CN103691530A - 多元醇的微粉化 - Google Patents
多元醇的微粉化 Download PDFInfo
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- CN103691530A CN103691530A CN201310650226.1A CN201310650226A CN103691530A CN 103691530 A CN103691530 A CN 103691530A CN 201310650226 A CN201310650226 A CN 201310650226A CN 103691530 A CN103691530 A CN 103691530A
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Classifications
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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Abstract
公开了具有20-60μm的粒度分布(d50)和低于或等于5s/100g、优选低于5s/100g的流动性的微粉化多元醇。微粉化多元醇具有改进的流动性,虽然与相应研磨多元醇相比它们具有更小的粒度分布。最优选,该多元醇是麦芽糖醇,异麦芽糖醇,甘露糖醇,山梨糖醇,木糖醇和赤藓醇中的一种或多种。优选的多元醇还显示不少于40的压缩指数(%)。将多元醇微粉化的方法包括以下步骤:a)取多元醇,它具有化学式CnH2n+2On和它在20℃到25℃下是固体,b)将多元醇加入到喷射磨中并用氮气加压和c)收集微粉化多元醇。该微粉化多元醇可用于食品,饲料,化妆品和药物组合物,尤其口香糖组合物。
Description
本申请是于2010年1月26日进入中国,国家申请号为200880100640.2,国际申请号为PCT/EP2008/059834,发明名称为“多元醇的微粉化”的PCT申请的分案申请。
技术领域
本发明涉及多元醇的微粉化。获得了具有改进性能的多元醇并且能够用于食品,饲料,化妆品和药物应用领域中。
背景技术
根据不同的技术制备多元醇粉末。多元醇能够结晶,冷冻干燥的,挤出,喷雾干燥,或蒸汽聚结(steam-agglomerated)。
US 4,408,041,US 6,120,612,US 5,932,015全部涉及用于结晶麦芽糖醇的不同方法。
US 5,160,680描述了直接制备可压缩的粒化甘露糖醇的方法,其中甘露糖醇粉末进行挤出处理。
EP-A-1430887描述了用于治疗活性物质由吸入法给药途径中的可吸入粉末的制备方法。这些粉末是通过将具有17-50μm的平均粒度的粗粉末与具有2-8μm的平均粒度的细粉末混合来形成的。
WO 2004/067595A公开了制备微粒状多元醇例如麦芽糖醇的方法,该方法包括研磨干燥的组合物以得到约200-约2000μm的粒度。
WO 2006/127560A涉及包括多元醇的口香糖组合物。所公开的多元醇组合物的平均粒度是约30μm到约600μm。
此外已知的是使用微粉磨机生产具有10-50μm的粒度分布的乳糖粉末,“Sanitary Design Micronizer, USDA-accepted Jet Mills”,2005 STURTEVANT, INC。
目前需要简单的、成本有效的方法,它允许获得高质量的多元醇。
本发明提供此类方法。
发明内容
本发明涉及具有20-60μm的粒度分布(d50),和低于或等于5 s/100 g,优选低于5 s/100 g的流动性的微粉化多元醇。
本发明进一步涉及将固体多元醇微粉化的方法,该方法包括下面步骤:
a) 取固体多元醇,
b) 将多元醇加入到喷射磨中并用氮气加压,收集微粉化多元醇。
本发明进一步涉及含有本发明的微粉化多元醇的食品,饲料,化妆品或药物组合物,尤其涉及口香糖组合物。
具体实施方式
本发明涉及具有20-60μm的粒度分布(d50)和低于或等于5 s/100 g、优选低于5 s/100 g的流动性的微粉化多元醇。
虽然没有固定的定义,但是术语“微粉化”一般用于描述具有低于10微米的平均粒径的颗粒,通常大部分的颗粒是在2和5微米之间。 然而,本发明涉及不同的粒度分布和,在本发明的背景中,微粉化多元醇具有20-60μm的粒度分布(d50)。
测量流动性的试验已描述在实施例中。
本发明的微粉化多元醇与相应的研磨多元醇相比更有利。虽然微粉化多元醇具有比相应研磨多元醇更小的粒度分布(d50)更较小,但是令人吃惊地是它的流动性得到改进。
本发明的多元醇典型地是具有以下化学式的多元醇:
CnH2n+2On,并且还典型地在20℃至25℃之间的温度下是固体材料。
这一化学式对于氢化(还原)碳水化合物是典型的,但是本发明的多元醇不一定通过碳水化合物的氢化来获得。这些多元醇中的一些(例如赤藓醇)可通过其它化学过程和/或微生物过程或发酵来获得。
典型地,该多元醇选自丁糖醇中,戊糖醇,己糖醇,氢化二糖,氢化三糖,氢化四糖,氢化麦芽糖糊精和它们的混合物。
更具体地说,该多元醇可以选自赤藓醇,苏糖醇,***糖醇,木糖醇,核糖醇,蒜糖醇,阿卓糖醇(altritol),古洛醇 (gulitol),半乳糖醇,甘露糖醇,山梨糖醇,塔罗糖醇,麦芽糖醇,异麦芽糖醇(isomaltitol),异麦芽糖醇(isomalt),乳糖醇,和它们的混合物。
在优选的实施方案中,该多元醇选自麦芽糖醇,异麦芽糖醇,甘露糖醇,山梨糖醇,木糖醇,赤藓醇和它们中的一种或更多种的混合物。在更特定的实施方案中,该多元醇是赤藓醇或甘露糖醇。
本发明的微粉化多元醇进一步体现特征于它具有等于或高于40的压缩指数。压缩性指数已描述在实施例中。
根据特别优选的实施方案,本发明涉及具有20-60μm的粒度分布(d50),和低于或等于 5 s/100 g,优选低于5 s/100 g的流动性的微粉化赤藓醇。本发明进一步具有高于40的压缩指数。
根据不同的优选实施方案,本发明涉及具有20-60μm的粒度分布(d50),和低于或等于5 s/100 g,优选低于5 s/100 g的流动性的微粉化甘露糖醇。本发明进一步具有高于40的压缩指数。这一压缩指数使得它成为在片剂中使用的潜在候选者。
本发明进一步涉及将多元醇微粉化的方法,该方法包括下面步骤:
a) 量取具有化学式CnH2n+2On的多元醇,它在20℃到25℃之间的温度下是固体材料,
b) 将多元醇加入到喷射磨中并用氮气加压,
c) 收集微粉化多元醇。
喷射磨包括任何设备,它允许颗粒状材料的微粉化,尤其,多元醇的微粉化。典型地,合适设备是允许由机械法降低粒度并且能够获得具有20-60μm的粒度分布(d50)的微粉化多元醇的一种设备。更典型的设备能够包括喷射磨,如螺旋喷射磨机(spiral jet mill)和相对的喷射磨。典型的合适设备包括外圆研磨腔(cylindrical grinding chamber),通过位于腔壁周围的喷嘴在腔中引入高速气体。所要微粉化的颗粒状材料被引入到由压缩气体推进的研磨腔室,并且在腔室内,利用高速气体在其中的引入沿着腔室的内壁加速。气体在腔室内的运动导致涡旋(vortex)的产生,在涡旋内夹含颗粒状材料。因此引起颗粒状材料的颗粒在它们之间发生反复的碰撞,和结果,颗粒状材料的粒度分布(d50)会下降。减少尺寸的颗粒,即微粉化产品,被排放气体携带离开该腔室,并且,典型地,被通入到合适的旋风过滤器中。
微粉化产品的粒度分布主要由腔室中的气体压力和固体颗粒状材料加入到研磨腔室中的进给速率所决定。
微粉化目前主要用于工业领域(在水泥或漆用颜料的生产中)和用于生产固体吸入产品的制药工业中。在这些用途中,目标是生产超细粉末(例如在1至10μm之间,或甚至更小的粒度)。为了能够获得这样小的粒度,需要非常高的气压(>7巴)。
本发明已经表明通过施加氮气获得合适的产品。
本发明涉及生产多元醇的微粉化粉末,它特别可用于可食用的产品如食品或饲料组合物的制造中,或用于化妆品或药物配制剂的制造中。此类应用要求该微粉化多元醇具有优选20-60μm的粒度分布(d50)。为了实现该粒度,使用合适的气压,典型地为2-6巴。其粒度已根据本发明的方法被减少的饲料多元醇(feed polyol)具有在50至500μm之间的起始粒度分布(d50)。
在本发明中,我们通过使用从Nuova Guseo S.r.l.商购的Micronet M100喷射磨或从Sturtevant Inc商购的超微粉碎机(Micronizer)喷射磨获得良好的结果。在进行本发明时,干燥颗粒多元醇典型地通过文丘里注射器被加入到喷射磨的研磨腔室中并且通过加压的干燥氮气传输。优选,进给速率是在0.5-7 kg/小时范围内(在10 cm直径腔室中)。该颗粒状多元醇利用高速干燥氮气注入到腔室中,从而在喷射磨的环形腔室内被加速成涡旋。在磨机的腔室中在气压作用下所引起的反复颗粒与颗粒冲击能够将多元醇颗粒研磨到所需粒度。
所获得的微粉化多元醇具有优异的性能。例如,因为粒度减小是在没有外部施加热量和不需要使用任何加工助剂(它们通常在颗粒的微粉化中使用)的情况下实现的,产品不会受到污染。此外,通过在喷射磨中使用干燥惰性气体,微粉化产品被干燥和因此在贮存过程中不易形成团块。
在普通锤磨机上微粉化的优点包括以下发现:微粉化的精细粉末显示出好得多的流动性质(流动性)和在贮存中的稳定性(在3个月贮存之后没有团块-没有任何抗结块剂添加)。 微粉化还改进糖果(confectionery)应用和/或药物应用,例如口香糖组合物或片剂。
本发明进一步涉及含有根据本发明的微粉化多元醇、优选微粉化甘露糖醇的口香糖组合物。包括本发明的微粉化甘露糖醇的口香糖组合物的附加特性是口香糖组合物的改进的硬度。更具体地说,它在生产后的24小时具有等于或高于3500 g,优选高于4000 g的硬度。
本发明进一步通过下面的实施例来举例说明。
实施例
实施例1
具有67μm的平均粒度的结晶甘露糖醇通过使用干氮气流被输入到具有10 cm直径研磨腔室的超微粉碎机中。结晶甘露糖醇加入到微粉磨机中的进给速率是3.1 kg/每小时。干氮气通过喷嘴被注入到腔室中来维持2巴(2×105 Pa)的腔室内气压(P2)。获得一致具有33μm的平均粒度的干燥、自由流动微粉化的甘露糖醇。
实施例2
重复实施例1中所述的步骤,只是加入到微粉磨机中的结晶甘露糖醇具有82μm的平均粒度,进给速率是1.1 kg/每小时和在磨机的腔室中N2的压力(P2)是1.5巴。微粉化产品再次具有33μm的平均粒度。
在两种不同的粒度下的结晶甘露糖醇的进给速率的影响示于下表1中。
表1
结晶甘露糖醇
进口微粒(μm) | 出口微粒(μm) | N2 进气(P1)(巴) | N2 微粉化(P2)(巴) | 螺杆转速(rpm) | 速率(kg/h) |
67 | 52 | 2 | 1 | 30 | 2.9 |
67 | 33 | 2 | 2 | 30 | 3.1 |
67 | 24 | 2 | 2 | 20 | 1.7 |
82 | 46 | 2 | 2 | 30 | 3.2 |
82 | 33 | 2 | 1.5 | 10 | 1.1 |
82 | 26 | 2 | 2 | 20 | 0.6 |
根据以上实施例1和2所获得的甘露糖醇的微粉化颗粒在干燥条件下贮存三个月,在这一段时间之后在产品中没有观察到团块形成。所获得的微粉化甘露糖醇颗粒适合用于口香糖的制造中,同时适合用于胶基(gum base)的制备中和用于口香糖的涂层的制备中。
实施例3
使用与以上实施例1中所述的类似的步骤,其它多元醇按照在下表2中所示成功地微粉化。
表2
其它多元醇
产品 | 进口微粒(μm) | 出口微粒(μm) | N2进气(P1)(巴) | N2微粉化(P2)(巴) | 螺杆转速(rpm) | 速率(kg/h) |
结晶麦芽糖醇(C* Maltidex CH 16385) | 180 | 38 | 5 | 5 | 20 | 4.1 |
麦芽糖醇HP粉末 | 200 | 33 | 5 | 5 | 27 | 2.8 |
结晶赤藓醇(C* Eridex 16954) | 400 | 61 | 4 | 4 | 30 | 6.0 |
山梨糖醇粉末(C* Sorbidex S16603) | 220 | 40 | 5.8 | 5.8 | 10 | 1.4 |
根据实施例3制备的微粉化赤藓醇根据所述的试验步骤进一步分析它的流动性和压缩指数(%)。
压缩性指数(%)是粉末的几种性质的量度:堆积密度,粒度和形状,表面积,水分含量和内聚性。所有这些能够影响到所观察到的压缩指数。
根据本发明的微粉化多元醇的样品的压缩性指数(%)是根据下列步骤测定的。
将100g的多元醇粉末的样品放入到250ml量筒中。记录在量筒中未沉降(unsettled)粉末的表观容积(Vo)。含有粉末样品的量筒然后以机械方式轻拍,引起量筒中的粉末沉降。继续轻拍,直至没有观察到由于沉降引起的进一步体积变化为止。在轻拍结束之后记录在量筒中的沉降粉末的最终容积(Vf)。
通过使用所观察到的Vo和Vf,根据以下方程式计算压缩指数(%):
使用三次测定值的平均值。
粉末的流动性是作为物料通过孔的流动速率测量的。它能够仅仅用于具有一定流动能力的材料并且因此无法用于内聚性材料。
根据本发明的微粉化多元醇的样品的流动性(s/100g)是根据下列步骤测定的。
装置
所使用的装置是从Pharma Test Apperatebau, Hainburg获得的Pharma Test PTG-1。该装置包括流动漏斗(flow funnel),在该漏斗的底部具有喷嘴(孔)和内部提供有搅拌器。 该流动漏斗垂直地悬挂在天平上提供的容器之上。该装置提供不同直径例如10mm,15mm和25mm的孔的选择。搅拌器能够用于帮助粉末通过喷嘴并且能够在5-25 rpm的速度下使用。
将微粉化多元醇的样品放入到流动漏斗中。在这一试验步骤中使用的孔直径是25mm。搅拌器在试验步骤中以25 rpm的速度运转。喷嘴打开,并记录100g样品流过喷嘴进入容器中所花费的时间。
三个测量值的平均值用于各样品。
对于流动性和压缩指数(%)所获得的结果示于下表中。
样品 | 流动性 (s/100 g) | 压缩指数 (%) |
细磨的赤藓醇 | 6.5 | 38.8 |
根据本发明的微粉化赤藓醇 | 4.8 | 41.1 |
实施例4 - 口香糖制备
下列配方用于制备口香糖。
配方:
成分 | %(商购基础(commercial base) ) | 干重(g) |
口香糖基料 | 36.30 | 23.60 |
山梨糖醇 (Cargill-C*Sorbidex S16603) | 33.70 | 21.91 |
根据本发明的微粉化甘露糖醇 | 20 | 13.00 |
麦芽糖醇 (Cargill-C*Maltidex L16303) | 8.50 | 5.53 |
薄荷香料 | 1.50 | 0.98 |
总计 | 100.00 | 65.00 |
与标准甘露糖醇和细磨的标准甘露糖醇相比,微粉化甘露糖醇的粒度分布和流动性示于下表中。
根据本发明微粉化的甘露糖醇 | 标准甘露糖醇(16705) | 细磨的标准甘露糖醇 | |
粒度(d50) | 43.71 μm | 77.21 μm | 34.17 μm |
流动性喷嘴25 mm ,伴随搅拌 | 4.6 sec / 100g(在制备后1年测量的样品) | 4.3 sec/100g | 7.4 sec / 100g |
再次测量在贮柜中在40%相对湿度下贮存一年后的微粉化甘露糖醇的流动性。在贮存之后没有观察到物料的流动性的变差。
口香糖组合物被成形为片,它们在室温下和在40%相对湿度的贮柜中贮存。
口香糖片的质量进一步通过测量口香糖片的硬度来测定。为了对比,使用其中采用标准细磨甘露糖醇代替本发明的微粉化甘露糖醇的组合物所制得的片也进行了该试验步骤。
硬度测量
设备:Texture Analyser Profile TA_XTPlus
TA-XTPlus设定值:
模式:测量压缩中的力
选项:回到起始
预试验速度:0.8 mm/s
试验速度:0.8 mm/s
后试验速度:3.0 mm/s
距离:2mm
接触力模式(Trigger Force Type):30.0g
数据获取速率:250pps
附件:2mm 圆柱形探针(P/2),使用25kg负荷传感器
具有空白板的重载工作台(HDP/90)
试验设定:将重役平台安装到机器底座之上。将样品口香糖片放置在平台上,在探针下居中,并且开始试验。
观察结果:探针接近样品和一旦达到30.0g接触力,观察到力的急剧增长,因为探针刺入该口香糖片中。当达到从触发点计的2mm的穿透距离时,探针回到它的原始的起始位置。 平均穿透力是作为硬度的指标测量的。
对于在制备后在室温(22℃)下在空调的房间中贮存24小时,一个星期和一个月的口香糖片的样品,在环境温度下进行试验。结果显示如下。
Claims (2)
1. 将固体多元醇微粉化的方法,该方法包括下面的步骤:
a) 取固体多元醇,
b) 将该多元醇加入到喷射磨中并用氮气加压,其中在喷射磨中施加的压力是在2巴到6巴范围内,
c) 收集微粉化多元醇,
和其中固体多元醇选自赤藓醇,苏糖醇,***糖醇,木糖醇,核糖醇,蒜糖醇,阿卓糖醇,古洛醇,半乳糖醇,甘露糖醇,山梨糖醇,塔罗糖醇,麦芽糖醇,异麦芽糖醇,异麦芽糖醇,乳糖醇和它们中的两种或更多种的混合物;
其中该微粉化多元醇具有在20μm至60μm范围内的平均粒度和低于或等于5 s/100 g、优选低于5 s/100 g的流动性。
2. 根据权利要求1的方法,其中固体多元醇选自麦芽糖醇,异麦芽糖醇,甘露糖醇,山梨糖醇,木糖醇,赤藓醇和它们中的两种或更多种的混合物。
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AU2008281850B2 (en) | 2013-10-10 |
DK2264042T3 (da) | 2012-08-20 |
EP2264042A1 (en) | 2010-12-22 |
US20100255307A1 (en) | 2010-10-07 |
AU2008281850A1 (en) | 2009-02-05 |
PL2264042T3 (pl) | 2012-10-31 |
JP5547068B2 (ja) | 2014-07-09 |
WO2009016133A1 (en) | 2009-02-05 |
CN101765606A (zh) | 2010-06-30 |
ES2388494T3 (es) | 2012-10-15 |
CA2694280A1 (en) | 2009-02-05 |
BRPI0814175A2 (pt) | 2015-01-20 |
RU2479587C2 (ru) | 2013-04-20 |
JP2010534637A (ja) | 2010-11-11 |
EP2183262A1 (en) | 2010-05-12 |
EP2264042B1 (en) | 2012-07-18 |
RU2010107188A (ru) | 2011-09-10 |
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