杨木浆板制备高取代度低粘度羧甲基纤维素钠的工艺研究
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摘要
以杨木浆板纤维素为原料,通过单因素实验和正交实验,采取预处理工艺和三次碱化两次醚化工艺,并采用超声波和高速剪切分散等辅助手段,制备高取代度羧甲基木质纤维素钠。结果表明,预处理工艺:70℃下用10%Na OH溶液(固液比1∶40 g/m L)浸泡搅拌90 min;碱化醚化工艺:室温下首次碱化时间为60 min,50℃下第二次碱化和首次醚化反应时间为30 min,最后在70℃下第三次碱化和第二次醚化反应时间为90 min,氯乙酸钠用量∶Na OH用量∶碱化纤维素用量=1. 4∶1∶1 (质量比);经过预处理和三次碱化两次醚化,产品取代度达到1. 33,黏度为404. 0 m Pa·s。在碱化醚化过程中,在室温碱化后用高速剪切分散处理10 min(A档),第一次醚化后用超声波处理10 min(49 k Hz,功率99%),最终产品的取代度由1. 33升高到1. 48,但黏度由404. 0 m Pa·s下降到181. 9 m Pa·s。
Wood pulp board cellulose is used as raw material,pretreatment technology and three times of alkalization and twice of etherification processes are adopted through single factor experiment and orthogonal experiment,and ultrasonic and high-speed shear dispersion are used as auxiliary methods. The preparation of high substitution sodium carboxymethyl lignocellulose were determined,and the results showed that the pretreatment process was that soaking and stirring lasted for 90 min with 10% sodium hydroxide solution( solid-liquid ratio 1 ∶ 40) at 70 ℃,and the alkalization and etherification process was that the first time of alkalization lasted for 60 min at room temperature,and the second time of alkalization and the first time of etherification reaction lasted for 30 min at 50 ℃,the third time of alkalization and the second time of therification reaction lasted for 90 min at 70 ℃,and the dosage ratio of sodium chloroacetate to sodium hydroxide to alkaline cellulose was 1. 4∶ 1∶ 1,after pretreatment and three times of alkalizations and twice of etherification,the degree of substitution is 1. 33 and the viscosity is 404. 0 m Pa·s. In the process of alkalization and etherification,when the high-speed shear dispersion was used for 10 min( Grade A)after alkalization at room temperature,and ultrasonic treatment was used for 10 min( 49 k Hz,power99%) after the first time of etherification,the degree of substitution of the final product increased from1. 33 to 1. 48,but the viscosity decreased from 404. 0 m Pa·s to 181. 9 m Pa·s.
Wood pulp board cellulose is used as raw material,pretreatment technology and three times of alkalization and twice of etherification processes are adopted through single factor experiment and orthogonal experiment,and ultrasonic and high-speed shear dispersion are used as auxiliary methods. The preparation of high substitution sodium carboxymethyl lignocellulose were determined,and the results showed that the pretreatment process was that soaking and stirring lasted for 90 min with 10% sodium hydroxide solution( solid-liquid ratio 1 ∶ 40) at 70 ℃,and the alkalization and etherification process was that the first time of alkalization lasted for 60 min at room temperature,and the second time of alkalization and the first time of etherification reaction lasted for 30 min at 50 ℃,the third time of alkalization and the second time of therification reaction lasted for 90 min at 70 ℃,and the dosage ratio of sodium chloroacetate to sodium hydroxide to alkaline cellulose was 1. 4∶ 1∶ 1,after pretreatment and three times of alkalizations and twice of etherification,the degree of substitution is 1. 33 and the viscosity is 404. 0 m Pa·s. In the process of alkalization and etherification,when the high-speed shear dispersion was used for 10 min( Grade A)after alkalization at room temperature,and ultrasonic treatment was used for 10 min( 49 k Hz,power99%) after the first time of etherification,the degree of substitution of the final product increased from1. 33 to 1. 48,but the viscosity decreased from 404. 0 m Pa·s to 181. 9 m Pa·s.
引文
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[18] Bao Y,Ma J,Li N. Synthesis and swelling behaviors of sodium carboxymethyl cellulose-g-poly(AA-co-AM-co-AMPS)/MMT superabsorbent hydrogel[J]. Carbohydrate Polymers,2011,84(1):76-82.
[19]余小龙,刘健,甘礼惠,等.竹屑制备高取代度羧甲基纤维素钠的优化及其表征[J].现代化工,2015,35(8):109-114.
[20]李瑞雪,杨丽娇,王庆福,等.蔗渣再生纤维素制备高取代度羧甲基纤维素钠的研究[J].化学与生物工程,2014,31(4):51-54.
[21]刘晓庚,王四青,彭冬梅.微波辅助法由豆渣制备羧甲基纤维素[J].中国粮油学报,2007,22(6):152-156.
[22]谭凤芝,李沅,王大鸷,等.微波辐射下高取代度羧甲基纤维素的制备[J].大连工业大学学报,2008,27(2):149-151.
[23]樊泽霞,夏俭英.测定羧甲基纤维素钠取代度的新方法——酸度计滴定法[J].钻井液与完井液,1997,14(5):37-38.
[24]王杰.竹浆粕制备高粘度羧甲基纤维素钠及其反应机理研究[D].杭州:浙江农林大学,2015.
[25]罗仓学,李丽,王白鸥,等.由苹果渣制备高取代度羧甲基纤维素钠的研究[J].食品工业科技,2008,29(7):207-212.
[26]唐爱民.超声波作用下纤维素结构与性质的研究[D].广州:华南理工大学,2000.
[27]李俊华,李俊莉,杨乃望.影响羧甲基纤维素粘度的实验研究[J].应用化学工业,2011,40(3):478-482,485.
[2]张超,郭晓飞,李武,等.羧甲基纤维素含量对大豆分离蛋白复合包装材料结构和性能的影响[J].中国食品学报,2014,14(2):187-192.
[3]董志俭,赵帅,孙丽平,等. CMC/阿拉伯胶/明胶复合凝聚橘油微胶囊的制备方法[J].中国食品学报,2013,13(6):69-76.
[4]李外,赵雄虎,季一辉,等.羧甲基纤维素制备方法及其生产工艺研究进展[J].石油化工,2013,42(6):693-701.
[5] Ibrahim S M. Preparation and properties of carboxymethyl cellulose(CMC)/sodium alginate(SA)blends induced by gamma irradiation[J]. Journal of Polymers and the Environment,2013,21(2):520-527.
[6]刘莹,谢峰,刘义武,等.果胶/羧甲基纤维素钠复合涂膜液在冷鲜肉保鲜中的应用效果[J].保鲜与加工,2015,15(2):25-28.
[7]李赢,姜帅,靳璇,等.稻壳基羧甲基纤维素的制备与其制膜性能研究[J].中国食品学报,2015,15(12):55-59.
[8]张超,郭晓飞,李武,等.干燥温度对大豆分离蛋白/羧甲基纤维素复合膜性能的影响[J].食品工业科技,2015,36(10):317-319.
[9]王卉,孙宏元,何节玉,等.羧甲基纤维素钠纳米抗菌复合膜的制备及其性能研究[J].食品工业科技,2016,37(5):77-280.
[10] Ragheb A A,Nassar S H,Abd E I,et al. Preparation characterization and technological evaluation of CMC derived from rice-straw as thickening agents in discharge,discharge-resist and burn-out printing[J]. Carbonhydrate Polymers,2012,89(4):1044-1049.
[11]潘旭琳,于璐,李建.绿豆芽可食性膜的制备及性能研究[J].包装工程,2013,34(13):5-9.
[12]邓丰林.羧甲基纤维素水凝胶纤维的制备及性能研究[D].武汉:武汉纺织大学,2016.
[13]吴奥丽.羧甲基纤维素钠凝胶载体的制备及其控制释放作用的研究[J].中国洗涤用品工业,2016(2):66-70.
[14] Serrano-Cruz M R,Villanueva-Carvajal A,Morales Rosales E J,et al. Controlled release and antioxidant activity of Roselle(Hibiscus sabdariffa L.)extract encapsulated in mixtures of carboxymethyl cellulose,whey protein,and pectin[J]. LWT-Food Science and Technology,2013,50(2):554-561.
[15] Chitprasert P,Sudsai P,Rodklongtan A. Aluminum carboxymethyl cellulose-rice bran microcapsules:Enhancing survival of Lactobacillus reuteri KUB-ACS[J]. Carbohydrate Polymers,2012,90(1):78-86.
[16] Yan H,Zhang W,Kan X,et al. Sorption of methylene blue by carboxymethyl cellulose and reuse process in a secondary sorption[J]. Colloids and Surfaces A:Physicochemical and Engineering Aspects,2011,380(1/2/3):143-151.
[17] Luna-Martinez J F,Hernandez-Uresti D B,Reyes-Melo M E,et al. Synthesis and optical characterization of Zn S-sodium carboxymethyl cellulose nanocomposite films[J].Carbohydrate Polymers,2011,84(1):566-570.
[18] Bao Y,Ma J,Li N. Synthesis and swelling behaviors of sodium carboxymethyl cellulose-g-poly(AA-co-AM-co-AMPS)/MMT superabsorbent hydrogel[J]. Carbohydrate Polymers,2011,84(1):76-82.
[19]余小龙,刘健,甘礼惠,等.竹屑制备高取代度羧甲基纤维素钠的优化及其表征[J].现代化工,2015,35(8):109-114.
[20]李瑞雪,杨丽娇,王庆福,等.蔗渣再生纤维素制备高取代度羧甲基纤维素钠的研究[J].化学与生物工程,2014,31(4):51-54.
[21]刘晓庚,王四青,彭冬梅.微波辅助法由豆渣制备羧甲基纤维素[J].中国粮油学报,2007,22(6):152-156.
[22]谭凤芝,李沅,王大鸷,等.微波辐射下高取代度羧甲基纤维素的制备[J].大连工业大学学报,2008,27(2):149-151.
[23]樊泽霞,夏俭英.测定羧甲基纤维素钠取代度的新方法——酸度计滴定法[J].钻井液与完井液,1997,14(5):37-38.
[24]王杰.竹浆粕制备高粘度羧甲基纤维素钠及其反应机理研究[D].杭州:浙江农林大学,2015.
[25]罗仓学,李丽,王白鸥,等.由苹果渣制备高取代度羧甲基纤维素钠的研究[J].食品工业科技,2008,29(7):207-212.
[26]唐爱民.超声波作用下纤维素结构与性质的研究[D].广州:华南理工大学,2000.
[27]李俊华,李俊莉,杨乃望.影响羧甲基纤维素粘度的实验研究[J].应用化学工业,2011,40(3):478-482,485.