CN1422299A - 基于泡沫淀粉的成型片材和产品 - Google Patents
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- CN1422299A CN1422299A CN01807894A CN01807894A CN1422299A CN 1422299 A CN1422299 A CN 1422299A CN 01807894 A CN01807894 A CN 01807894A CN 01807894 A CN01807894 A CN 01807894A CN 1422299 A CN1422299 A CN 1422299A
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Abstract
本发明涉及一种泡沫塑料片材形式的材料，其中包括作为连续相膨胀的改变结构的或复合的淀粉，材料密度为20－150kg/m3，蜂窝尺寸为25－700μm，蜂窝的分布是，在未拉伸的情况下，80％的蜂窝尺寸为20－400μm。
Description
发明背景
本发明涉及一些半成品如不同厚度的片材和型材，它们基于改变结构的和/或复合的淀粉，这些淀粉是采用挤压方法膨胀的，在采用各种方法处理后，可作为可生物降解的产品使用，这些淀粉可在挤出头的出口或在随后的阶段成型，生产成型的产品。
根据本发明的淀粉基产品，特别适合在包装领域中使用。
直到目前为止，聚苯乙烯、聚氨酯、聚乙烯、和聚丙烯等塑料材料在包装领域的应用仍占主要地位；然而，与这些产品有关的废物处置问题正为淀粉基材料展示出新的前景，特别是在泡沫塑料材料领域，因为它们是可生物降解的，并来自可更新的来源。
目前的技术状态表明了制造淀粉基泡沫塑料产品有各种不同的方法。然而，由于淀粉的性质和特征，在半成品的尺寸、蜂窝分布、和密度方面，成功地获得具有最佳性能的淀粉基泡沫塑料产品，以便采用常规方法以工业速率将半成品转化成具有竞争性的产品，就重量和性能而言，特别是就产品折合处的脆性而言还成问题。而用于制造片材和相关的模塑制品的淀粉基泡沫塑料的制备，却是特别理想的。
特别是，在市场上已经可以买到在连续相中含有淀粉的非淀粉基半成品，这种半成品可以采用工业方法成型，在尺寸、蜂窝分布、和密度方面具有最佳性能，如此获得的产品，即使在经过一系列的折合之后，特别是在折合区域仍有弹性。
迄今为止，人们的大部分注意力，实际上一直集中在研究和利用包含与各种合成聚合物和添加剂组合的各种淀粉基组合物而对能生产性能完全确定的泡沫塑料产品的挤出和发泡方法上的问题，例如泡沫塑料结构的均匀性、表面的光滑度、和泡沫塑料加工件的低脆性，却只受到有限的关注。
原料组会物
根据本发明的产品，是从供给挤压机的原料组合物获得的，其中包含淀粉材料、占组合物总重量4-30％的水、和可以使用的热塑性聚合物和其它添加剂如增塑剂、润滑剂、表面活性剂、和弱酸等。就原料组合物的成分而言，在本申请中引入欧洲专利申请EP/0 696 611的内容作为参考。
本发明尤其涉及发泡的半成品，例如各种厚度的片材和其本身可以用作产品的型材，以及相关的成形或成型的产品，其中包括在半成品和成品本身中作为连续相的改变结构和/或复合的淀粉。
就淀粉材料而言，这些淀粉可能是粗制淀粉和改性淀粉，或它们的混合物。优选采用土豆、小麦、玉米和木薯淀粉。就改性淀粉而言，可以是利用物理和化学方法改性的淀粉，例如乙氧基化的淀粉、乙酸酯淀粉、丁酸酯淀粉、丙酸酯淀粉、羟丙基化的淀粉、阳离子淀粉、氧化的淀粉、交联的淀粉、凝胶化的淀粉、与能获得“V”形复合物的分子和/或聚合物复合的淀粉、糊精化的淀粉、和与如聚酯、聚氨酯、聚酯型氨基甲酸酯、聚脲、聚酯脲、聚硅氧烷、硅烷、钛酸酯、和脂肪链等接枝的淀粉。优选的化学或物理改性的淀粉，是任一种改性类型的淀粉，在30℃下在DMSO中测定，其固有粘度为2dl/g-0.6dl/g，优选1.5dl/g-0.8dl/g，更优选1.3dl/g-1dl/g。
这意味着，从磨坊加工排料获得的各种粉末和细粒，也在本发明的范围内。
术语改变结构的淀粉系指在其成分的玻璃转化温度和熔化温度以上热处理过的淀粉，以达淀粉颗粒的分子结构秩序紊乱，使其成为热塑性的。在这方面可以参考专利EP 118240和EP 327505。
另一方面，复合淀粉系指其中的直链淀粉成分部分或全部参与形成“V”型复合物的淀粉(单螺旋结构)，这种复合物具有二阶导数X-射线光谱和FTIR特性。
关于热塑性聚合物，熔点或玻璃转化点在60-175℃的聚合物，特别是熔点或玻璃转化点在70-110℃的聚合物特别适合根据本发明的产品。
特别适合使用的聚合物，选自：—— 天然来源的聚合物，可以是改性的，也可以是未改性的，特
别是从纤维素衍生的聚合物如取代程度为1-2.5的乙酸纤
维素、丙酸纤维素、丁酸纤维素、和它们的共聚物；烷基纤
维素类型的聚合物、羟烷基纤维素、羧烷基纤维素、特别是
羧甲基纤维素、硝基纤维素和脱乙酰壳多糖、支链淀粉
(pullulan)、或酪蛋白和酪蛋白酸酯、玉米蛋白、大豆蛋
白质、藻酸和藻酸酯、天然橡胶、天冬氨酸酯、和谷蛋白；—— 合成或发酵来源的可生物降解的聚合物，特别是聚酯，例如
C2-C24脂肪族羟酸或它们相应内酯或交酯的聚合物或共聚
物，特别是具有各种D/L乳酸比例的乳酸聚合物，优选D-
乳酸的含量为4-25mol％，聚乳酸与脂肪族聚酯和芳香族-
脂肪族聚酯的共聚物，聚己内酯，聚戊内酯，它们的共聚物，
从二官能酸和脂肪族二元醇衍生的聚酯，脂肪族-芳香族聚
酯，特别是不论是否用链增长剂处理过的亚烷基-对苯二甲
酸酯己二酸酯类型的共聚物，优选对苯二甲酸的量小于40
mol％，优选小于30mol％，一般为环氧树脂，特别是双
酚型树脂；—— 能使淀粉反应生成复合物的聚合物，也就是包含加在疏水链区
中的亲水性基团的聚合物，例如乙烯-乙烯醇(ethylenevinyl
alcohol)共聚物、乙烯-乙酸乙烯酯共聚物、丙烯酸酯、乙
烯-丙烯酸酯共聚物、乙烯与丙烯酸、甲基丙烯酸、巴豆酸、
衣康酸等不饱和酸的共聚物；具有醇和羧酸官能团的脂肪族
聚酯和/或脂肪族-芳香族聚酯的共聚物，环氧树脂，其中包
括包含双酚树脂的环氧树脂。—— 与淀粉生成氢键的聚合物，特别是各种水解程度的聚乙烯
醇，可改性成丙烯酸酯或甲基丙烯酸酯，和为了降低熔点而
初步增塑或改性的聚乙烯醇。
优选的热塑性聚合物是聚乙烯醇，烯烃单体共聚物，优选乙烯与选自下列单体的共聚物，这些单体是乙烯醇，乙酸乙烯酯，丙烯酸和甲基丙烯酸，从己内酯衍生的脂肪族聚酯，聚亚烷基琥珀酸酯，壬二酸、癸二酸、巴西基酸的聚合物和它们的共聚物，脂肪族聚酰胺，聚亚烷基癸二酸酯，聚亚烷基壬二酸酯，和聚亚烷基巴西基酸酯，特别是乙烯与包括C2-C13的二元醇、包含二聚酸类的聚酯、聚亚烷基对苯二甲酸酯己二酸酯类型的芳香族-脂肪族聚合物和环氧树脂，特别是具有双酚基团的环氧树脂形成的共聚物。
根据本发明，挤出的发泡半成品还优选包含成核剂。应用适宜的成核剂，实际上能提高片材中蜂窝的均匀性。在加工过程中成核剂的用量，取决于加工条件和挤出的半成品所需的结构。优选成核剂的量相对原料组合物为0.05-10重量％，优选0.5-7重量％，更优选1-5重量％。
可以使用的成核剂是无机化合物如滑石(硅酸镁)、碳酸钙、钠和钡等的硫酸盐、和二氧化钛等，可以采用如硅烷、钛酸酯等粘合促进剂处理表面。也可以采用有机填料和纤维如木材粉末、纤维素粉末、葡萄的残余物、糠、玉米皮、和其它天然纤维，含量为0.5-20％。为了改善刚性、水和气体的渗透性、和尺寸的稳定性，可以使用另一些能被分散和/或压缩在亚微尺寸薄层中的材料，优选小于500μm，更优选小于300μm，甚至更优选小于50μm。特别优选沸石和各种类型的硅酸盐如分子能与淀粉反应的官能化的硅灰石、蒙脱石、和水滑石(hydrotalcytes)。特别优选的是亚微颗粒的复合淀粉，其中具有由硅烷、钛酸酯等引入的特殊官能团。
此外，原料组合物还可以包含适宜的添加剂如润滑剂和/或分散剂、阻燃剂、着色剂、增塑剂、和填料等。特别是食用油，例如棕榈、玉米、大豆、和葵花油是特别优良的，它们是C12-C22的脂肪酸类和它们不同取代程度的甘油酯，特别是加氢合成的脂肪或动物来源的脂肪，这些脂肪至少在环境温度下，优选在环境温度以上是固体，以改善防潮性能和降低可湿润性。也可以采用弱酸类如乳酸、酒石酸、柠檬酸等，以在挤出过程中调节淀粉的粘度，也可以采用增塑剂如甘油、山梨醇、甘露糖醇、季戊四醇、和它们的衍生物、柠檬酸的酯类和它们的衍生物。
可将原料组合物直接供给挤压机，也可以以初步挤压过的或成丸的团粒的形式供给挤压机。片材的生产方法
根据本发明的泡沫塑料半成品可采用特定的挤压机进行基本淀粉组合物的挤出过程制备，例如采用缓慢的双螺杆挤压机，或二个单螺杆阶式串联挤压机或它们的组合，采用这种方法，能保证相当长的保压时间，使淀粉材料的粘度和成核剂的均匀性达到最佳状态，以及发泡剂在熔融体中的混合。特别优选采用缓慢型双螺杆挤压机。
在挤出过程的操作性能中，挤出温度可随具体的配方、所需半成品和成品的性质而改变。因此控制熔融体的温度对获得具有指定特性的产品是重要的。
在挤压过程中熔融体的温度沿螺旋分布，一般可从50℃变化到230℃，优选从60℃变化到210℃，更优选从70℃变化到200℃。
根据本发明，热塑性产品的发泡是采用适宜的物理发泡剂的混合物进行的，物理发泡剂也可以包含化学发泡剂。特别优选使用气体形式的CO2与水组合，或气体形式的CO2与水或其它物理和化学的发泡剂组合。在化学发泡剂中，还可以考虑柠檬酸、酸式碳酸盐、和它们的组合。
优选将发泡剂加入挤压机中的供料组合以熔融状态存在的区域。特别是将发泡剂加到挤压机的前置区域，采用这种方式，挤压过程不受熔融体向挤压机加料区域返回现象的影响。
向熔融体温度为100℃-200℃，优选130℃-190℃的区域加入CO2，相对加到加料漏斗中的总组合物量，其含量大于0.4重量％，优选大于0.8重量％。CO2和H2O的混合物以及比浓度(specificconcentrations)对低密度和蜂窝结构是决定性的因素。
CO2量可在0.4重量％-10重量％范围内变化，优选0.8重量％-7重量％，更优选1重量％-4重量％。将CO2加到熔融体中。为了膨胀，加到挤压机加料漏斗中的组合物的总含水量为4重量％-30重量％，优选8重量％-20重量％，更优选10重量％-18重量％。
挤压机可配备扁平的或管型的挤压机头；特别优选管状的挤压机头。
优选挤压机头具有能保证均匀地向喷嘴供料的结构。这个问题与根据本发明的泡沫塑料片材原料组合物有关，因为剪切速率很小的变化会使局部粘度可能产生相当大的变化，随后发泡过程发生变化，因而清楚地表明，片材的厚度、蜂窝尺寸、和优先塑变等会不一致。
因此挤压机头优选以这样的方式构成，以消除材料的弹性记忆，同时在材料进入喷嘴之前，不产生任何泡沫。就片材而言，优选的挤压剪切速率为500-50000s-1，优选800-40000s-1，更优选900-35000s-1。
在挤出头的出口，在成型过程之前，本发明的泡沫塑料片材可以与无纺织物、纺织物、纸、可生物降解的或不能生物降解的膜、或铝层层压成叠层。就无纺织物或纺织物而言，这些材料可由天然纤维制成，例如黄麻、棉花、和羊毛纤维，基于多糖的纤维，例如乙酸纤维素、淀粉乙酸酯、和粘胶丝等，或由可生物降解的聚合物生产的纤维，特别是脂肪族聚酯如聚乳酸、聚己内酯、二元醇和二元酸的聚亚烷基羧酸酯，二元酸选自直链C2-C13二元酸，和/或脂环族、脂肪族-芳香族聚酯，特别是聚亚烷基对苯二甲酸酯己二酸酯(terephthalatepolyalkylene adipates)家族的脂肪族-芳香族聚酯和它们的共聚物，特别是相对于对苯二甲酸+己二酸，对苯二甲酸含量小于55％的聚酯，聚酰胺，特别是基于己内酰胺、脂肪胺等的聚酰胺，脂肪族聚氨酯，聚酯型氨基甲酸酯，聚脲，和环氧树脂。对于叠层或覆层，也可以以膜的形式使用上述可生物降解的聚合物。
一般是通过温度和/或施加适宜的可生物降解的粘合剂，和热熔融体，特别是基于脂肪族聚酯的热熔融体，将膜偶合到片材上，可生物降解的粘合剂是基于聚合物，乳酸，聚氨酯，聚乙酸乙烯酯和聚乙烯醇，蛋白质如酪蛋白和谷蛋白，淀粉和其它多糖的粘合剂。
这些膜可采用浇注或发泡成膜(bubble film-forming)方法制备，也可与泡沫塑料载体的附着面共挤出。优选膜的熔点高于60℃，优选高于80℃，更优选高于100℃。
与膜偶合的半成品，在未成型时，可以用作那样的片材，也可以采用发泡或成型方法制成成品。
对于涂覆，可以采用在欧洲专利EP 696612中所述类型的乳化物、溶液、或分散体处理包括在本发明中的被研究的膨胀颗粒。根据用途，还可以使用熔点高达120℃的天然和合成的蜡。在这种情况下，处理可以在成型或成形阶段之前或之后进行。
泡沫塑料片材也可以与其它淀粉基材料的膨胀层共挤出，以在多层的内部和外部之间具有差异性，或者泡沫塑料片材与上述的如聚酯类亲水性较低的材料层共挤出，制成层压膜。
根据本发明的泡沫塑料片材，必须从均匀的熔融体开始制备，其中成核剂和气体和/或蒸汽均匀地分散在整个熔融体中。为此挤压机中的保压时间应为5-40分钟，优选10-35分钟，更优选15-25分钟。
泡沫塑料片材的厚度，可利用挤压条件和压延作用控制。
在管状片材的情况下，和采用发泡成膜方法的情况一样，可在挤出头内安装吹风或吹蒸汽的系统，或由吹风或吹蒸汽的方位使片材膨胀，获得在双轴方向上的伸长，避免或限制波浪形的生成。片材的厚度可以为0.5mm-15mm，优选1.0mm-10mm。可以通过对片材的拉伸和压延，使半成品达到该厚度。
可以使泡沫塑料片材成波纹状，利用波纹提高泡沫塑料的缓冲性能。波纹可具有不同的宽度和高度。相应所制片材的厚度，其高度可为泡沫塑料片材厚度的约2倍。在每米直线距离上，波纹的个数可达350个。
可将这种类型的片材以多层的形式组合起来，对包装领域的不同产品，制成不同的几何形状，例如片材、高弹性的膨胀块、弯头、或保护容器。适合应用的领域的具体实例是家用电器设备领域、电子产品、食品领域、药物、装置和家具、邮购、和快件的包封物。也可以利用这些片材与其它的载体组合，制成与木材、纸、特等纸板、天然和合成纤维织物、铝和其它金属混合的多层片材。特别是利用它们在增湿时的特征粘性，或优选采用喷洒热熔融体或融体，可将这一类产品直接固定在被包装件上。
从偶合片材获得的产品或成型产品，可以采用外加的膜保护，以增强性能。
产品也可以是通过粘结和胶合片材或采用直接挤出的管状物获得的卷筒和管，卷筒和管可以用作手纸、厨房用纸、或其它类型用纸的载体，也可以用作瓶子等圆筒状物的保护物。片材的成型方法
可以采用连续方法或间歇方法进行成型。
采用连续方法生产根据本发明的膨胀产品，需设置挤出/压延阶段，可能的调整阶段，和连续的成型阶段。采用间歇方法生产根据本发明的泡沫塑料产品，需设置挤出/压延阶段，将片材卷曲成卷或以片材形式收集；在第二阶段，对半成品本身进行调整和成型。
在泡沫塑料连续制备方法中，从挤压机生产的片状半成品，保持在不低于40℃的温度下，优选不低于80℃，片材的水分含量为6-30重量％，优选10-25重量％，更优选15-20重量％。片材的温度应不超过150℃，优选100℃。
特别是，如果有合成成分存在，成型温度应接近玻璃转化温度或热塑性聚合物的熔点。
也可以采用间歇方法制造半成品，使其经过初步调整过程，优选将含水量和温度范围调整到连续方法以上。
调整阶段可以立即进行，或与成型工段同时进行。
即使是复合形式的产品，具有特定的、甚至是优美的特征，例如在环境温度下采用成型方法，可以获得在图1中所示的蛤壳形状，在任何情况下，在对接的阳模和阴模之间的温度，都不得高于100℃，以限定最高压力水平和最终产品的最小厚度。
在图2中以实施例的方式示出，使用根据本发明的泡沫塑料片材成型图1蛤壳的模具。阳模(10)和阴模(11)可以这样设计，使它们刚好接近蛤壳侧面的壁而不发生接触。在成形过程中，在无剪切的情况下，在阳模和阴模之间的这些空间，容许泡沫片材滑动。
本发明研制材料的成型方法以及半成品的特性，一般使成型周期小于20秒，优选小于10秒，更优选小于7秒。就成型方法而言，为了使半成品具有优良的可成型性，与含水量和温度有关的参数是极其重要的。在挤压机喷嘴的出口，半成品发生水蒸汽损失，为了避免崩塌现象和过度干燥现象，实际上必须严格控制水的损失程度。
可以在环境温度下，采用模具或模子将制成膨胀的但未打开的管状片材成型。在限制片材干燥问题的情况下，这个系统每次塑模能同时模塑二层片材。如果管状片材能方便地发生相互偏离，获得的产品表面，就能具有类似织物表面织纹的外观。
通常使用开管状态下进行成形，在这种情况下，利用使用蒸汽的调整工段调节水分的含量。片材的特征
构成半成品的材料或形成本发明的泡沫塑料片材，在30℃下在DMSO中测定的特性粘度为1.5-0.3dl/g，优选1.2-0.4dl/g，更优选1-0.6dl/g。
根据本发明，在膨胀的半成品中，蜂窝的尺寸可为25-700μm，优选40-600μm(根据显微镜检查确定)。
膨胀的半成品具有闭合的蜂窝结构，其中蜂窝基本上是互相不连通的，这种结构与开口的蜂窝结构不同，在开口的结构中，蜂窝基本上是互相连通的。
半成品的密度可以为20-150kg/m3，优选25-100kg/m3，更优选30-70kg/m3。
片材的泡沫结构特征在于蜂窝的分布，在未拉伸的情况下，其中80％的蜂窝尺寸为20-400μm，优选25-300μm，更优选30-200μm。
然而，当对片材施加拉伸时，这些蜂窝可随着壁的变薄进行取向。
在本发明的范围内，也有弹性最佳的片材，其特征密度为30-70kg/m3，平均蜂窝尺寸为80-120μm。
采用本发明研制的材料成型的产品主要用在食品包装领域，特别是用作肉、乳制品、蔬菜、鸡蛋、和水果的食品盘，使用期限约30天；玻璃、塑料、或尺寸非常小的金属的包装容器，快餐食品的容器如汉堡包、土豆条、和类似食品的容器；食品用的多隔室容器，也称作午餐盒，快餐食品的咖啡和其它热饮料或冷饮料的杯子。
本发明的成型产品，还用作重量小的物体的容器如便携式电话和小家用电器的多隔室盘，特别是具有能避免使用压制纸等容器所遇到的摩擦现象等的机械性质。
在预料会有高温和低温液体的食品应用中，可将这些容器与另一层泡沫塑料或聚酯膜和/或乙酸纤维素和/或淀粉或其它在使用温度下耐液体的聚合物共挤压或偶合起来。特别是可以使用芳香族-脂肪族聚酯类型的膜，特别是聚亚烷基对苯二甲酸酯己二酸酯、亚烷基丁酸酯、聚亚烷基琥珀酸酯、聚亚烷基癸二酸酯、聚亚烷基壬二酸酯、聚亚环烷基二羧酸酯、特别是聚己基二甲基二羧酸酯、聚环己基二羧酸酯。如果和在包装肉的情况下一样，需要吸收液体，则可以考虑使用高吸收材料，这种材料可直接插入片材中，施加到表面上，或在粘结起来的二个外壳之间的中间层形式，或放在膜下，使盘不透水。
也可以考虑将本发明研制的材料制成微波炉使用的产品，其特征在于，这些产品可用防水性涂料处理，以避免在烹调阶段中干燥容器。成型产品的特征
根据本发明成型的产品，具有闭合的蜂窝结构，其密度较低，为40-400kg/m3，优选45-200kg/m3，更优选50-150kg/m3。
根据本发明成型的产品，还具有优良的挠性，特别是在折合区域，这是由于蜂窝的结构细小而均匀。这些产品还具有非常均匀的优良表面。
在成型阶段获得的产品中，通过形成纸板折合节点所用类型的肋，可以产生折合节点，例如在图2中编号为12的折合节点，在35％RH和23℃下，折合能耐陆续进行至少10个(优选＞20)打开180°/闭合循环，而不发生破裂，每个打开180°/闭合操作，花费约2-4秒，在40％RH和23℃下，优选进行至少100个陆续打开-闭合循环而不破裂，每个打开-闭合循环花费约2-4秒。
也可以采用适合将温度和相对湿度调节到上述值的气候室，使用测力计检测优良的挠性性能。对在长度方向中间具有折合节点的25×10cm试样，进行从0-180°的打开/闭合循环，测力计的指针(bar)在速度3000-10,000mm/min的范围内移动。
实施例
采用下列实施例进一步说明本发明，所提供的实施例，对本发明是说明性的和非限制性的。实施例1
制备具有下列成分的混合物：
-88.9％改变结构的土豆淀粉，在30℃下在DMSO中测定的特性粘度为1.1dl/g，含水量为14％
-8.9重量％的聚乙烯醇
-1.8重量％的滑石
-0.35重量％的甘油
-0.36重量％的1oxial G10
-2重量％的水
将这种组合物加入缓慢的双螺杆挤压机中，共旋转螺杆的直径(d)＝113.8mm，L/D比例＝19∶1。在挤压机的末端，安装用于管状片材的挤出头，其直径为100mm，凸缘开口为0.5mm。在挤压机中熔融体的保压时间为约20分钟。
进料混合物中除了包含的水以外，还在进料压力等于37bar的情况下，在熔融体中还加入1重量％的另一种膨胀剂CO2。CO2是在螺杆的第11个直径处加入的。
操作条件如下：
-RPM：16
-温度分布(℃)：
95/120/120/150/180/180/185/190/197
-进料速率：54kg/h
-凸缘的剪切速率：912s-1
所制的泡沫塑料片材的密度为56kg/m3，蜂窝尺寸为40-170μm，蜂窝尺寸的平均值为81μm。
构成片材的材料在30℃下在DMSO中测定的特性粘度为0.86dl/g。将片材卷曲成卷。实施例2
制备具有下列成分的混合物：
-小麦淀粉 34.4％(12％的H2O)
-土豆淀粉 34.4％(16％的H2O)
-聚乙烯醇 13.5％
-H2O 17.4％
-单油酸甘油酯 0.3％
将这种混合物加入双螺杆APV 2080挤压机中，挤压机直径(d)＝80mm，L/D比例＝40。挤压机在下列条件下操作：
-RPM：285
-温度分布(℃)：
50/75/75/180/180/170/170/175/175/165/165/155/155/145
/120
调节脱气，以这种方式维持颗粒中总含水量为约14.5％。颗粒的特性粘度为1.98dl/g。
将如此获得的颗粒与2.5％的平均颗粒直径约1.5μm的滑石混合，将其加入缓慢的双螺杆挤压机中，挤压机的直径(d)＝113.8mm，L/D比例＝19∶1，管状片材挤出头的直径100mm，凸缘的间距为0.4mm，挤压机在下列条件下操作：
-RPM：14
-温度分布(℃)：
90/120/120/140/165/165/170/186/186
-进料速率：50kg/h
-剪切速率：1360s-1
在进料压力等于40bar下，向熔融体中加入另一种膨胀剂CO2，其量等于1.5重量％。
所获得的管状片材的厚度等于约3mm，密度为70kg/m3，平均蜂窝尺寸等于90μm(最小/最大的蜂窝尺寸＝10/290μm)。片材的含水量等于约1.8重量％，构成片材的材料的特性粘度是m＝1.1dl/g。实施例3
将实施例2获得的管状片材打开，使其经过压延和蒸汽调整过程，直到片材的含水量等于15％为止。采用图2所示适宜的阳-阴型模具进行成型，生产适合快餐食品能折合的蛤壳型盘。
成型是在环境温度下，采用模子对温度维持在约80℃下的片材施加6kg/cm2的压力进行的。模塑循环约6秒，如此制备的产品，厚度等于约1.6mm，底壁的密度为165kg/m3。
特别是，所制的产品是由二个不对称的壳瓣(Valve)构成的，它们的长度为12.5cm，由10cm宽的折合节点连接。这个折合区域具有特殊的机械强度性能。在35％RH和23℃下，在陆续20次每次折曲3秒(相应于约5000mm/min)的打开/闭合循环之后，仍能继续发挥其功能。
所制的产品还具有由特别施加的扁肋构成的非常光滑的表面，这使产品具有令人愉快的优美外观。实施例4
根据实施例1制备的成卷片材，含水量保持在14％。向该片材上施加14μm厚的聚亚丁基对苯二甲酸酯-己二酸酯薄膜，该膜包含33mol％的对苯二甲酸酯，在THF中的特性粘度为1.1dl/g。将施加薄膜的片材加热到80℃，采用实施例3所述的模具成型。所制的容器对80℃的水能耐1小时，在温度从80℃降到20℃所需的时间内，泡沫淀粉容器不会发生崩塌或浸透。实施例5
与实施例4相同，唯一的差别是施加了聚亚乙基癸二酸酯薄膜。该盘非常耐水，淀粉产品不会发生浸透和/或崩塌。实施例6
与实施例4相同，所不同的是，应用30g/m2的粘胶无纺织物代替聚酯膜。实施例7
与实施例4相同，所不同的是，采用密度为80kg/m3，厚度为300μm的聚亚乙基癸二酸酯泡沫塑料片材代替聚酯膜。实施例8
与实施例4相同，所不同的是，对两侧施加薄膜。利用所制的盘进行牛肉包装实验。与机械性能和保存肉有关的实验结果可与采用膨胀的聚苯乙烯制造的盘所观测的结果相比。实施例9
根据实施例1的方法制备的管状片材，在实施例3的条件下，采用盘深2.5cm，15×12cm形式的阳/阴模具直接成形，制成厚度约3mm的双容器。双容器位于实施例4所述类型的二个10μm薄膜之间，将这二个膜粘结起来，形成一个袋，该盘就装在袋内。该膜能热收缩，形成压紧的不透气的用于装肉产品。实施例10
制备具有下列组成的混合物：
-74.3重量％的土豆淀粉(H2O16％)
-0.0重量％的Ecoflex EBX 7000(BASF)
-0.3重量％的Loxiol G 10 F
-15.4重量％的水。
将组合物加入双螺杆挤压机APV 2030中，螺杆直径(d)＝30.0mm，L/D＝40。操作条件如下：
-RPM：170
-温度分布(℃)：
30/100/100/150/160/150/140/130/110×8
调节脱气步骤，使颗粒的含水量为约13.5-14.5％。
然后将颗粒与2.5％的滑石混合，滑石的平均颗粒直径为1.5μm，然后加入缓慢的双螺杆挤压机中，共旋转螺杆的直径(d)＝113.8mm，L/D比例＝19∶1。在挤压机的末端，安装一个用于管状片材的挤出头，直径为100mm，凸缘的开口为0.1mm。操作条件如下：
-RPM：14
-温度分布(℃)：
90/120/140/180/210/210/210/195/196
-进料速率：75kg/h
-剪切速率：31531s-1
还在进料压力等于40bar下，向熔融体中加入按加入的组合物计为0.8重量％的另一种膨胀剂CO2。所制的泡沫塑料片材的厚度为约5mm，密度为81kg/m3(压延的)，蜂窝尺寸的平均值为86μm(蜂窝尺寸为35-188μm)。
Claims (45)
1.一种半成品，特别是泡沫塑料片材形式的半成品，其中包括改变结构或复合的泡沫淀粉连续相，其密度为20-150kg/m3，蜂窝尺寸为25-700μm，蜂窝的分布为在未拉伸的情况下，80％蜂窝的尺寸是20-400μm。
2.根据权利要求1的半成品，特别是泡沫塑料片材形式的半成品，其密度为25-100kg/m3，蜂窝尺寸为40-600μm，蜂窝的分布为在未拉伸的情况下，80％蜂窝的尺寸是25-300μm。
3.根据权利要求2的半成品，特别是泡沫塑料片材形式的半成品，其密度为30-70kg/m3，蜂窝的分布为在未拉伸的情况下，80％的蜂窝尺寸是30-200μm。
4.根据权利要求3的半成品，特别是泡沫塑料片材形式的半成品，其密度为30-70kg/m3，平均蜂窝尺寸是80-120μm。
5.根据权利要求1-4任一项的半成品，其中淀粉是天然的或改性的淀粉，或它们的混合物。
6.根据权利要求5的半成品，其中天然或改性的淀粉，是从土豆、小麦、玉米和木薯淀粉衍生的。
7.根据权利要求5的半成品，其中改性的淀粉，是物理或化学改性的，特别是乙氧基化的淀粉、乙酸酯淀粉、丁酸酯淀粉、丙酸酯淀粉、羟丙基化的淀粉、阳离子淀粉、氧化的淀粉、交联的淀粉、凝胶化的淀粉、与能产生“V”型复合物的分子和/或聚合物复合的淀粉、糊精化的淀粉、和与聚酯、聚氨酯、聚酯型氨基甲酸酯、聚脲、聚酯脲、聚硅氧烷、硅烷、钛酸酯、和脂肪链等接枝的淀粉。
8.根据权利要求1-7任一项的半成品，能在成型阶段制成具有折合节点的产品，在35％RH和23℃下，该折合节点能耐至少10个陆续打开/闭合循环而不破裂，每个打开-闭合操作花费2-4秒。
9.根据权利要求1-8任一项的半成品，其中制造泡沫塑料片材的材料在30℃下在DMSO中的特性粘度为1.5-0.3dl/g。
10.根据权利要求9的半成品，其中在30℃下在DMSO中的特性粘度为1.2-0.4dl/g。
11.根据权利要求10的半成品，其中在30℃下在DMSO中的特性粘度为1.1-0.6dl/g。
12.根据权利要求1-11任一项的半成品，其中包含一种或多种热塑性的聚合物，其熔点为60-175℃。
13.根据权利要求12的半成品，其中热塑性的聚合物是改性或未改性的天然来源的聚合物，特别是从纤维素衍生的如取代程度为1-2.5的乙酸纤维素、丙酸纤维素、丁酸纤维素、和它们的共聚物；烷基纤维素、羟烷基纤维素、和羧烷基纤维素类型的聚合物，特别是羧甲基纤维素、硝基纤维素和脱乙酰壳多糖支链淀粉、或酪蛋白和酪蛋白酸酯、玉米蛋白、大豆蛋白质、藻酸和藻酸酯、天然橡胶、和聚天冬氨酸酯；谷蛋白，糊精。
14.根据权利要求12的半成品，其中热塑性聚合物是合成或发酵来源的可生物降解的聚合物，特别是包括C2-C24脂肪族羟基酸的聚合物或共聚物，或它们相应的内酯或交酯类型的聚酯，特别是具有各种D/L乳酸比例的乳酸聚合物，聚乳酸与脂肪族和脂肪族-芳香族聚酯的共聚物，聚己内酯，聚戊内酯，它们的共聚物，以及从二官能酸和脂肪族二元醇衍生的聚酯，脂肪族-芳香族聚酯，特别是包含用或没用链增长剂处理的亚烷基-对苯二甲酸酯己二酸酯类型的共聚物，优选对苯二甲酸含量小于40mol％的一般环氧树脂、特别优选双酚树脂。
15.根据权利要求12的半成品，其中热塑性聚合物是包含加在疏水链区中的亲水性基团的聚合物，例如乙烯-乙烯醇共聚物，乙烯-乙酸乙烯酯共聚物，丙烯酸酯，乙烯-丙烯酸酯共聚物，乙烯与不饱和酸，例如丙烯酸、甲基丙烯酸、巴豆酸、和衣康酸等的共聚物，具有亲水单元的共聚物，其中具有脂肪族聚酯和/或芳香族-脂肪族聚酯中官能醇基团和羧酸基团，环氧树脂，其中包括包含双酚的树脂。
16.根据权利要求12的半成品，其中热塑性聚合物是能与淀粉生成氢键的聚合物，特别是可以采用丙烯酸酯或甲基丙烯酸酯改性的，具有不同水解程度的聚乙烯醇，为了降低其熔点而初步增塑或改性的聚乙烯醇。
17.根据权利要求12的半成品，其中包含下列聚合物如聚乙烯醇，烯烃聚合物的共聚物，优选乙烯与选自乙烯醇、乙酸乙烯酯、丙烯酸和甲基丙烯酸单体的共聚物，脂肪族聚酯如己内酯，聚亚烷基琥珀酸酯，壬二酸、癸二酸、巴西基酸的聚合物，和它们的共聚物，脂肪族聚酰胺，聚亚烷基癸二酸酯，聚亚烷基壬二酸酯，聚亚烷基巴西基酸酯，特别是乙烯与包括C2-C13的二元醇、包含二聚酸的聚酯、聚亚烷基对苯二甲酸酯己二酸酯类型的芳香族-脂肪族聚酯和环氧树脂、特别是含双酚基团的环氧树脂形成的共聚物。
18.根据权利要求1-17任一项的半成品，其中包含成核剂，就原料组合物而言，其含量为0.05-10重量％、优选0.5-7重量％，更优选1-5重量％。
19.根据权利要求18的半成品，其中成核剂是由无机成分如滑石(硅酸镁)、碳酸钙、钠和钡的硫酸盐、和二氧化钛构成的，其表面可用硅烷、钛酸酯等粘合促进剂处理。
20.根据权利要求1-19任一项的半成品，其中包含有机的填料和纤维如木材粉末、纤维素、葡萄残余物的粉末、糠、玉米皮、或其它天然纤维，其含量为0.5-20％。
21.根据权利要求1-20任一项的半成品，其中包含成核剂、润滑剂和/或分散剂、和增塑剂。
22.根据权利要求1-21任一项的半成品，其中包括食用油如棕榈油、玉米油、豆油、葵花油、C12-C22脂肪酸、和其不同取代程度的甘油酯，特别是氢化的动物或合成来源的脂肪，它们至少在环境温度下，优选在环境温度以上是固体，以改善耐湿性能和降低水的可湿润性。
23.根据权利要求1-22任一项的半成品，其中包含乳酸、酒石酸、和柠檬酸等弱酸，以在挤压过程中调节淀粉的粘度。
24.从根据权利要求1-23的半成品获得的产品和半成品，是通过与无纺织物、纺织物、纸、可生物降解的和不能生物降解的薄膜或铝层层压制备的。
25.根据权利要求24的产品和半成品，是通过与无纺织物或天然纤维的纺织物层压生产的，天然纤维是如黄麻、棉花、和羊毛的纤维，基于多糖的纤维如乙酸纤维素、淀粉乙酸酯、和粘胶丝等，或从可生物降解的聚合物开始生产的纤维，特别是脂肪族聚酯如聚乳酸、聚己内酯、二元醇与二元酸的聚亚烷基羧酸酯，二元酸选自直链C2-C13二元酸，和/或脂环族、脂肪族-芳香族聚酯，特别是己二酸酯化的聚亚烷基对苯二甲酸酯家族的脂肪族-芳香族聚酯和它们的共聚物，聚酰胺，特别是基于己内酯、脂肪胺等的聚酰胺，脂肪族聚氨酯，聚酯型氨基甲酸酯，聚脲，和环氧树脂。
26.根据权利要求24的产品和半成品，与一些由可生物降解的聚合物，特别是脂肪族聚酯如聚乳酸、聚己内酯、和/或二元醇和二元酸的脂环族聚亚烷基羧酸酯，二元酸选自直链C2-C13二元酸，脂肪族-芳香族聚酯，特别是己二酸酯化的聚亚烷基对苯二甲酸酯家族的脂肪族-芳香族聚酯和它们的共聚物，聚酰胺，特别是基于己内酯、脂肪胺等的聚酰胺，脂肪族聚氨酯，聚酯型氨基甲酸酯，聚脲，和环氧树脂构成的膜偶合，这些膜是通过挤出吹胀、共挤出、和/或浇注制备的。
27.采用涂覆的方法从权利要求1-23的半成品获得的产品和半成品，它们采用可生物降解的聚合物，特别是脂肪族聚酯如聚乳酸，聚己内酯，二元醇和二元酸的聚亚烷基羧酸酯，二元酸选自直链和/或脂环族C2-C13二元酸，脂肪族-芳香族聚酯，特别是己二酸酯化的聚亚烷基对苯二甲酸酯家族的脂肪族-芳香族聚酯和它们的共聚物，聚酰胺，特别是基于己内酯、脂肪胺类等的聚酰胺，脂肪族聚氨酯，聚酯型氨基甲酸酯、聚脲、和环氧树脂的乳化物、分散体、溶液、和热熔体涂覆。
28.根据权利要求26的产品和半成品，其中利用温度和/或施加适宜的可生物降解的粘合剂将膜偶合到半成品上，这些粘合剂是基于乳酸聚合物、聚氨酯、聚乳酸乙烯酯和聚乙烯醇、酪蛋白和谷蛋白等蛋白质、淀粉、糊精、和其它多糖。
29.根据权利要求26和28的产品和半成品，其中的膜是由浇注和发泡成膜法制备的，可以与泡沫塑料载体的附着面共挤出。
30.根据权利要求29的产品和半成品，其中膜的熔点高于60℃，优选高于80℃，更优选高于100℃。
31.一种根据权利要求26或28的片材，能制成非层压的片材。
32.由权利要求1-23的材料获得的产品和半成品，根据它们的不同应用，采用熔点高达120℃的天然和合成的蜡处理。
33.一种采用挤压机生产泡沫塑料片材的方法，其中包括下列步骤：
-在占组合物总重量6-30％比例的水存在下，将特性粘度为2-0.6dl/g的淀粉加入挤压机中，其加入量能使淀粉成分构成材料的连续相，还可以加入天然或合成的热塑性聚合物和其它添加剂，例如增塑剂、润滑剂、成核剂、表面活性剂、弱酸、和填料；
-使淀粉物质完全熔融；
-将CO2加入到温度为100-180℃，优选120-160℃的熔融体中，加入量为0.4-10重量％，优选0.8-7重量％，更优选1.0-4重量％；和
-将熔融体加工5-40分钟，使膨胀剂、水、和CO2的混合物分布均匀，可以采用柠檬酸和酸式碳酸盐等化学膨胀剂，将组合物的粘度调节到1.5-0.3dl/g。
34.根据权利要求33的方法，其中熔融体的挤压是通过扁平或管状的挤出头进行的，挤出头能对熔融体施加500-50,000s-1的剪切速率，优选800-40,000s-1，更优选900-35,000s-1。
35.根据权利要求34的方法，其中用空气或蒸汽将挤出的管状片材吹胀，在双轴向拉伸，提供光滑的表面，把片材保存在所需的湿度下，将管状片材打开，压延，进一步的调整，卷曲成卷。
36.根据权利要求34的方法，其中用空气和蒸汽将管状片材吹胀，使片材本身膨胀，将片材保存在所需的湿度下，打开管状片材压延，切制成平整的片材。
37.根据权利要求34的方法，其中检验，调整，然后收集所生产的管状半成品。
38.根据权利要求1-32任一项成型半成品的方法，其中包括：
-在温度40-120℃，优选在40-100℃，将产品或半成品的含水量调整到6％-30％，优选10％-25％，更优选15％-20％，
-在环境温度至80℃下，采用阳-阴型冲压模成型，
-可以形成波纹，提供密度为40-400kg/m3，优选45-200kg/m3，更优选50-150kg/m3的成型产品，产品可具有耐反复闭合/打开循环的折合节点。
39.根据权利要求1-32任一项的半成品的组合，制成多层结构的各种几何形状不同的产品，例如卷筒，块，具有显著弹性的塑料片，弯头零件，在家用电器领域使用的保护容器，或电子产品、食品领域、药物、装置和家具、邮购或快件信封的保护容器。
40.根据权利要求1-32的材料与其它载体的组合，以提供与木材、纸、特等纸板、无纺织物、天然或合成纤维的织物、在包装领域使用的铝或其它金属混合的多层材料。
41.根据权利要求38的成型产品，主要在食品包装领域使用，特别是用作使用期约30天的食品盘，用于封装肉、乳制品、蔬菜、鸡蛋、和水果；小尺寸的玻璃、塑料、或金属包装的陈列容器，快餐食品的容器，例如汉堡包、土豆条和类似食品的容器；快餐食品和膳食的多隔室容器。
42.根据权利要求38的成型产品，用于热的和冷的液体，作为咖啡和饮料的杯子，用作亚洲国家所用类型的盛汤容器，用于快餐食品和膳食中液体含量高的其它食品的容器。
43.根据权利要求38成型的产品，用作重量小的物体的容器，例如便携式电话和小家用电器的多隔室盘，特别是它具有能避免加压纸等容器所遇到的摩擦现象的机械性质。
44.根据权利要求38的产品，在超级市场中以盘的形式包裹肉类，以使用吸收剂或高吸收材料，为消除存在的血提供了条件，将这些材料直接加到片材中，施加到表面上，或制成粘合在一起的二个外壳的中间层，或放在膜内，使盘不透水。
45.根据权利要求38的成型产品，以经表面处理的容器用于炉和微波炉，可避免因去除水的影响使容器太不结实。
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-
2000
- 2000-02-15 IT IT2000TO000141A patent/IT1320163B1/it active
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2001
- 2001-02-14 JP JP2001560276A patent/JP2003523432A/ja not_active Withdrawn
- 2001-02-14 AT AT01103390T patent/ATE423159T1/de not_active IP Right Cessation
- 2001-02-14 KR KR1020027010615A patent/KR100827255B1/ko not_active IP Right Cessation
- 2001-02-14 ES ES01103390T patent/ES2322544T3/es not_active Expired - Lifetime
- 2001-02-14 EP EP01103390A patent/EP1127914B1/en not_active Expired - Lifetime
- 2001-02-14 CA CA002399964A patent/CA2399964A1/en not_active Abandoned
- 2001-02-14 WO PCT/EP2001/001601 patent/WO2001060898A1/en active IP Right Grant
- 2001-02-14 AU AU3174201A patent/AU3174201A/xx active Pending
- 2001-02-14 AU AU2001231742A patent/AU2001231742B8/en not_active Ceased
- 2001-02-14 IL IL15121201A patent/IL151212A0/xx active IP Right Grant
- 2001-02-14 DE DE60137659T patent/DE60137659D1/de not_active Expired - Lifetime
- 2001-02-14 CN CNB01807894XA patent/CN1273522C/zh not_active Expired - Fee Related
- 2001-02-14 BR BRPI0108382-1A patent/BR0108382B1/pt not_active IP Right Cessation
- 2001-02-15 US US09/784,707 patent/US20010014388A1/en not_active Abandoned
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- 2002-08-12 IL IL151212A patent/IL151212A/en not_active IP Right Cessation
- 2002-08-13 ZA ZA200206462A patent/ZA200206462B/en unknown
- 2002-08-14 NO NO20023839A patent/NO20023839L/no not_active Application Discontinuation
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- 2009-06-16 US US12/485,495 patent/US20090324913A1/en not_active Abandoned
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861352B (zh) * | 2006-06-12 | 2011-01-19 | 南星家居科技(湖州)有限公司 | 用蒸压法制造轻质菱苦土木丝板的方法 |
| CN101613485B (zh) * | 2009-06-23 | 2011-07-27 | 扬州大学 | 一种基于生物相容高分子的超多孔材料的制备方法 |
| CN102892826A (zh) * | 2010-05-14 | 2013-01-23 | 诺瓦蒙特股份公司 | 通过辐照发泡的可生物降解粒料 |
| CN102892826B (zh) * | 2010-05-14 | 2014-12-24 | 诺瓦蒙特股份公司 | 通过辐照发泡的可生物降解粒料 |
| CN108675823A (zh) * | 2018-04-20 | 2018-10-19 | 安徽中都环宇新材料科技有限公司 | 一种柴油机碳烟颗粒净化dpf用蜂窝陶瓷载体 |
| CN117510998A (zh) * | 2023-11-14 | 2024-02-06 | 中山市泰源新材料科技有限公司 | 一种可降解环保发泡材料及其制备方法 |
| CN117510998B (zh) * | 2023-11-14 | 2024-04-09 | 中山市泰源新材料科技有限公司 | 一种可降解环保发泡材料及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1127914A2 (en) | 2001-08-29 |
| ATE423159T1 (de) | 2009-03-15 |
| AU2001231742B2 (en) | 2005-01-20 |
| CA2399964A1 (en) | 2001-08-23 |
| EP1127914B1 (en) | 2009-02-18 |
| US20090324913A1 (en) | 2009-12-31 |
| DE60137659D1 (de) | 2009-04-02 |
| US20010014388A1 (en) | 2001-08-16 |
| WO2001060898A1 (en) | 2001-08-23 |
| AU3174201A (en) | 2001-08-27 |
| ITTO20000141A1 (it) | 2001-08-15 |
| KR20020086537A (ko) | 2002-11-18 |
| BR0108382B1 (pt) | 2011-01-25 |
| ZA200206462B (en) | 2003-08-13 |
| EP1127914A3 (en) | 2001-09-26 |
| IL151212A0 (en) | 2003-04-10 |
| BR0108382A (pt) | 2002-10-29 |
| CN1273522C (zh) | 2006-09-06 |
| NO20023839D0 (no) | 2002-08-14 |
| WO2001060898B1 (en) | 2001-12-06 |
| IL151212A (en) | 2007-06-03 |
| IT1320163B1 (it) | 2003-11-18 |
| JP2003523432A (ja) | 2003-08-05 |
| KR100827255B1 (ko) | 2008-05-07 |
| ES2322544T3 (es) | 2009-06-23 |
| AU2001231742B8 (en) | 2005-02-24 |
| NO20023839L (no) | 2002-09-27 |
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