CN1051093C - 溶剂法制取纳米级微晶纤维素粉体的方法 - Google Patents
溶剂法制取纳米级微晶纤维素粉体的方法 Download PDFInfo
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- CN1051093C CN1051093C CN94115873A CN94115873A CN1051093C CN 1051093 C CN1051093 C CN 1051093C CN 94115873 A CN94115873 A CN 94115873A CN 94115873 A CN94115873 A CN 94115873A CN 1051093 C CN1051093 C CN 1051093C
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920002678 cellulose Polymers 0.000 claims abstract description 13
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Abstract
本发明属于用溶剂制取纳米级微晶纤维素粉体方法。
用化学方法处理棉花、苎麻等植物性纤维得到尺寸2.5nm-10nm的纳米级微晶纤维素,本发明所提供的方法,是以水溶性、低沸点的有机溶剂如丙酮或酒精洗涤纤维素,离心脱溶剂,重复洗涤过程,再进行低温干燥、粉碎和过筛得纳米级微晶纤维素粉体。
Description
本发明涉及用溶剂法制取纳米级微晶纤维素粉体的方法。
通常的微晶纤维素广泛用作药品赋形剂、焊药填料及化工原料等方面。微晶纤维素的制取是用盐酸水解棉花或苎麻等天然纤维,再经水洗、中和、脱水、干燥、粉碎等工序而得产品。微晶纤维素呈纤维状,长20μm~50μm,作为食品添加剂(如饮料、冰淇淋、奶油定型剂等)使用时口感不好,作为化工反应原料使用时仍有反应不均匀的现象。微晶纤维素由于粒子较粗,互不粘结、吸水性较低,易于用喷雾干燥制得产品。纳米级微晶纤维素呈颗粒状,尺寸在2.5nm~10nm之间,它是在微晶纤维素的基础上进一步用化学方法处理而制得,其口感柔滑可作多种保健型食品添加剂,用作化学反应时更均匀。纳米级微晶纤维素在烘干脱水后,由于纤维素颗粒与水分子结成氢键使产品粘结成较大硬块,不易粉碎。
本发明的目的是企图提供一种用溶剂制取纳米级微晶纤维素粉体的方法。
本发明提供的制备方法,是采用水溶性低沸点的有机溶剂,洗涤湿纳米级微晶纤维素,溶剂和纤维素的重量比为1∶1,处理后用离心法除去溶剂,再用有机溶剂重复洗涤处理过程后,再经过离心脱水并且在≤45℃,相对真空度为80000Pa~93325Pa下干燥2小时,然后粉碎和过筛,得到纳米级微晶纤维素粉体产品。所用的有机溶剂是纯度85%以上的酒精或丙酮。这些溶剂使用后可以回收再利用。有机溶剂在洗涤过程中所起的作用如下:
1.将纤维素中的水分置换出来而脱水,而且使纤维素干燥时不能与水结合成氢键。
2.由于有机溶剂沸点低,蒸发潜热小,因此使物料容易干燥,而且有机溶剂的逸出使纤维素颗粒间留下空隙,易于粉碎。
3.有机溶剂可以洗去纤维素中的可溶色素和杂质,使产品纯度提高。
本发明提供的制备方法,所得产品有以下优点:
微晶纤维素的吸水性强,且能起增稠作用,由于颗粒小,作食品添加剂时口感柔滑,若参与化学反应时,接近均相反应,可以提高产品质量。
实施例
采用化学方法处理棉花得到的纳米级微晶纤维素,在未经研磨或高速搅拌时,多个纤维素颗粒以疏松形式结合成较大颗粒,比重大于水,此时可用清水洗涤至中性,置于放有滤布的离心机中脱水,得含水量约50%的纳米级微晶纤维素。在离心机中每25公斤湿料中加入25公斤纯度大于85%的丙酮洗涤,离心脱丙酮,加入等量的新丙酮重复上述洗涤过程。离心后将纳米级纤维素置于45℃烘箱中真空干燥2小时,用棒式旋转粉碎机粉碎物料,过0.05mm的标准筛得产品。第一次丙酮洗涤母液用蒸馏法回收丙酮,第二次洗涤的丙酮母液留作下一批料作第一次洗涤用,烘箱蒸出的丙酮用冷凝法回收。
Claims (2)
1一种溶剂法制取纳米级微晶纤维素粉体的方法,其特征在于用水溶性低沸点的有机溶剂洗涤湿纳米级微晶纤维素,溶剂和纤维素的重量比为1∶1,用离心法除去溶剂,再用有机溶剂重复洗涤过程,再经过离心脱水并干燥2小时,干燥温度≤45℃,相对真空度为80000Pa~93325Pa,然后粉碎和过筛,得到纳米级微晶纤维素粉体产品,所用有机溶剂为纯度大于85%(重量)的酒精或丙酮。
2.根据权利要求1中所述的方法,其特征在于所述的有机溶剂可回收利用。
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CN1051093C true CN1051093C (zh) | 2000-04-05 |
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Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1089618C (zh) * | 1998-07-30 | 2002-08-28 | 武汉大学 | 凝胶渗透色谱柱用再生纤维素多孔填料的制备方法 |
CN1075515C (zh) * | 1998-12-30 | 2001-11-28 | 中国科学院广州化学研究所 | 一种微晶纤维素胶体的制法 |
WO2004055250A1 (en) * | 2002-12-18 | 2004-07-01 | The Hong Kong Polytechnic University | Method for pulverizing natural organic substance into nano-scale fibrous material |
CN101864684A (zh) * | 2010-06-11 | 2010-10-20 | 中国林业科学研究院林产化学工业研究所 | 棉短绒制备药品级微晶纤维素的方法 |
CN107365392B (zh) * | 2017-08-31 | 2019-10-18 | 泸州北方化学工业有限公司 | 一种提高水溶性纤维素醚产品流散性的方法 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3345357A (en) * | 1964-02-06 | 1967-10-03 | Fmc Corp | Method of purifying cellulose crystallite aggregates |
JPS5255513A (en) * | 1975-10-30 | 1977-05-07 | Fujitsu Ltd | Magnetic head |
JPH0284401A (ja) * | 1988-09-20 | 1990-03-26 | Asahi Chem Ind Co Ltd | 多孔性微小セルロース粒子 |
EP0415193A2 (en) * | 1989-08-17 | 1991-03-06 | Asahi Kasei Kogyo Kabushiki Kaisha | Finely divided suspension of cellulosic material and process for producing the same |
EP0460609A1 (en) * | 1990-06-07 | 1991-12-11 | Nisshinbo Industries, Inc. | Process for producing fine cellulose powder |
CN1081185A (zh) * | 1992-07-04 | 1994-01-26 | 苏志刚 | 用硫酸化废棉绒生产微晶纤维素工艺 |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3345357A (en) * | 1964-02-06 | 1967-10-03 | Fmc Corp | Method of purifying cellulose crystallite aggregates |
JPS5255513A (en) * | 1975-10-30 | 1977-05-07 | Fujitsu Ltd | Magnetic head |
JPH0284401A (ja) * | 1988-09-20 | 1990-03-26 | Asahi Chem Ind Co Ltd | 多孔性微小セルロース粒子 |
EP0415193A2 (en) * | 1989-08-17 | 1991-03-06 | Asahi Kasei Kogyo Kabushiki Kaisha | Finely divided suspension of cellulosic material and process for producing the same |
EP0460609A1 (en) * | 1990-06-07 | 1991-12-11 | Nisshinbo Industries, Inc. | Process for producing fine cellulose powder |
CN1081185A (zh) * | 1992-07-04 | 1994-01-26 | 苏志刚 | 用硫酸化废棉绒生产微晶纤维素工艺 |
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