CN101039961B - 纤维素醚的成形方法 - Google Patents

纤维素醚的成形方法 Download PDF

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Publication number
CN101039961B
CN101039961B CN2006800010257A CN200680001025A CN101039961B CN 101039961 B CN101039961 B CN 101039961B CN 2006800010257 A CN2006800010257 A CN 2006800010257A CN 200680001025 A CN200680001025 A CN 200680001025A CN 101039961 B CN101039961 B CN 101039961B
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cellulose
ether
compresses
carboxymethyl
pushed away
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CN101039961A (zh
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A·希尔德
M·O·施米特
A·阿尔特曼
B·兰格
W·奥泊曼
B·施里韦尔
H·蒂尔金
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Dow Global Technologies LLC
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Wolff Cellulosics GmbH and Co KG
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B11/00Preparation of cellulose ethers
    • C08B11/02Alkyl or cycloalkyl ethers
    • C08B11/04Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
    • C08B11/10Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
    • C08B11/12Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B11/00Preparation of cellulose ethers
    • C08B11/20Post-etherification treatments of chemical or physical type, e.g. mixed etherification in two steps, including purification
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/08Cellulose derivatives
    • C08J2301/26Cellulose ethers

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Crushing And Grinding (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

本发明涉及将纤维素醚推过多孔盘来制备纤维素醚的方法,所述纤维素醚相比已知纤维素醚具有更高的堆积密度和更均一的粒径分布。

Description

纤维素醚的成形方法
本发明涉及将纤维素醚推过多孔盘来制备纤维素醚的方法,所述纤维素醚相比已知纤维素醚具有更高的堆积密度和更窄的粒径分布。
在纤维素醚的制造过程中,成形步骤是影响产品性质的一个重要加工步骤。具体地说,该步骤可影响强度性质,例如级配曲线(grading curve)和堆积密度。
该步骤通常在清洗产品之后和干燥和研磨之前进行。
现有技术中,在水平振荡混合器中通过累积团聚来实现成形,从而使湿产品团聚、密实和压紧(参见例如DE2028310和DE3308420A1)。
该技术的具体缺陷是累积团聚取决于在混合器中的停留时间(这必然与制粒机的尺寸有关)相关,以及输入能源的可能是有限的。分割停留时间会得到不均匀的产品。所述团聚物仅疏松地粘在一起,因此可快速发生解团聚(disaggregation)。这会提高极细灰尘的实质比例,这对于某些等级是不利的。因此,对于堆积密度和分级曲线这类强度性质的影响能力是有限的。
因此,本发明的目的在于提供一种方法,所述方法能够将清洗后的纤维产品成形为高度压缩的、紧密颗粒(小球),这样就提高了堆积密度,且在随后的研磨过程中仅形成少量分级曲线低于所需粒径的颗粒(如果有的话)。另外,形成的颗粒应尽可能均一。且应不影响其它产品性能。
令人吃惊地是,已经发现上述目的可用如下方法达到,所述方法包括将纤维素醚推过多孔盘。
在本发明的一个实例中,将所述纤维素醚输送到包括垂直轴的设备中。固定盘连接到所述轴上,所述固定盘具有直径-长度比一定的穿孔。辊(碾子、轮、辊)在该盘上旋转,将纤维素醚推入所述穿孔,并压过所述穿孔。在盘下面,所述纤维素醚用旋转脱模器(stripper)分离,并分成小颗粒。
在本发明的另一个实例中,将所述纤维素醚推过平压模(也称为轮碾磨)的模子中的穿孔,在所述平压模中,旋转碾子(轮)在多孔模子(盘)上滚动。在模子的下面,用剪切装置将颗粒切成所需的长度。至少一个碾子在轮碾磨上滚动。通常有两个碾子,但是也可以超过两个碾子。这取决于单元的尺寸和碾子的直径。
但是,另一种可能性是,在笔直、多孔盘子上,轮(辊、碾子)在来回滚动时将纤维素醚推过模子,从而将其压紧。
所述纤维素醚在经过所述穿孔时压紧。通过穿孔的几何形状可调节压紧的程度。这可调节压紧工艺所必需的能量。成形体的截面形状由穿孔的截面形状决定。
如果是圆形穿孔的话,压紧的纤维素醚的密实性取决于压缩比P,P定义为模子中穿孔长度与穿孔直径的比例。压缩比P应为0.5-5.0,较好为2-4.0。
穿孔也可具有方形、矩形、椭圆形或不规则形截面。每单位面积盘中的穿孔数取决于盘的稳定性。
适合根据本发明方法进行加工的纤维素醚的例子是离子型和非离子型纤维素醚。离子型纤维素醚的例子可以是:羧甲基纤维素、羟乙基羧甲基纤维素、羧甲基磺乙基纤维素和磺乙基纤维素,较好为羧甲基纤维素。非离子型纤维素醚的离子可以是:羟乙基甲基纤维素、羟丙基甲基纤维素、羟乙基纤维素、羟丙基纤维素、乙基羟乙基纤维素和甲基纤维素,较好为羟乙基甲基纤维素和羟丙基甲基纤维素。
用本发明方法压紧的纤维素醚相比用现有技术处理的纤维素醚具有更高的堆积密度,并形成了更稳定的颗粒,但是其它性质是相同的。而且,粒径分布更均匀,用以表征粒径分布的筛网尺寸[mm]和分布函数[%]之间的相关系数K约为1.0,即几乎是线性关系。
用本发明方法压紧的有商业价值的纤维素醚的堆积密度通常为400-800g/l。这些纤维素醚的粒径分布通常为125-1000微米,且平均粒径为500微米。
用计量装置(例如螺杆、输送带)将未压紧的材料送入轮碾磨。也可以使轮碾磨处于惰性气氛,例如氮气或二氧化碳。下述实施例将描述本发明的方法,但并没有限制本发明的范围。
实施例
比较例(根据现有技术制备):
将产品CMC CRT 40000(取代度(DS)为0.9,产品含水量为42%,2%水溶液的粘度为40000mP·s)作为无醇纤维原料输送到水平混合机中,连续造粒。所得颗粒在间歇式设备中干燥,然后在装有筛分篮的冲击式研磨机中研磨成所需细度。将产物中大于1mm的部分筛分掉。
堆积密度为621g/l,低于0.125mm的比例为18重量%,K=0.979
实施例1(基于本发明)
产品CMC CRT 40000(产品含水量为42%)用本发明的方法代替水平混合机压紧造粒(6毫米穿孔,P=4),然后如上述干燥和研磨。
堆积密度为711g/l,低于0.125mm的比例为14重量%,K=0.995
实施例2(基于本发明)
产品CMC CRT 10000(产品含水量为40%,2%水溶液的粘度为10000mP·s)用本发明的方法代替代替水平混合机压紧造粒(6mm穿孔,P=3),然后如上述干燥和研磨。
堆积密度为680g/l,低于0.125mm的比例为12重量%,K=0.999

Claims (8)

1.一种制造纤维素醚的方法,所述方法包括将纤维素醚推过多孔盘,其特征在于,所用的压缩比P为2.0-4.0,并对压紧的纤维素醚进行干燥和研磨。
2.如权利要求1所述的方法,其特征在于,用一个或多个旋转的碾子将所述纤维素醚推过穿孔。
3.如权利要求1所述的方法,其特征在于,用一个或多个往复回转的轮将所述纤维素醚推过穿孔。
4.如权利要求1所述的方法,其特征在于,用辊将所述纤维素醚推过穿孔。
5.如权利要求1-4中任一项所述的方法,其特征在于,将所述压紧的纤维素醚在盘的下面分成所需长度的段。
6.如权利要求1-4中任一项所述的方法,其特征在于,所述压紧的纤维素醚选自:羧甲基纤维、羟乙基羧甲基纤维素、羧甲基磺乙基纤维素、磺乙基纤维素、羟乙基甲基纤维素、羟丙基甲基纤维素、羟乙基纤维素、羟丙基纤维素、乙基羟乙基纤维素或甲基纤维素。
7.用权利要求1-5中任一项所述的方法制得的产品。
8.如权利要求7所述的产品,其特征在于,所述产品是选自下组的压紧的纤维素醚:羧甲基纤维、羟乙基羧甲基纤维素、羧甲基磺乙基纤维素、磺乙基纤维素、羟乙基甲基纤维素、羟丙基甲基纤维素、羟乙基纤维素、羟丙基纤维素、乙基羟乙基纤维素或甲基纤维素。
CN2006800010257A 2005-02-03 2006-01-21 纤维素醚的成形方法 Expired - Fee Related CN101039961B (zh)

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DE102005004893.5 2005-02-03
DE102005004893A DE102005004893B4 (de) 2005-02-03 2005-02-03 Verfahren zur Formgebung von Celluloseethern
PCT/EP2006/000528 WO2006081955A1 (de) 2005-02-03 2006-01-21 Verfahren zur formgebung von celluloseethern

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BR (1) BRPI0605928A2 (zh)
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JP2012521785A (ja) * 2009-03-31 2012-09-20 ダウ グローバル テクノロジーズ エルエルシー ワイン用酒石酸塩安定剤
MX2016013830A (es) * 2015-10-27 2017-05-10 Shinetsu Chemical Co Eter de celulosa porosa no ionico soluble en agua que tiene excelente solubilidad y metodo para producir el mismo.

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US4044198A (en) * 1974-03-07 1977-08-23 Hoechst Aktiengesellschaft Method for cold-milling cellulose derivatives
US4507473A (en) * 1983-03-09 1985-03-26 Wolff Walsrode Aktiengesellschaft Process for the continuous granulation of carboxymethyl cellulose
US5100576A (en) * 1988-12-22 1992-03-31 Hoechst Aktiengesellschaft Process for the preparation of a readily soluble bleach activator granulate with a long shelf life
CN1237104A (zh) * 1996-09-12 1999-12-01 罗赫诊断器材股份有限公司 可迅速崩解的小药丸
CN1311258A (zh) * 2000-02-28 2001-09-05 沃尔夫瓦尔斯罗德有限公司 生产粒状水溶性纤维素衍生物的方法
CN1342168A (zh) * 1999-03-03 2002-03-27 沃尔夫瓦尔斯罗德有限公司 压实的松散漆原料的制备方法

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DE2038310C3 (de) * 1970-08-01 1982-04-01 Henkel KGaA, 4000 Düsseldorf Verfahren und Vorrichtung zur kontinuierlichen Herstellung reiner und trockener Carboxymethylcellulose
DE3038001A1 (de) * 1980-10-08 1982-05-06 Henkel KGaA, 4000 Düsseldorf Verfahren zur herstellung von mikropulvern aus celluloseether oder cellulose
US5488104A (en) * 1994-06-30 1996-01-30 The Dow Chemical Company Process for comminuting cellulose ethers

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US3054705A (en) * 1960-11-07 1962-09-18 Rayonier Inc Hydroxyethylcellulose pellets and process
US4044198A (en) * 1974-03-07 1977-08-23 Hoechst Aktiengesellschaft Method for cold-milling cellulose derivatives
US4507473A (en) * 1983-03-09 1985-03-26 Wolff Walsrode Aktiengesellschaft Process for the continuous granulation of carboxymethyl cellulose
US5100576A (en) * 1988-12-22 1992-03-31 Hoechst Aktiengesellschaft Process for the preparation of a readily soluble bleach activator granulate with a long shelf life
CN1237104A (zh) * 1996-09-12 1999-12-01 罗赫诊断器材股份有限公司 可迅速崩解的小药丸
CN1342168A (zh) * 1999-03-03 2002-03-27 沃尔夫瓦尔斯罗德有限公司 压实的松散漆原料的制备方法
CN1311258A (zh) * 2000-02-28 2001-09-05 沃尔夫瓦尔斯罗德有限公司 生产粒状水溶性纤维素衍生物的方法

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KR20070101236A (ko) 2007-10-16
CN101039961A (zh) 2007-09-19
DE102005004893A1 (de) 2006-08-10
DE102005004893B4 (de) 2011-02-10
EP1846456A1 (de) 2007-10-24
JP2008528773A (ja) 2008-07-31
US20060205935A1 (en) 2006-09-14
WO2006081955A1 (de) 2006-08-10
BRPI0605928A2 (pt) 2009-05-26

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