CN107208373A - 制造微原纤化多糖的方法 - Google Patents
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Abstract
本发明涉及用于制造微原纤化多糖、优选微原纤化纤维素的方法。本发明还涉及能通过所述方法获得的微原纤化纤维素以及微原纤化纤维素的用途。制造微原纤化多糖的方法包括以下步骤:a)提供包含半纤维素的纸浆,b)提供木材降解酶,c)将所述纸浆与酶混合,d)将所述混合物保持在基本上圆柱状几何形状的连续、流动的系统中(例如塞流反应器),e)将所述混合物输送至一个或多个混合区以用于使所述混合物循环和均化,和f)在所述循环期间收获具有相对窄的尺寸分布微原纤化纤维素。
Description
技术领域
本发明涉及用于制造微原纤化多糖、优选微原纤化纤维素的方法,其中所述方法是无精磨机(磨浆机,refiner)的。本发明还涉及能由所述方法获得的多糖例如微原纤化纤维素以及所述多糖的用途。
背景技术
微原纤化纤维素(MFC)(其也称作纳米纤维素)是典型地由木纤维素纤维制成的材料。其也可由微生物源、农业纤维、溶解纤维素或CMC等制成。在微原纤化纤维素中,各个微纤丝(microfibrils)已经部分地或者完全地彼此脱离。
WO2013121108中公开了利用多次穿过(passages through)均化器并且将其在200–1000巴的压力下进行而制造MFC的方法。
另外,在WO2007091942中公开了使用精磨机制造MFC的方法。
因此需要如下的改进方法:其用于提供具有更均匀的尺寸分布(其相应地(inturn)为可预测的)的微原纤化多糖,然而同时可取消精磨机的使用,并且所述方法可在相对低的压力下运行。
发明内容
本发明通过提供根据第一方面的用于制造微原纤化多糖、优选微原纤化纤维素的方法解决了以上问题的一个或多个,所述方法包括以下步骤:
a)提供包含半纤维素的纸浆、优选化学纸浆,
b)提供一种或多种木材降解酶,
c)将所述纸浆与一种或多种木材降解酶混合,
d)将所述混合物保持在基本上圆柱状几何形状的连续、流动的系统中,
e)将所述混合物输送至一个或多个混合区以用于使所述混合物循环(环流,recirulate)和均化,和
f)在所述步骤e)的循环期间收获微原纤化多糖。
根据第二方面,本发明还提供能通过根据第一方面的方法获得的微原纤化多糖、优选微原纤化纤维素。
根据第三方面,本发明还提供根据第二方面的微原纤化多糖、优选微原纤化纤维素在强度添加剂、增稠剂、粘度调节剂、流变调节剂、清洁粉(去污粉,cleaning powder)、洗涤粉(washing powder)、清洁剂、泡沫组合物、阻隔物、膜、食品、药物组合物、化妆品、纸或板产品、涂料、卫生/吸收产品、乳液/分散剂、钻探泥浆、复合材料中,在水净化中,在过滤器中,在太阳能电池中,在电池(battery)中,在电子电路中,或者用于增强纤维素在制造再生纤维素或纤维素衍生物中的反应性的用途。
具体实施方式
在整个本说明书中表述“微原纤化多糖”意在涵盖任意类型的微原纤化纤维素、例如微原纤化纤维素纤维(纤维素材料)。所述纤维素也可为微原纤化纤维素(MFC)或者纳米纤维素、纳米原纤化纤维素(NFC)或者纤维素纳米纤丝(CNF)。所述纤维素可为漂白的或未漂白的。所述纤维素也可为结晶纤维素、MCC(微晶纤维素;由于其在药物组合物或者其它医疗用途中的潜在用途而具有高纯度需求)、BNC、NCC(纳晶纤维素;可用于电学应用并且具有磁性性质)、CNC、CMC(羧甲基化纤维素)或者合成聚合物纤维和由溶解纸浆制成的纤维。所述纤维素可以纸浆的形式存在,所述纸浆可为化学纸浆、机械纸浆、热机械纸浆或者化学(热)机械纸浆(CMP或CTMP)。所述化学纸浆优选为亚硫酸盐纸浆或硫酸盐纸浆(牛皮纸浆,kraft pulp)。在微原纤化纤维素中,各个微纤丝已经部分地或者完全地彼此脱离。MFC可用不同手段例如以机械方式或者以化学方式或者以酶方式、或者通过使用细菌、或者通过将例如化学和机械处理步骤组合而制成。
根据第一方面的方法中初始使用的纸浆可由来自阔叶木(硬木)、针叶木(软木)或两种类型的纸浆构成。所述纸浆可例如包含松树和云杉的混合物或者桦树和云杉的混合物。可用于本发明中的化学纸浆包括所有类型的基于木材的化学纸浆,例如漂白的、半漂白的和未漂白的亚硫酸盐、硫酸盐和碱法纸浆、以及这些的混合物。所述纸浆可为溶解类型的。所述纸浆还可包括纺织纤维。所述纸浆还可来自农业(例如土豆、竹子或胡萝卜)。
本发明还涉及能通过以上第一方面的方法获得的微原纤化多糖、例如微原纤化纤维素。已经显示,通过使用根据本发明第一方面的方法,可获得窄且可预测的尺寸分布并且同时取消精磨机的使用。此外,所述微原纤化多糖可在相对低的压力下制造。所述微原纤化多糖的尺寸分布也将类似于通过使用涉及精磨机的方法所制成的微原纤化多糖的分布。
另外,微原纤化纤维素纤丝通常非常细(~20nm)并且长度经常在100nm-10μm之间。然而,所述微纤丝还可更长,例如在10-200μm之间,但是由于宽的长度分布,可发现甚至2000μm的长度。已经原纤化并且在表面上具有微纤丝的纤维和分开的且位于浆料的水相中的微纤丝也包括在定义MFC中。此外,晶须也包括在定义MFC中。
所述微原纤化纤维素典型地由木纤维素纤维制成,如所述那样可使用阔叶木和针叶木纤维两者。其也可由微生物源,农业纤维例如麦秆纸浆、竹子或其它非木纤维源制成。其也可通过细菌生产或者由CMC制成。
根据本发明第一方面优选的实施方式,步骤f)中获得的微原纤化多糖具有相对窄的尺寸分布,优选其中所述分布类似于高斯曲线,最优选所述曲线的尺寸级别的端点分别在约1-5到约100-300μm,然而尤其优选同时在所述曲线的顶部的体积密度为约9.0-约10%,特别优选所述高斯曲线的尺寸级别的端点在约3-5到约200-300μm。
根据本发明第一方面优选的实施方式,在约0.5%的体积密度下的所述高斯曲线的尺寸级别的端点在约8到约100-200μm、或者在约1.0%的体积密度下的尺寸级别的端点在约9到约150-175μm、或者在约4.0%的体积密度下的尺寸级别的端点在约从15–20到100μm、或者所述特征的两个或者全部三个的组合,其中优选在约30–40μm的尺寸级别提供所述体积密度的峰。
根据本发明第一方面优选的实施方式,均化压力为约500巴或更高、优选约700-约1000巴。
根据本发明第一方面优选的实施方式,步骤d)、e)或f)的一个或多个中的压力保持约2-约6巴、优选约3-约5巴,最优选在步骤d)期间应用所述范围。
根据本发明第一方面优选的实施方式,圆柱状几何形状的连续、流动的系统为塞流反应器。基本上圆柱状几何形状的连续、流动的系统可进一步地为多边形形状(因此具有多边形几何形状)例如八边形形状。
根据本发明第一方面优选的实施方式,在收获所述微原纤化多糖之前,步骤e)中所述混合物的循环进行至少5次。
根据本发明第一方面优选的实施方式,使用至少两种输送手段例如管道进行步骤e)中所述混合物的循环,所述输送手段优选连接至所述系统并且顺序地连接,最优选通过泵和任选地另外一个混合罐互连。
根据本发明第一方面优选的实施方式,在1-5小时、优选2-4小时的期间将所述塞流反应器中的混合物保持在约50℃-约70℃的温度、优选在约60℃下和在2-6巴、优选3-5巴的压力。
根据本发明第一方面优选的实施方式,所述纸浆为亚硫酸盐纸浆、优选来自针叶木的纸浆。
根据本发明第一方面优选的实施方式,以0.1-500ECU/g纤维、优选0.5-250ECU/g纤维、最优选5-150ECU/g纤维、尤其优选50-150ECU/g纤维的浓度使用所述酶。
根据本发明第一方面优选的实施方式,其中所述酶为半纤维素酶或者纤维素酶或者其混合物。
根据本发明第一方面优选的实施方式,其中所述酶为纤维素酶、优选内切葡聚糖酶型纤维素酶、最优选单组分内切葡聚糖酶。
本发明各方面的优选特征加以细节上的必要修正同样用于其它方面的每一个。将本文中提及的现有技术文献在法律所允许的最完整程度上引入。在以下实施例以及附图中进一步描述本发明,其唯一目的是说明本发明并且绝不意图以任何方式限制本发明的范围。
附图说明
图1公开了使用根据本第一方面方法的设置,由此已经引入了将分开的间歇的酶处理与循环容器组合成连续工艺的塞流反应器。图1给出了根据第一方面的工艺设置的概述。通过塞流反应器的引入,可省略用于间歇的酶处理的分开的(单独的,separate)容器并且酶处理可以连续模式运行(e-处理的=酶处理的)。
图2公开了根据第一方面的方法的其它设置。图2显示作为根据第一方面的无精磨机MFC工艺设置的示意的一般工艺的其它优选实施方式。
图3公开了使用根据第一方面的方法制得的MFC。
图4公开了使用根据第一方面的方法制得的MFC的尺寸分布。黑色曲线(红色曲线)显示用根据本发明第一方面的无精磨机工艺生产的MFC通过激光衍射的尺寸分布,而灰色曲线(绿色曲线)显示在工厂批次生产的(produced at a plant batch)作为对比的MFC。
实施例
根据第一方面的方法仅具有两个步骤:将5%或更高固体物的纸浆与稀释在水中的酶(892-4816,AB Enzymes–以前称作)混合,使得纸浆的最终固体物为4%。在混合之前使所述纸浆和所述酶溶液两者均保持在60℃。该温度然后保持3小时而没有进一步混合。然后在循环模式中将该经预处理的材料在700巴下均化,使得温度升高至90℃,从而杀灭所述酶和潜在的微生物。如果温度达到90°之上C,则将所述材料冷却以避免沸腾。对所述循环容器加压并且使温度进一步提高,因此蒸汽可被闪蒸出来用于能量回收。
产生了粘稠(viscous)的MFC(参见图3),其表明高长径比材料并且通过激光衍射学的粒度分析表明与基于精磨机的预处理工艺相当的粒度分布,参见图4。该简化的工艺方案,因此根据本发明第一方面的工艺,更容易清洁和启动并且也更容易在均化阶段中保持杀菌温度。
与基于精磨机的预处理相比,用于MFC起始材料和酶的评估(evaluation)的时间也大幅减少。这也是由于该设计中降低的循环体积,在实质上减少了启动序列时间。
小结,在大型实验室规模以及在工业规模开发和实现了用于制造MFC的简化工艺。该简化的方案除了所述均化器之外仅具有两个容器,一个用于酶处理和一个用于进料、循环和混合。精磨段被完全省略。酶通过在均化步骤期间温度升高至90℃而变性(失活)。还可使用高的或者低的pH。
所述工艺设备容易清洁并且所述温度升高保证了产品的微生物纯度。
与目前的工艺相比,由于所述简化评判改善了可扩展性(可升级性、可量测性,scalability),并且因此,还改善了将所述工艺保持在高的卫生标准下的能力。
鉴于本发明的以上详述的描述,其它改动和变化对于本领域技术人员来说将变得明晰。然而,应明晰,这样的其它改动和变化可在不背离本发明的精神和范围的情况下实施。
Claims (15)
1.用于制造微原纤化多糖、优选微原纤化纤维素的方法,其包括以下步骤:
a)提供包含半纤维素的纸浆、优选化学纸浆,
b)提供一种或多种木材降解酶,
c)将所述纸浆与一种或多种木材降解酶混合,
d)将所述混合物保持在基本上圆柱状几何形状的连续、流动的系统中,
e)将所述混合物输送至一个或多个混合区以用于使所述混合物循环和均化,和
f)在所述步骤e)的循环期间收获微原纤化多糖。
2.根据权利要求1的方法,其中步骤f)中获得的微原纤化多糖具有相对窄的尺寸分布,优选其中所述分布类似于高斯曲线,最优选所述曲线的尺寸级别的端点分别在约1-5到约100-300μm,然而尤其优选同时在所述曲线的顶部的体积密度为约9.0-约10%,特别优选所述高斯曲线的尺寸级别的端点在约3-5到约200-300μm。
3.根据权利要求2的方法,其中在约0.5%的体积密度下的所述高斯曲线的尺寸级别的端点在约8到约100-200μm、或者在约1.0%的体积密度下的尺寸级别的端点在约9到约150-175μm、或者在约4.0%的体积密度下的尺寸级别的端点在约从15–20到100μm、或者所述特征的两个或者全部三个的组合,其中优选在约30–40μm的尺寸级别提供所述体积密度的峰。
4.根据权利要求1的方法,其中均化压力为约500巴或更高、优选约700-约1000巴。
5.根据权利要求1的方法,其中步骤d)、e)或f)的一个或多个中的压力保持约2-约6巴、优选约3-约5巴,最优选在步骤d)期间应用所述范围。
6.根据前述权利要求任一项的方法,其中所述基本上圆柱状几何形状的连续、流动的系统为塞流反应器。
7.根据前述权利要求任一项的方法,其中在收获所述微原纤化多糖之前,步骤e)中的所述混合物的循环进行至少5次。
8.根据前述权利要求任一项的方法,其中使用至少两种输送手段进行步骤e)中的所述混合物的循环。
9.根据前述权利要求任一项的方法,其中在1-5小时、优选2-4小时的期间将所述塞流反应器中的所述混合物保持在约50℃-约70℃的温度、优选在约60℃。
10.根据前述权利要求任一项的方法,其中以0.1-500ECU/g纤维、优选0.5-250ECU/g纤维、最优选5-150ECU/g纤维、尤其优选50-150ECU/g纤维的浓度使用所述酶。
11.根据前述权利要求任一项的方法,其中所述酶为半纤维素酶或者纤维素酶或者其混合物。
12.根据前述权利要求任一项的方法,其中所述酶为纤维素酶、优选内切葡聚糖酶型纤维素酶、最优选单组分内切葡聚糖酶。
13.根据前述权利要求任一项的方法,其中所述纸浆为亚硫酸盐纸浆、优选来自针叶木的纸浆。
14.能通过根据权利要求1-13任一项的方法获得的微原纤化多糖、优选微原纤化纤维素。
15.根据权利要求14的所述微原纤化多糖、优选微原纤化纤维素在强度添加剂、增稠剂、粘度调节剂、流变调节剂、清洁粉、洗涤粉、清洁剂、泡沫组合物、阻隔物、膜、食品、药物组合物、化妆品、纸或板产品、涂料、卫生/吸收产品、乳液/分散剂、钻探泥浆、复合材料中,在水净化中,在过滤器中,在太阳能电池中,在电池中,在电子电路中,或者用于增强纤维素在制造再生纤维素或纤维素衍生物中的反应性的用途。
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