.杉木根精油化学成分研究[J].江西师范大学学报:自然科学版,2000,24(1):45-49.SUN L F,CHEN X,LIU X J,et al. Studies on chemical constituents of the essential oil from the root of Cunninghamia lanceolata[J]. Journal of Jiangxi Normal University:Natural Sciences Edition,2000,24(1):45-49.
[19]HUANG L H,QIN T F,TATSURO O. Studies on preparations and analysis of essential oil from Chinese fir[J]. Journal of Forestry Research,2004,15(1):80-82.
[20]朱凯,曹少元,陈科.杉木油的提取及干馏油的精制[J].农业工程学报,2012,28(9):282-286.ZHU K,CAO S Y,CHEN K. Extraction of Chinese fir wood oil and refinement of pyroligneous oil[J]. Transactions of the Chinese Society of Agricultural Engineering,2012,28(9):282-286.
[21]朱凯,陈科.杉木根的干馏及干馏可燃气的组成[J].农业工程学报,2011,27(S2):135-138.ZHU K,CHEN K. Fir root dry distillation and composition of combustible gases[J]. Transactions of the Chinese Society of Agricultural Engineering,2011,27(S2):135-138.
[22]马莉,陈君,朱凯,等.墨西哥柏精油的提取及成分分析[J].林业工程学报,2016,1(3):63-67.MA L,CHEN J,ZHU K,et al. Extraction and component analysis of Cupressus lusitanica essential oil[J]. Journal of Forestry Engineering,2016,1(3):63-67.
[23]KATO Y,ENOMOTO R,AKAZAWA M,et al. Characterization of Japanese cedar bio-oil produced using a bench-scale auger pyrolyzer[J/OL]. Springerplus,2016,5:1-11[2018-03-16].https:∥link.springer.com/content/pdf/10.1186%2Fs40064-016-1848-7.pdf.
[24]FLETCHER T L,HARRIS E E. Destructive distillation of Douglas fir lignin[J]. Journal of the American Chemical Society,1947,69(12):3144-3145.