以桉木为原料制备醋酸纤维的研究
摘要
醋酸纤维用途广泛,所用原料为高纤维素含量的棉浆或高级针叶木浆粕,而目前木浆粕仍需进口。研究开发木浆粕,己成为我国醋酸纤维行业能否实现可持续性发展的关键问题,桉木作为一种重要的速生阔叶材种,如能用于生产纯度高的醋酸纤维浆粕,对我国醋酸纤维工业具有重要的意义。
论文以尾叶桉为原料,研究了制浆、漂白、木聚糖酶处理和碱精制工艺,得到了满足醋酸纤维要求的浆粕,再进行活化、醋酸化、水解等处理,并对其反应机理进行了探讨。实验的主要结果如下:
(1)桉木浆粕采用KP+AQ法制得,条件为:用碱量17%(Na_2O计),硫化度16%,AQ 0.05%,液比1:4,空转30 min,升温90 min至130℃;再次升温90 min至170℃,保温60 min。
(2)为了得到高白度浆粕,又不造成环境污染,对D_1ED_2常规漂白条件进行了探讨,D_1段用氯量必须控制在3.6%以内;碱处理的条件需要强烈些,以去除半纤维素,提高浆粕的α-纤维素含量和平均平均聚合度。但是想要通过提高用碱量来大幅提高α-纤维素含量是不可行的。桉木制醋酸纤维浆粕的漂白条件为:D_1段用氯量3.6%,70℃,90 min,浆浓10%,pH 3.5;E段NaOH 2.0%,75℃,60 min,浆浓10%;D_2段用氯量0.9%,70℃,90 min,浆浓10%,pH 3.5;P段NaOH用量与H_2O_2用量一致为2.5%,70℃,90 min,浆浓10%。
(3)木聚糖酶处理最佳条件为:酶用量120 IU/g,60℃,时间2h,浆浓3%,pH6.0;碱精制中,NaOH除了可以去掉部分半纤维素,而且可以溶解掉部分短链纤维素,当碱浓度为4%时,平均聚合度增至1163,白度增至90.0%,α-纤维索含量为96.78%,达到了醋酸纤维浆粕国际标准。
(4)对木聚糖酶处理前后的浆粕进行红外扫描。发色基团和助色基团如C=O伸展振动(1058cm~(-1))、木素-烷基醚基C-O-C伸展振动(1164cm~(-1))、芳基-烷基醚键(1240cm~(-1))、木素羰基伸展振动C=O(1637cm~(-1))、木素芳环振动(1430 cm~(-1))处的吸收峰在木聚糖酶处理后,强度有所减弱,这或许是木聚糖酶处理后浆粕白度提高的原因。
(5)桉木浆粕最佳活化条件:活化时间为3.0 h、活化温度50℃,醋酸用量为500%;醋酸化最佳条件为:醋酸酐用量400%,催化剂硫酸用量7.5%,温度60℃,时间2h;水解最佳条件为:醋酸含量为80%,水解温度为60℃,制得醋酸纤维取代度为2.51。
(6)对活化后的浆粕进行X-射线衍射扫描,并结合红外图谱。活化处理仅仅是一个物理溶胀的过程,确实改变了纤维素的结晶结构,使得可及区增加,有更多的羟基为醋酸化剂可及,有利于醋酸化反应的进行,用醋酸对浆粕的活化处理,为醋酸化做足准备,其他并无明显化学反应发生。
(7)对醋酸纤维红外扫描。1752cm~(-1)为C=O的伸缩振动,3348 cm~(-1)为-OH伸缩振动,其强度明显减弱,说明浆粕醋酸化产物的主要成分是醋酸纤维;对醋酸纤维进行X-射线衍射扫描,醋酸化使纤维素氢键作用减弱,同时醋酸基的引入使纤维素结晶结构受到一定程度的破坏,从而导致纤维素结晶度的降低。
Cellulose acetate is used widely,its raw materials is cotton of high-cellulose content or senior coniferous wood pulp,which is needed to import from abroad.Therefore,the research and development of wood pulp become the key issues of sustainable development of cellulose acetate,Eucalyptus is an important fast-growing hardwood species,which has importance to ease the cellulose acetate industry in China.
Eucalyptus is studied as raw materials in this paper,including pulping、bleaching、xylanase and alkaline purification process,the product meet the requirements of cellulose acetate pulp,and then activation、acetic anhydirde、hydrolysis process and its mechanism explore.The main experimental results:
(1) The pulp is cooked by means of KP+AQ,conditions:alkaline 17%(Na_2O),sulphidity 16%,AQ 0.05%,liquid ratio 1:4,idling about 30 min,heating to 130℃within 90min;then warming up to 170℃in 90min,holding temperature about 60min.
(2) In order to increase brightness without causing environmental pollution,it's needed to research the conditions of D_1ED_2 conventional bleaching,the amount of chlorine must be controlled within 3.6% at D_1 stage;in order to improve a-cellulose content and degree of polymerization,alkaline conditions is needed more stronger to remove the hemicellulose.But it is not feasible to increase a-cellulose content by increasing the amount of alkaline.Eucalyptus wood pulp bleaching conditions for cellulose acetate: D_1,the amount of chlorine 3.6%,70℃,90 min,plup consistence 10%,pH 3.5;E paragraphs NaOH 2.0%,75℃,60 min,pulp concentration 10%;D_2,the amount of chlorine 0.9%,70℃,90 min,plup consistence 10%,pH 3.5;P,the amount of NaOH and H_2O_2 are the same amount of 2.5%,70℃,90 min, plup consistence 10%.
(3) Pulp's xylanase purification conditions:enzyme dosage 120 IU/g,60℃,time 2h,plup consistence 3%,pH 6.0.Alkali purification,NaOH can not only remove part of hemicellulose,also dissolve some short-chain cellulose,when the alkali consistence is 4%,the degree of polymerization 1163,brightness 90.0%,a-cellulose content 96.78%,cellulose acetate pulp achieve international standards.
(4) Scanning the pulp before and after purification treatment by 1R.It's found that:the chromophoric group and color auxochrome group,such as the C=O stretching vibration(1058cm~(-1)), lignin-alkyl ether-based C-O-C stretching vibration(1164cm~(-1)),aryl-alkyl ether bond(1240cm~(-1)), lignin carbonyl stretching vibration C=O(1637cm~(-1)),lignin aryl ring vibration(1430 cm~(-1)),their absorption peak intensity has weakened after purification,and this is why the pulp's brightness increased after purificationt.
(5) The activation of eucalyptus pulp's conditions:time 3.0 h,temperature 50℃,the amount of acetic acid 500%;acetic anhydride conditions:the amount of acetic anhydride 400%,the amount of catalyst sulfate 7.5%,temperature 60℃,time 2.0 h;the hydrolysis conditions:80%acetate content, temperature 60℃,degree of substitution of CA is 2.51.
(6) Scanning pulp before and after activation by means of X-ray diffraction and IR.The activation is just a physical process,change the crystalline structure of cellulose,making available district increased,more hydroxyl can be reached by acetic anhydride.The activation processing is a preparation for next step,there is no obvious chemical reaction occurred.
(7) Scanning the CA by IR.1752cm~(-1) C=O stretching vibration,3348 cm~(-1) -OH stretching vibration,which intensity decreased significantly,it's proved that the product is CA.X-ray diffraction of CA:hydrogen bonds weaken,the introduction of acetic group make crystal structure damaged to a certain extent,which result in the reduction of cellulose crystallinity.
论文以尾叶桉为原料,研究了制浆、漂白、木聚糖酶处理和碱精制工艺,得到了满足醋酸纤维要求的浆粕,再进行活化、醋酸化、水解等处理,并对其反应机理进行了探讨。实验的主要结果如下:
(1)桉木浆粕采用KP+AQ法制得,条件为:用碱量17%(Na_2O计),硫化度16%,AQ 0.05%,液比1:4,空转30 min,升温90 min至130℃;再次升温90 min至170℃,保温60 min。
(2)为了得到高白度浆粕,又不造成环境污染,对D_1ED_2常规漂白条件进行了探讨,D_1段用氯量必须控制在3.6%以内;碱处理的条件需要强烈些,以去除半纤维素,提高浆粕的α-纤维素含量和平均平均聚合度。但是想要通过提高用碱量来大幅提高α-纤维素含量是不可行的。桉木制醋酸纤维浆粕的漂白条件为:D_1段用氯量3.6%,70℃,90 min,浆浓10%,pH 3.5;E段NaOH 2.0%,75℃,60 min,浆浓10%;D_2段用氯量0.9%,70℃,90 min,浆浓10%,pH 3.5;P段NaOH用量与H_2O_2用量一致为2.5%,70℃,90 min,浆浓10%。
(3)木聚糖酶处理最佳条件为:酶用量120 IU/g,60℃,时间2h,浆浓3%,pH6.0;碱精制中,NaOH除了可以去掉部分半纤维素,而且可以溶解掉部分短链纤维素,当碱浓度为4%时,平均聚合度增至1163,白度增至90.0%,α-纤维索含量为96.78%,达到了醋酸纤维浆粕国际标准。
(4)对木聚糖酶处理前后的浆粕进行红外扫描。发色基团和助色基团如C=O伸展振动(1058cm~(-1))、木素-烷基醚基C-O-C伸展振动(1164cm~(-1))、芳基-烷基醚键(1240cm~(-1))、木素羰基伸展振动C=O(1637cm~(-1))、木素芳环振动(1430 cm~(-1))处的吸收峰在木聚糖酶处理后,强度有所减弱,这或许是木聚糖酶处理后浆粕白度提高的原因。
(5)桉木浆粕最佳活化条件:活化时间为3.0 h、活化温度50℃,醋酸用量为500%;醋酸化最佳条件为:醋酸酐用量400%,催化剂硫酸用量7.5%,温度60℃,时间2h;水解最佳条件为:醋酸含量为80%,水解温度为60℃,制得醋酸纤维取代度为2.51。
(6)对活化后的浆粕进行X-射线衍射扫描,并结合红外图谱。活化处理仅仅是一个物理溶胀的过程,确实改变了纤维素的结晶结构,使得可及区增加,有更多的羟基为醋酸化剂可及,有利于醋酸化反应的进行,用醋酸对浆粕的活化处理,为醋酸化做足准备,其他并无明显化学反应发生。
(7)对醋酸纤维红外扫描。1752cm~(-1)为C=O的伸缩振动,3348 cm~(-1)为-OH伸缩振动,其强度明显减弱,说明浆粕醋酸化产物的主要成分是醋酸纤维;对醋酸纤维进行X-射线衍射扫描,醋酸化使纤维素氢键作用减弱,同时醋酸基的引入使纤维素结晶结构受到一定程度的破坏,从而导致纤维素结晶度的降低。
Cellulose acetate is used widely,its raw materials is cotton of high-cellulose content or senior coniferous wood pulp,which is needed to import from abroad.Therefore,the research and development of wood pulp become the key issues of sustainable development of cellulose acetate,Eucalyptus is an important fast-growing hardwood species,which has importance to ease the cellulose acetate industry in China.
Eucalyptus is studied as raw materials in this paper,including pulping、bleaching、xylanase and alkaline purification process,the product meet the requirements of cellulose acetate pulp,and then activation、acetic anhydirde、hydrolysis process and its mechanism explore.The main experimental results:
(1) The pulp is cooked by means of KP+AQ,conditions:alkaline 17%(Na_2O),sulphidity 16%,AQ 0.05%,liquid ratio 1:4,idling about 30 min,heating to 130℃within 90min;then warming up to 170℃in 90min,holding temperature about 60min.
(2) In order to increase brightness without causing environmental pollution,it's needed to research the conditions of D_1ED_2 conventional bleaching,the amount of chlorine must be controlled within 3.6% at D_1 stage;in order to improve a-cellulose content and degree of polymerization,alkaline conditions is needed more stronger to remove the hemicellulose.But it is not feasible to increase a-cellulose content by increasing the amount of alkaline.Eucalyptus wood pulp bleaching conditions for cellulose acetate: D_1,the amount of chlorine 3.6%,70℃,90 min,plup consistence 10%,pH 3.5;E paragraphs NaOH 2.0%,75℃,60 min,pulp concentration 10%;D_2,the amount of chlorine 0.9%,70℃,90 min,plup consistence 10%,pH 3.5;P,the amount of NaOH and H_2O_2 are the same amount of 2.5%,70℃,90 min, plup consistence 10%.
(3) Pulp's xylanase purification conditions:enzyme dosage 120 IU/g,60℃,time 2h,plup consistence 3%,pH 6.0.Alkali purification,NaOH can not only remove part of hemicellulose,also dissolve some short-chain cellulose,when the alkali consistence is 4%,the degree of polymerization 1163,brightness 90.0%,a-cellulose content 96.78%,cellulose acetate pulp achieve international standards.
(4) Scanning the pulp before and after purification treatment by 1R.It's found that:the chromophoric group and color auxochrome group,such as the C=O stretching vibration(1058cm~(-1)), lignin-alkyl ether-based C-O-C stretching vibration(1164cm~(-1)),aryl-alkyl ether bond(1240cm~(-1)), lignin carbonyl stretching vibration C=O(1637cm~(-1)),lignin aryl ring vibration(1430 cm~(-1)),their absorption peak intensity has weakened after purification,and this is why the pulp's brightness increased after purificationt.
(5) The activation of eucalyptus pulp's conditions:time 3.0 h,temperature 50℃,the amount of acetic acid 500%;acetic anhydride conditions:the amount of acetic anhydride 400%,the amount of catalyst sulfate 7.5%,temperature 60℃,time 2.0 h;the hydrolysis conditions:80%acetate content, temperature 60℃,degree of substitution of CA is 2.51.
(6) Scanning pulp before and after activation by means of X-ray diffraction and IR.The activation is just a physical process,change the crystalline structure of cellulose,making available district increased,more hydroxyl can be reached by acetic anhydride.The activation processing is a preparation for next step,there is no obvious chemical reaction occurred.
(7) Scanning the CA by IR.1752cm~(-1) C=O stretching vibration,3348 cm~(-1) -OH stretching vibration,which intensity decreased significantly,it's proved that the product is CA.X-ray diffraction of CA:hydrogen bonds weaken,the introduction of acetic group make crystal structure damaged to a certain extent,which result in the reduction of cellulose crystallinity.
引文
1.刘海洋,王乐军,李琳等.再生纤维素纤维的现状与发展方向[J].纺织导报,2006,(4):57-59.
2.罗伟国.世界纤维素纤维的现状及发展[J].人造纤维,2002,32(2):24-25.
3.姜繁昌,邵宽,周岩等.苎麻纺纱学[M].北京:纺织工业出版社,1985:15-35.
4.马君志,葛红.醋酸纤维工业的发展现状[J].上海纺织科技,2006,34(9):15-17.
5.Hans-J,Koslowski.国际化纤编辑部(德国).醋酯纤维诞生100周年纪念[J].国际纺织导报,2005,(3):10-18.
6.邹盛欧.醋酸纤维制造技术的进步[J].化工科技动态,1992,(12):20-22.
7.韩亚冬,李天霞.湿法生产再生二醋纤烟用滤嘴丝束的研究[J].合成纤维,1993,(2):20-23.
8.杨占平,徐坦.二醋酸纤维浆液精细过滤及高密度生产技术研究[J].中国烟草报,2006,12(3):27-30.
9.王桂花.液晶显示屏(LCD)用三醋酸纤维(TAC)薄膜的发展现状与前景[J].影像技术,2005,(3-4):15-18.
10.杨韶辉,马宇平.醋纤和改性丙纤滤嘴对卷烟烟气成分的影响比较[J].烟草科技,2006,(7):51-55.
11.潘燕如,邹君.勒木研制烟用二醋酸纤维[J].广西化纤通讯,1996,(2):3-11.
12.马晓龙,沈琳,杨占平等.国产木浆合成烟用醋酸纤维的研究[J].合成纤维,2004,(5):10-12.
13.陈克利,林治助.稻草的氧碱法制浆(1)—中浓法制浆与高浓法制浆的比较[J].中国造纸学报,1996,11(增刊):8-13.
14.闫东坡,杨淑惠,李友森.从木素物理性质比较AP及AS预处理对红麻杆芯部的作用[J].中国造纸,1999,(1):31-35.
15.魏春学,杜增举,张会荣.醋酸纤维工业形势分析及发展建议.山东纺织经济,2002(5):33-35.
16.谢澄,陈中豪,陈昌华等.两种桉木APMP制浆及其磨浆过程的研究[J].中国造纸学报,2000,15:27-32.
17.许文璋.发展我国尾叶桉制浆造纸的几点看法[J].国际造纸,1995.14(4):14-20.
18.祁述雄.中国桉树[M].中国林业出版社,2002.
19.王金昌.混合阔叶木制人纤浆粕[J].纸和造纸,2002,(4):13-14.
20.包雯霞,管红星.尾叶桉浆粕制粘胶纤维的研究[J].广东化纤,1994,(1):16-19.
21.谢来苏,詹怀宇.制浆原理与工程[M].中国轻工业出版社,2001:240.
22.肖玲,河东保,杜予民.棉杆制漂白化学浆和人造丝浆的研究[J].林产化学与工业,1995,15(3):51-55.
23.苏纯阳,程学慧,劳泰财等.新一代饲用酶制剂-细菌性聚木糖酶[J].饲料工业,2004,25(2):40-42.
24.刘昭铁,一种制备三醋酸纤维的方法,陕西师范大学.专利号:200710017461.X 2007.3.5.
25.赵建,石淑兰,胡惠仁.速生桉木硫酸盐浆的无元素氯漂白[J].黑龙江造纸,1998(01):5-8.
26.肖长发,尹翠玉,张华等.化学纤维概论[M].北京:中国纺织出版社,1997:42-44.
27.刘利娟.麦草NaOH和NaOH/O_2两段蒸煮及其过氧化氢漂白[J],北方造纸,1996,17(4):4-7.
28.陈克利,林治助.稻草的氧碱法制浆(1)——中浓法制浆与高浓法制浆的比较[J],中国造纸学报,1996(增刊):8-10.
29.刘玉新,胡慧仁.三倍体毛白杨硫酸盐法制浆中半纤维预提取工艺的研究[C]/天津科技大学.第二届国际造纸与环境学术会议论文集.北京:中国轻工业出版社,2008:142-145.
30.马晓龙,沈琳等.国产木浆合成烟用醋酸纤维的研究[J].合成纤维,2004,(5):10-12.
31.杨淑惠.植物纤维化学[M].北京:中国轻工业出版社,2001:239-240.
32.吕卫军,蒲俊文,漆小华.聚木糖酶在溶解浆制备中的应用研究[J].造纸科学与技术.2007(02):16-19.
33.吴宁,姚春丽,夏耀玲等.尾巨桉KP-AQ制浆及漂白特性的研究[J].中国造纸,2007.26(3):4-6.
34.杨玲.蒸煮助剂在竹片KP/AQ法制浆中的应刚,两南造纸,2006(1):33-34.
35.李元禄.无污染全无氯漂白(TCF).中国造纸,1997(5):42.
36.黄文荣,陈中豪.ECF和TCF漂白是造纸工业可持续发展的方向[J],中国造纸,2003(8):40-44.
37.安郁琴,于伟东.TCF高白度按木化学浆漂白[J].中国造纸学报增刊,1996,11:24-28.
38.谢米苏.制浆原理与工程[M].北京:中国轻工业出版社,2001:226.
39.赵建,李雪芝,曲音波等.助剂改善的桉木硫酸盐浆的H_2O_2漂白[J].西南造纸,2000,6:5-7.
40.覃程荣,詹怀宇,李兵云等.硫酸盐法竹浆无元素氟漂白的研究[J].福建林学院学报,2005,25(4):54-55.
41.蒲云桥,詹怀宇,伍红等.湿地松硫酸盐浆ECF漂白过程中木素结构的变化[J].中国造纸学报,2002,(17)1:26-51.
42.张曾,黄干强.螯合剂在H_2O_2,漂白及废水处理中的变化与影响[J].中国造纸,2001,(4):48-52.
43.周学飞,陈嘉翔,余家鸾.鳌合处理过氧化氢漂白中的金属离子[J].纸和造纸,1997,(5):12-15.
44.黄干强.螯合作用与过氧化氢漂白[J].广东造纸,1996,(4):12.
45.刘明友.马尾松硫酸盐浆脱木素的研究[J].中国造纸学报,1997,12:25-29.
46.李元禄.兰桉硫酸盐浆TCF漂白的氧脱木素和预处理研究[J].中国造纸学报,1998,15:27-55.
47.周学飞.硫酸盐浆氧脱木素工艺参数的影响及其优化的研究[J].中国造纸学报,1998,15:10-15.
48.尹素红,刘云,张军等.过氧化氢漂白影响因素的研究[J].北京轻工业学院学报,2005,19(1):25-28.
49.陈嘉川.湿地松KP浆氧和过氧化氢脱木索的研究[J].中国造纸,1993,15:10-16.
50.制浆造纸手册.第三分册.碱法制浆,北京:轻工业出版社,1988:115-120.
51.邢益林译.制浆漂白新技术概述吉林造纸,1998,2:53-67.
52.梅洁,陈家楠,欧义芳.醋酸纤维的现状与发展趋势[J].纤维素科学与技术,1997,7(4):56-63.
53.马孝田.醋酸纤维的制造[J].广东化纤,1994,(02):27-34.
54.孟庆莉,李英春.纤维素醋酸酯的均相合成[J].化学研究与应用,2004,(02):288-289.
55.任天瑞,,沈斌,李永红等.纤维素的均相化学反应[J].化学进展,2004,(06).
56.孟庆莉,乔艳辉.纤维素有机酸酯的研究进展[J].青岛科技大学学报(自然科学版),2003, (9):18-20.
57.梅洁,欧义芳,陈家楠.醋酸纤维的高温合成及其性质的研究[J].纤维素科学与技术,2000,(01):9-16.
58.Iribarne T,Schroeder L R.High pressure oxygen delignification of kraft pulps[J],Tappi,1997,80(10):241-250.
60.Kishi rnoto T,Nakatsubo F.Non-chlorine bleaching of kraft pulp[J].Holzforsching,1996,50(4):572-578.
61.Amini B,W ebster J.On-site peradds {Tools for bleaching strategies to the cluster rule and considerations On selecting among them.Tappi,19951 78(10):121-133.
62.Sund quist J.Bleached pulp without sulphur and chlorine chemicals by a peroxyacid/alkllne peroxlde-methnd-an overview.Paperila puut1986 68(9):616-620.
63.Carlton W Dence,Douglas W Reeve.Pulp Bleaching-Principles and Practice.Atlanta:Tappi Press,1996:349.
64.Yang J L,Lou G,Eriksson KEL.The impact of xylanase on bleaching of kraft pulps[J].Tappi,1992,75(10):95-101.
65.Viikari L,Ranua M,Kantelinen A,et al.Proceedings of the 3rd International Conference on Biotechnology in the Pulp and Paper Industry[M].STFI:Stockholm,1986:67-69.
66.Suurnakki A,Clark T A,Allison R W,et al.Xylanase-and mannanase-aided ECF and TCF bleaching[J].Tappi,1996,79(7):111-117.
67.Wong K K Y,Yokota S,Saddler J N,et al.Enzymic hydrolysis of lignin-carbohydrade complex isolated from kraft pulp[J].Journel of wood chemistry technology,1996,16(2):121-125.
68.Clark T A,Steward D,Bruce M E,et al.Improved bleachability of Radiata pine kraft pulps following treatment with hemicelluloytic enzymes[J].Appita,1991,44(6):389-39.
69.Renzi,Gabriete.Synthesis for cellulose acetate at low temperature[P].USP:24/8425,1982.
70.Brewer.Catylyst for and method of preparing cellulose esters[P].USP:4314056,1982.
71.C.J.Mlam,L.J.Tangle,J.T Schmitt.The catalysts in esterification of cellulose[J].Ind.Eng,Chem,1961,53:363-372.
72.Zhang ZB,McCormick CL.Journal of Applied Polymer Science,1997,66:293-305.
73.Marson GA,El Seoud O A.Journal of Polymer Science:Part A:Polymer Chemistry,1999,37:3738-3744.
74.Saka Shiro Takanashi Keiko,Matsumura Hiroyukj.Effects of solbent to acetylation medium on cellulose triacetate prepared from low-grade hardwood dissolving pulp[J].Journal of Applied Polymer Science,1998,69:1445-1449.
75.MAJDANAC L D,POLETI D,TEODOROVIC M J.Determination ofthe crystilinity of celulose samples by X-ray difraction[J].Acta Polymer,1991,42:351-357.
76.Me r J et al.bleaching and delignification of lignoceliulosic materials USP:8248543.
77.Hans U,Sulse,Chreeson Moodley.Progress in bleaching to top brightenss with low reservision [J]. TAPPSA Journal, 2005(3): 89.
78. Sunna A, Autranikian G. Xylanolytic enzymes from fungi and bacterial[J]. Crtical Revieas in Biotechology, 1997, 17(1): 39-67.
79. Saka Shiro Takanashi Keiko. Cellulose triacetate prepared from low-grade hardwood dissolving pulp and its insoluble residued in acetylation mediums[J]. Journal of A pplied Polymer Science,1998,67:289-297.
80. Hinck J F, Casabier R L, Hamilton J K. Production of Dissolving Grade Pulp from Poplar Wood by Ethanol[J]. Tappi, 68(4):213-243.
81. H. Matsumura, S.Saka. Cellulose triacetate prepared from low-grade wood pulp: insoluble residue in acetylation solution[J ]. Mokuzai Gakkaishi, 1992, 38(3): 270-276.
2.罗伟国.世界纤维素纤维的现状及发展[J].人造纤维,2002,32(2):24-25.
3.姜繁昌,邵宽,周岩等.苎麻纺纱学[M].北京:纺织工业出版社,1985:15-35.
4.马君志,葛红.醋酸纤维工业的发展现状[J].上海纺织科技,2006,34(9):15-17.
5.Hans-J,Koslowski.国际化纤编辑部(德国).醋酯纤维诞生100周年纪念[J].国际纺织导报,2005,(3):10-18.
6.邹盛欧.醋酸纤维制造技术的进步[J].化工科技动态,1992,(12):20-22.
7.韩亚冬,李天霞.湿法生产再生二醋纤烟用滤嘴丝束的研究[J].合成纤维,1993,(2):20-23.
8.杨占平,徐坦.二醋酸纤维浆液精细过滤及高密度生产技术研究[J].中国烟草报,2006,12(3):27-30.
9.王桂花.液晶显示屏(LCD)用三醋酸纤维(TAC)薄膜的发展现状与前景[J].影像技术,2005,(3-4):15-18.
10.杨韶辉,马宇平.醋纤和改性丙纤滤嘴对卷烟烟气成分的影响比较[J].烟草科技,2006,(7):51-55.
11.潘燕如,邹君.勒木研制烟用二醋酸纤维[J].广西化纤通讯,1996,(2):3-11.
12.马晓龙,沈琳,杨占平等.国产木浆合成烟用醋酸纤维的研究[J].合成纤维,2004,(5):10-12.
13.陈克利,林治助.稻草的氧碱法制浆(1)—中浓法制浆与高浓法制浆的比较[J].中国造纸学报,1996,11(增刊):8-13.
14.闫东坡,杨淑惠,李友森.从木素物理性质比较AP及AS预处理对红麻杆芯部的作用[J].中国造纸,1999,(1):31-35.
15.魏春学,杜增举,张会荣.醋酸纤维工业形势分析及发展建议.山东纺织经济,2002(5):33-35.
16.谢澄,陈中豪,陈昌华等.两种桉木APMP制浆及其磨浆过程的研究[J].中国造纸学报,2000,15:27-32.
17.许文璋.发展我国尾叶桉制浆造纸的几点看法[J].国际造纸,1995.14(4):14-20.
18.祁述雄.中国桉树[M].中国林业出版社,2002.
19.王金昌.混合阔叶木制人纤浆粕[J].纸和造纸,2002,(4):13-14.
20.包雯霞,管红星.尾叶桉浆粕制粘胶纤维的研究[J].广东化纤,1994,(1):16-19.
21.谢来苏,詹怀宇.制浆原理与工程[M].中国轻工业出版社,2001:240.
22.肖玲,河东保,杜予民.棉杆制漂白化学浆和人造丝浆的研究[J].林产化学与工业,1995,15(3):51-55.
23.苏纯阳,程学慧,劳泰财等.新一代饲用酶制剂-细菌性聚木糖酶[J].饲料工业,2004,25(2):40-42.
24.刘昭铁,一种制备三醋酸纤维的方法,陕西师范大学.专利号:200710017461.X 2007.3.5.
25.赵建,石淑兰,胡惠仁.速生桉木硫酸盐浆的无元素氯漂白[J].黑龙江造纸,1998(01):5-8.
26.肖长发,尹翠玉,张华等.化学纤维概论[M].北京:中国纺织出版社,1997:42-44.
27.刘利娟.麦草NaOH和NaOH/O_2两段蒸煮及其过氧化氢漂白[J],北方造纸,1996,17(4):4-7.
28.陈克利,林治助.稻草的氧碱法制浆(1)——中浓法制浆与高浓法制浆的比较[J],中国造纸学报,1996(增刊):8-10.
29.刘玉新,胡慧仁.三倍体毛白杨硫酸盐法制浆中半纤维预提取工艺的研究[C]/天津科技大学.第二届国际造纸与环境学术会议论文集.北京:中国轻工业出版社,2008:142-145.
30.马晓龙,沈琳等.国产木浆合成烟用醋酸纤维的研究[J].合成纤维,2004,(5):10-12.
31.杨淑惠.植物纤维化学[M].北京:中国轻工业出版社,2001:239-240.
32.吕卫军,蒲俊文,漆小华.聚木糖酶在溶解浆制备中的应用研究[J].造纸科学与技术.2007(02):16-19.
33.吴宁,姚春丽,夏耀玲等.尾巨桉KP-AQ制浆及漂白特性的研究[J].中国造纸,2007.26(3):4-6.
34.杨玲.蒸煮助剂在竹片KP/AQ法制浆中的应刚,两南造纸,2006(1):33-34.
35.李元禄.无污染全无氯漂白(TCF).中国造纸,1997(5):42.
36.黄文荣,陈中豪.ECF和TCF漂白是造纸工业可持续发展的方向[J],中国造纸,2003(8):40-44.
37.安郁琴,于伟东.TCF高白度按木化学浆漂白[J].中国造纸学报增刊,1996,11:24-28.
38.谢米苏.制浆原理与工程[M].北京:中国轻工业出版社,2001:226.
39.赵建,李雪芝,曲音波等.助剂改善的桉木硫酸盐浆的H_2O_2漂白[J].西南造纸,2000,6:5-7.
40.覃程荣,詹怀宇,李兵云等.硫酸盐法竹浆无元素氟漂白的研究[J].福建林学院学报,2005,25(4):54-55.
41.蒲云桥,詹怀宇,伍红等.湿地松硫酸盐浆ECF漂白过程中木素结构的变化[J].中国造纸学报,2002,(17)1:26-51.
42.张曾,黄干强.螯合剂在H_2O_2,漂白及废水处理中的变化与影响[J].中国造纸,2001,(4):48-52.
43.周学飞,陈嘉翔,余家鸾.鳌合处理过氧化氢漂白中的金属离子[J].纸和造纸,1997,(5):12-15.
44.黄干强.螯合作用与过氧化氢漂白[J].广东造纸,1996,(4):12.
45.刘明友.马尾松硫酸盐浆脱木素的研究[J].中国造纸学报,1997,12:25-29.
46.李元禄.兰桉硫酸盐浆TCF漂白的氧脱木素和预处理研究[J].中国造纸学报,1998,15:27-55.
47.周学飞.硫酸盐浆氧脱木素工艺参数的影响及其优化的研究[J].中国造纸学报,1998,15:10-15.
48.尹素红,刘云,张军等.过氧化氢漂白影响因素的研究[J].北京轻工业学院学报,2005,19(1):25-28.
49.陈嘉川.湿地松KP浆氧和过氧化氢脱木索的研究[J].中国造纸,1993,15:10-16.
50.制浆造纸手册.第三分册.碱法制浆,北京:轻工业出版社,1988:115-120.
51.邢益林译.制浆漂白新技术概述吉林造纸,1998,2:53-67.
52.梅洁,陈家楠,欧义芳.醋酸纤维的现状与发展趋势[J].纤维素科学与技术,1997,7(4):56-63.
53.马孝田.醋酸纤维的制造[J].广东化纤,1994,(02):27-34.
54.孟庆莉,李英春.纤维素醋酸酯的均相合成[J].化学研究与应用,2004,(02):288-289.
55.任天瑞,,沈斌,李永红等.纤维素的均相化学反应[J].化学进展,2004,(06).
56.孟庆莉,乔艳辉.纤维素有机酸酯的研究进展[J].青岛科技大学学报(自然科学版),2003, (9):18-20.
57.梅洁,欧义芳,陈家楠.醋酸纤维的高温合成及其性质的研究[J].纤维素科学与技术,2000,(01):9-16.
58.Iribarne T,Schroeder L R.High pressure oxygen delignification of kraft pulps[J],Tappi,1997,80(10):241-250.
60.Kishi rnoto T,Nakatsubo F.Non-chlorine bleaching of kraft pulp[J].Holzforsching,1996,50(4):572-578.
61.Amini B,W ebster J.On-site peradds {Tools for bleaching strategies to the cluster rule and considerations On selecting among them.Tappi,19951 78(10):121-133.
62.Sund quist J.Bleached pulp without sulphur and chlorine chemicals by a peroxyacid/alkllne peroxlde-methnd-an overview.Paperila puut1986 68(9):616-620.
63.Carlton W Dence,Douglas W Reeve.Pulp Bleaching-Principles and Practice.Atlanta:Tappi Press,1996:349.
64.Yang J L,Lou G,Eriksson KEL.The impact of xylanase on bleaching of kraft pulps[J].Tappi,1992,75(10):95-101.
65.Viikari L,Ranua M,Kantelinen A,et al.Proceedings of the 3rd International Conference on Biotechnology in the Pulp and Paper Industry[M].STFI:Stockholm,1986:67-69.
66.Suurnakki A,Clark T A,Allison R W,et al.Xylanase-and mannanase-aided ECF and TCF bleaching[J].Tappi,1996,79(7):111-117.
67.Wong K K Y,Yokota S,Saddler J N,et al.Enzymic hydrolysis of lignin-carbohydrade complex isolated from kraft pulp[J].Journel of wood chemistry technology,1996,16(2):121-125.
68.Clark T A,Steward D,Bruce M E,et al.Improved bleachability of Radiata pine kraft pulps following treatment with hemicelluloytic enzymes[J].Appita,1991,44(6):389-39.
69.Renzi,Gabriete.Synthesis for cellulose acetate at low temperature[P].USP:24/8425,1982.
70.Brewer.Catylyst for and method of preparing cellulose esters[P].USP:4314056,1982.
71.C.J.Mlam,L.J.Tangle,J.T Schmitt.The catalysts in esterification of cellulose[J].Ind.Eng,Chem,1961,53:363-372.
72.Zhang ZB,McCormick CL.Journal of Applied Polymer Science,1997,66:293-305.
73.Marson GA,El Seoud O A.Journal of Polymer Science:Part A:Polymer Chemistry,1999,37:3738-3744.
74.Saka Shiro Takanashi Keiko,Matsumura Hiroyukj.Effects of solbent to acetylation medium on cellulose triacetate prepared from low-grade hardwood dissolving pulp[J].Journal of Applied Polymer Science,1998,69:1445-1449.
75.MAJDANAC L D,POLETI D,TEODOROVIC M J.Determination ofthe crystilinity of celulose samples by X-ray difraction[J].Acta Polymer,1991,42:351-357.
76.Me r J et al.bleaching and delignification of lignoceliulosic materials USP:8248543.
77.Hans U,Sulse,Chreeson Moodley.Progress in bleaching to top brightenss with low reservision [J]. TAPPSA Journal, 2005(3): 89.
78. Sunna A, Autranikian G. Xylanolytic enzymes from fungi and bacterial[J]. Crtical Revieas in Biotechology, 1997, 17(1): 39-67.
79. Saka Shiro Takanashi Keiko. Cellulose triacetate prepared from low-grade hardwood dissolving pulp and its insoluble residued in acetylation mediums[J]. Journal of A pplied Polymer Science,1998,67:289-297.
80. Hinck J F, Casabier R L, Hamilton J K. Production of Dissolving Grade Pulp from Poplar Wood by Ethanol[J]. Tappi, 68(4):213-243.
81. H. Matsumura, S.Saka. Cellulose triacetate prepared from low-grade wood pulp: insoluble residue in acetylation solution[J ]. Mokuzai Gakkaishi, 1992, 38(3): 270-276.