CN116529173A - 用于改善阻隔性能的水性分散体 - Google Patents
用于改善阻隔性能的水性分散体 Download PDFInfo
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- CN116529173A CN116529173A CN202180082069.1A CN202180082069A CN116529173A CN 116529173 A CN116529173 A CN 116529173A CN 202180082069 A CN202180082069 A CN 202180082069A CN 116529173 A CN116529173 A CN 116529173A
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Abstract
本发明涉及用具有7.5‑9.4的pH值的水性聚烯烃分散体处理的纤维制品,所述水性聚烯烃分散体包含:a.50‑100重量%的含有以下成分的水性分散体A:i.41‑98重量%的A1,其是具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的乙烯/(甲基)丙烯酸共聚物,或是各自具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的不同的乙烯/(甲基)丙烯酸共聚物的混合物,ii.1‑59重量%的A2,其是其它含烯属结构单元的烃聚合物,或其它含烯属结构单元的烃聚合物的混合物,和iii.0‑35重量%的不同于A1和A2的添加剂;b.0‑50重量%的化合物B,其中化合物B是可分散或可溶于水的材料并且与分散体A的任何成分不同,其中‑A和B的重量%是基于整个水性聚烯烃分散体的固含量计,‑分散体A的成分的重量%是基于分散体A的固含量计,‑分散体A的成分i至iii的重量%之和是100%。
Description
本发明涉及纤维制品、基于所述纤维制品的产品以及水性分散体的用途。
通过聚烯烃在水中的机械分散,可以制成所谓的二次水性聚烯烃分散体(secondary aqueous polyolefin dispersions)。这些分散体在施加到各种基底上时提供聚烯烃的特殊特性,包括防水性/耐化学品性。通过机械分散技术,可获得聚合物的水性分散体。一般而言,在载液中的二次聚合物分散体可以通过在聚合物熔融温度以上的温度下在载液中高剪切混合该聚合物来制备。根据US 2014/0255683,通过熔融捏合法可以获得适合作为涂料组合物的水性聚烯烃分散体,在所述熔融捏合法中加工特殊的热塑性和酸性聚烯烃。
耐油性、防水性和防水蒸气性属于阻隔性能,被视为涂布纸和涂布纸板(两者通常都基本含有植物纤维)的典型关键性质,其可通过正确选择涂层而改进。聚烯烃广泛用于纸张涂布,但通常作为热塑性熔体使用挤出涂布技术施加。水基聚烯烃分散体的可得性提供了经济上有吸引力的替代方案。可以使用水基涂料的常规方法将聚烯烃分散体施加到纸上,包括各种喷涂技术。此外,可以将分散体印刷到纸幅上,例如通过凹版印刷、辊涂等。
US 7,528,080提出使用特殊的水性聚烯烃分散体处理纤维,从而获得具有有吸引力的浸渍性质的相应处理过的纺织产品。
但是,上述技术没有提供适合用于纸应用的具有满意阻隔性能的聚烯烃分散体。所以,本发明要解决的问题是提供适合用于纸和纸板(carton)处理的水性聚烯烃分散体。所述用水性聚烯烃分散体的处理应当允许制造高品质的纸/纸板产品,其具有与耐油性、防水性和/或防水蒸气性相关的有益特性。
此问题的解决方案是用具有7.5-9.4的pH值的水性聚烯烃分散体处理的纤维制品(fiber preparation),所述水性聚烯烃分散体包含:
a.50-100重量%的含有以下成分的水性分散体A:
i.41-98重量%的A1,其是具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团((meth)acrylic based groups)含量的乙烯/(甲基)丙烯酸共聚物,或是各自具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的不同的乙烯/(甲基)丙烯酸共聚物的混合物,
ii.1-59重量%的A2,其是其它含烯属结构单元的烃聚合物,或其它含烯属结构单元的烃聚合物的混合物,和
iii.0-35重量%的不同于A1和A2的添加剂,
b.0-50重量%的化合物B,其中化合物B是可分散或可溶于水的材料并且与分散体A的任何成分不同,
其中
-A和B的重量%是基于整个水性聚烯烃分散体的固含量计,
-分散体A的成分的重量%是基于分散体A的固含量计,
-分散体A的成分i至iii的重量%之和是100%。
作为定义,烃共聚物仅仅含有碳和氢元素。术语“烯属结构单元”是指通过相应烯烃的聚合反应产生的(聚合物的)结构单元。含烯属结构单元的烃聚合物(及其相应混合物)可以由相应的均聚物和/或共聚物提供。
用水性聚烯烃分散体处理的纤维制品提供优异的阻隔性能,特别是耐油性、防水性和防水蒸气性。所用的分散体具有高稳定性和优良品质。
水性聚合物分散体A
根据本发明使用的水性聚烯烃分散体包含具有以下成分的水性聚合物分散体A:
i.41-98重量%的A1,其是具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的乙烯/(甲基)丙烯酸共聚物,或是各自具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的不同的乙烯/(甲基)丙烯酸共聚物的混合物,
ii.1-59重量%的A2,其是其它含烯属结构单元的烃聚合物,或其它含烯属结构单元的烃聚合物的混合物,和
iii.0-35重量%的不同于A1和A2的添加剂,
其中分散体A的成分的重量%是基于分散体A的固含量计,并且分散体A的成分i至iii的重量%之和是100%。
根据本发明的一个有益实施方案,根据本发明使用的水性聚烯烃分散体包含具有以下成分的水性分散体A:
i.51-95重量%的A1,其是具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的乙烯/(甲基)丙烯酸共聚物,或是各自具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的不同的乙烯/(甲基)丙烯酸共聚物的混合物,
ii.5-49重量%的A2,其是其它含烯属结构单元的烃聚合物,或其它含烯属结构单元的烃聚合物的混合物,和
iii.0-35重量%的不同于A1和A2的添加剂,
其中分散体A的成分的重量%是基于分散体A的固含量计,并且分散体A的成分i至iii的重量%之和是100%。
所述乙烯/(甲基)丙烯酸共聚物A1优选由具有与熔体加工性相关的足够性能的乙烯/(甲基)丙烯酸共聚物提供,例如具有在2.16kg载荷下在190℃下测得的2至3000g/10min的熔体流动指数(MFI)的共聚物。根据一个具体的实施方案,至少60重量%的A1具有基于共聚物的总重量计至少19重量%的(甲基)丙烯酸系基团含量。
所用的水性分散体具有高的分散稳定性(也可以由于较高量的A1),这对于相关的纸/纸板应用而言是有益的。
可用于本发明分散体中的合适的市售聚乙烯/(甲基)丙烯酸共聚物的实例包括PrimacorTM5980(来自SK-Chemicals),NucrelTM925,NucrelTM960(来自Dow)和EscorTM5200(来自Exxonmobil)。
存在于聚合物分散体A中的其它含烯属结构单元的共聚物A2可以根据所用水性分散体的具体(纸)应用来选择。相关的烯属结构单元是基于聚合的烯烃单体,通常选自链烯和/或多烯。
优选,至少60重量%的A2由含有乙烯结构单元(通过乙烯聚合产生的结构单元)的共聚物提供。
根据一个具体实施方案,至少60重量%的A2选自下组:
-具有乙烯和1-辛烯结构单元的聚烯烃,和
-具有乙烯和丙烯结构单元的聚烯烃。
可用于本发明分散体A中的合适的市售其它聚合物A2的实例包括:Dutral CO 034和Dutral CO 038,乙烯丙烯共聚物(28重量%的丙烯),“Versalis”;Vistamaxx 6202弹性体,具有15重量%的乙烯含量,“Exxonmobil”;Engage 8407,基于丙烯的烯属乙烯-辛烯共聚物,“Dow”。
可存在于根据本发明的水性分散体中的添加剂包括分散剂、流变添加剂、附着促进剂、增粘剂、消泡剂、填料、颜料和已知用于聚合物分散体或聚合物组合物的任何其它材料。可用于根据本发明的水性分散体中的典型添加剂的实例包括硬脂酸,油酸和其它长链羧酸,粘土,合成硅酸盐,二氧化硅,蜡例如石蜡和聚烯烃蜡,和磺基琥珀酸二辛酯钠。
化合物B任选地存在于根据本发明的水性分散体中。化合物B是一种可分散或可溶于水的材料,或多种可分散或可溶于水的材料的混合物,并且化合物B不同于分散体A的任何成分。例如,可以加入化合物B以改进包含本发明水性分散体的材料或者通过从这种分散体蒸发溶剂形成的材料或制品的再循环能力。化合物B可以是无机材料或有机材料。例如,化合物B可以是可分散或可溶于水的一种不含烯属结构单元的聚合物(例如聚醚)或多种聚合物的混合物。
因此,在本发明的一个具体实施方案中,存在化合物B,并且其可以包含回收辅助组分(recycling auxiliary component)。回收辅助组分通常由聚乙烯基吡咯烷酮(PVP)(Mw为5000-200000)和/或聚乙二醇(PEG)(Mw为1000 -100000)提供。根据一个实施方案,基于整个水性分散体的固含量计,水性聚烯烃分散体含有(作为B的成分)小于5重量%、优选小于4重量%的PEG。
通常,(整个)水性聚烯烃分散体具有10-60重量%的固含量。
水性聚合物分散体的制备:
制备所施加的水性聚烯烃分散体的方法通常包括步骤a.至c.,其中
a.在第一步骤中在50℃至200℃范围内的温度下密切混合分散体A的所有固体组分,此后获得所有组分的均匀配混物(homogenous compound),
b.在下一步骤中,将所述均匀配混物在比在第一步骤中混合的组分的最高熔融温度高2至20℃的温度下与水、化合物B和用于调节pH值的中和剂混合直到获得水性分散体,和
c.将步骤b.中得到的水性分散体冷却到低于A1的熔融温度或熔程(如果A1组分没有一致的熔融温度)的温度以下。
通常,第一步骤中的混合操作在双螺杆挤出机中进行。通常,所述均匀配混物与水、化合物B(如果包含的话)和中和剂化合物(neutralizing compound)的混合操作在升高的压力下进行。
“预混步骤”a.允许在不使用(附加)乳化剂的情况下制备水性分散体。由于食品安全原因和与可热封性相关的性质,在分散体中避免这些乳化剂是有利的。所述均匀配混物与水、化合物B和中和剂化合物的混合操作可以在比水在混合温度下的蒸气压更高的压力下进行。
为了得到具有有吸引力的阻隔性能的产品,冷却步骤c.是重要的。通常,将水性分散体冷却到50℃以下,优选30℃以下。有利地,水性分散体的冷却非常快速地进行(通常至少10℃/分钟,优选至少50℃/分钟),这另外改进热封性能。
在制备根据本发明的水性聚烯烃分散体的方法中,在比在第一步骤中混合的组分的最高熔融温度高2至20℃的温度下,将在第一步骤中获得的均化配混物与水、化合物B(如果包含的话)和中和剂混合直到获得水性分散体,其中所有分散的粒子通常具有低于60μm的粒度,优选低于20μm。“比在第一步骤中混合的组分的最高熔融温度高2至20℃的温度”是指比为获得均化配混物而混合的任何单一组分的最高熔融温度高2至20℃的温度。例如,如果通过各自具有自身的熔融温度(TMA1、TMA2、TMA3)且其中TMA2>TMA1>TMA3的3种成分A1、A2和A3获得均化配混物,比最高熔融温度高2至20℃是指比TMA2高2至20℃。
在制备根据本发明的水性聚烯烃分散体的方法中所用的中和剂可以是任何碱性水溶液,例如NH3的水溶液。相关的水性聚烯烃分散体应当具有7.5-9.4的pH值。
在根据本发明使用的水性聚烯烃分散体中存在的粒子的粒度通常<60μm。可以使用Microtrac S3500激光衍射系统,使用湿分散模块测量这一粒度。对于各测量,将1毫升的分散体添加到湿分散模块的1升分散单元中,其中该分散模块装有pH在7-10的范围内的水。
根据本发明的水性聚烯烃分散体的液体含量是可变的,并通常依照常规聚烯烃分散体。通常,作为分散液体,完全使用水。
所用的水性分散体含有被批准为间接食品添加剂的成分,即,可能作为包装或加工设备的一部分与食品接触、但无意直接添加到食品中的物质。该成分有时被称为食品安全材料或适合直接食品接触的材料。在这方面,“食品安全”是指这些材料符合欧盟法规“EU10-2011for plastics intended to come into contact with food(用于与食品接触的塑料)”的标准及其修订版本。在本发明的一个实施方案中,存在于水性聚合物分散体中的所有成分都是食品安全材料或适合直接食品接触的材料。
一般而言,根据本发明使用的水性聚烯烃分散体具有下列性质:
-固含量为10-60重量%,
-粘度为10-10000mPa*s,
-储存稳定性≥6个月,
-平均粒度为0.1至50μm。
根据本发明的方法提供(干)组分的一种预混,这在第一步骤中进行:在50℃至200℃的温度下密切混合分散体A的所有固体组分,尤其是组分A1和A2,此后获得所有组分的均匀配混物。通常,在预混步骤中不使用水。在所述预混步骤似乎是生成含有A1和A2的混杂粒子(hybrid particles)的基础。在下一步骤中,在预混步骤中提供的均匀配混物进一步与水,任选地与化合物B和与中和剂混合:结果获得一种水性聚烯烃分散体,其包含分散的含有A1和A2的混杂粒子。
为了提供关于分散体的组成的实验信息,作为分析方法,尤其可以使用差示扫描量热法(DSC)和/或红外光谱法。根据所述DSC方法,一方面对所用原料(聚合物)和另一方面对制成的混合物(分散体的固体内容物)测定熔融温度(熔程)。制成的混合物的熔程通常比所用原料的熔程宽得多。
定义:
在本说明书的内容中,使用下列定义:
-(甲基)丙烯酸是指丙烯酸和/或甲基丙烯酸;
-均匀的含聚合物的配混物是在流延成厚度为1至2mm的膜时没有显示光学缺陷的混合物。
测量方法
使用下列测量方法表征本说明书中提到的各组分和所得产物:
根据ISO 1133在Zwick/Roell挤压式塑性计中测定熔体流动指数(MFI)。在2.16kg载荷下在190℃下测量MFI。对于各测量,在开始测量前将6克材料在测量筒内加热5分钟。MFI是三个部分的平均值。
使用根据ISO 11357的差示扫描量热法测定组分的熔融温度。对于该测量,使用Mettler Toledo DSCStar System。此测量在氮气中在-60至200℃的温度范围内和以10K/min的加热速率进行。
在来自Mettler-Toledo GmbH的Moisture Analyzer HC103中测定分散体的固含量。此测量在130℃下进行30分钟,然后重量恒定。
使用Thermo Fisher Scientific HAAKETM旋转流变仪RV1在20℃下使用与MPC/DC60几何结合的双锥体DC60/2Ti L配置测量分散体的粘度。此测量在0至120s-1的剪切速率下进行120秒。评估在114s-1的剪切速率下的粘度值。
使用Microtrac S3500激光衍射系统,使用湿分散模块测量粒度。对于各测量,将1毫升的分散体添加到1升分散模块中,其中该分散模块装有pH在7-10范围内的水。进一步的设置是小室尺寸(cell size)为2mm、超声持续时间60秒。具体值是x50-值,单位为μm,这对应于平均粒度。
使用PCE Instruments的pH计PCE-228根据DIN ISO 8975测定未稀释的分散体的pH值。
用于不同阻隔试验的样品的制备包括多个步骤:用绕线棒将分散体涂布到基底上,然后在烘箱中在120℃下干燥120秒。
通过重力法测定所涂布的分散体层的涂层重量。为此目的,从未涂布的基底用圆形切割器切下具有限定面积的圆形物,并用分析天平称重。然后,从经涂布的基底切下具有相同面积的圆形物,也称量重量。重量差异进行标准化,并用于表示负载量,单位为克/平方米。
根据ISO 15106-2和ASTM F1249使用来自的C390H水蒸气透过率试验系统检测水蒸气渗透性。此检测在两种不同的条件下进行(23℃和50%rh(相对湿度),以及38℃和90%rh)。基底的经涂布的那侧朝向检测仪器的水蒸气侧。
使用COBB测量仪根据DIN EN ISO 535(“纸和纸板-测量吸水性”)检测吸水/防水性。为此目的,切出样品并用分析天平称量重量。然后,使样品在COBB测量仪中在水中暴露特定的时间段,然后置于两张吸墨纸之间以从样品表面除去过量的水。然后,也称量“湿”样品的重量,此重量差异进行标准化,并用于表示吸水性,单位为克/平方米。时间可以在60秒(COBB 60)和1800秒(COBB 1800)之间变化。
也使用COBB测量仪根据DIN EN ISO 535的试验程序检测耐油/油脂性。切出样品并用分析天平称量重量。然后,使样品在COBB测量仪中在油中暴露特定的时间段,然后置于两张吸墨纸之间以从样品表面除去过量的油。然后,也称量“油性”样品的重量,此重量差异进行标准化。并用于表示吸油性,单位为克/平方米。
根据一个优选实施方案,根据本发明的纤维制品形成固体产品,后者优选由片材提供。通常,至少80重量%的纤维由纤维素纤维提供,从而由纸或纸板制品提供纤维制品。相关的纤维可以选自纤维素和木质纤维素及其组合,其可以从年生植物或多年生植物获得,尤其从木材获得。
也可以使用合成纤维,特别是热塑性合成纤维,例如基于以下聚合物:乙醇酸聚合物,聚烯烃,聚对苯二甲酸乙二酯,聚酯,聚酰胺,聚交酯,聚乙烯醇,或聚琥珀酸丁二酯。另外,可以使用增强纤维,例如选自聚合物纤维、矿物纤维、非木类的天然纤维和玻璃纤维,及其组合。纤维可以是可生物降解的和/或可循环使用的。
相应的由纤维制成的产品可以是运输袋和大袋子,购物袋,垃圾袋,食品包装,工业包装,医用包装,掩护物(coverts),包裹物,和用于替代塑料袋的袋子。
本发明还涉及基于上述纤维制品的产品,其中用水性聚烯烃分散体处理的操作是通过将水性聚烯烃分散体作为粘合剂和/或作为纤维的涂料施加、然后除去水性聚烯烃分散体中的水进行。
通常,通过干燥除去水性聚烯烃分散体中的水,这优选在75℃以上的温度下进行。相关的(干燥)温度应当一般足够高以允许所含的聚合物形成膜。所述成膜可以在阻隔性能方面是重要的。
所述产品通常由纸或纸板提供。用水性聚合物分散体处理相关纸基底的操作可以通过用橡皮辊/绕线棒、柔性辊筒涂布或通过喷涂进行。另外,本发明提供上述水性聚烯烃分散体作为粘合剂和/或作为涂料组合物用于纤维型基底的用途,优选用于纸或纸板。
所述应用优选用于改善与耐油性、防水性和/或防水蒸气性相关的阻隔性能。
特别是,这些阻隔性能对于纸包装材料的品质而言是重要的。
实施例
使用下列程序制备各种水性分散体:
-在第一步骤中通过在Leistritz ZSE 18Maxx双螺杆挤出机中在80-150℃范围内的温度下(根据成分选择温度)混合和捏合各成分来制备混合物,其中在挤出机内创建不同的温度区。挤出机内的压力是最大35巴。
-在下一步骤中,将挤出的混合物供入Büchi 2l压力反应器,该反应器配有以100-1000rpm速度运行的溶解器混合机。在有时升高的压力下(0-100巴的附加压力)在90-150℃范围内的升高温度下制备分散体。在形成均匀分散体后,该混合物的冷却是必要的。冷却必须在聚合物的结晶温度下尽可能快地进行直到40℃的最高温度。
在下表1中列出用于各实施例的成分(重量份,基于固含量计)和条件。
表1
EAA#3:可分散的聚合物,其是乙烯/丙烯酸共聚物(20重量%的丙烯酸),
POE#8:含有乙烯和1-辛烯的聚烯烃弹性体,
POP#11:基于丙烯的弹性体,具有15重量%的乙烯含量,
EPM#82:乙烯/丙烯共聚物(28重量%的丙烯),
Laponite:合成的层状磷酸盐改性硅酸盐,具有330m2/g的比表面积。
Claims (15)
1.用具有7.5-9.4的pH值的水性聚烯烃分散体处理的纤维制品,所述水性聚烯烃分散体包含:
a.50-100重量%的含有以下成分的水性分散体A:
i.41-98重量%的A1,其是具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的乙烯/(甲基)丙烯酸共聚物,或是各自具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的不同的乙烯/(甲基)丙烯酸共聚物的混合物,
ii.1-59重量%的A2,其是其它含烯属结构单元的烃聚合物,或
其它含烯属结构单元的烃聚合物的混合物,和
iii.0-35重量%的不同于A1和A2的添加剂,
b.0-50重量%的化合物B,其中化合物B是可分散或可溶于水的材料并且与分散体A的任何成分不同,
其中
-A和B的重量%是基于整个水性聚烯烃分散体的固含量计,
-分散体A的成分的重量%是基于分散体A的固含量计,
-分散体A的成分i至iii的重量%之和是100%。
2.根据权利要求1的纤维制品,其中水性分散体A包含以下成分:
i.51-95重量%的A1,其是具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的乙烯/(甲基)丙烯酸共聚物,或是各自具有基于共聚物的总重量计至少14重量%的(甲基)丙烯酸系基团含量的不同的乙烯/(甲基)丙烯酸共聚物的混合物,
ii.5-49重量%的A2,其是其它含烯属结构单元的烃聚合物,或
其它含烯属结构单元的烃聚合物的混合物,和
iii.0-35重量%的不同于A1和A2的添加剂,其中分散体A的成分的重量%是基于分散体A的固含量计,并且分散体A的成分i至iii的重量%之和是100%。
3.根据权利要求1或2的纤维制品,其中至少60重量%的A1具有基于共聚物的总重量计至少19重量%的(甲基)丙烯酸系基团含量。
4.根据权利要求1-3之一的纤维制品,其中至少60重量%的A2由含有乙烯结构单元的共聚物提供。
5.根据权利要求1-4之一的纤维制品,其中至少60重量%的A2选自下组:
具有乙烯和1-辛烯结构单元的聚烯烃,和
具有乙烯和丙烯结构单元的聚烯烃。
6.根据权利要求1-5之一的纤维制品,其中基于整个水性分散体的固含量计,作为B的成分,所述水性聚烯烃分散体含有小于5重量%、优选小于4重量%的PEG。
7.根据权利要求1-6之一的纤维制品,其中所述水性聚烯烃分散体包含分散的含有A1和A2的混杂粒子。
8.根据权利要求1-7之一的纤维制品,其中(整个)水性聚烯烃分散体具有10-60重量%的固含量。
9.根据权利要求1-8之一的纤维制品,其形成固体产品,优选由片材提供。
10.根据权利要求1-9之一的纤维制品,其中至少80重量%的纤维由纤维素纤维提供,从而由纸或纸板制品提供该纤维制品。
11.基于根据权利要求1-10之一的纤维制品的产品,其中用水性聚烯烃分散体处理的操作是通过将水性聚烯烃分散体作为粘合剂和/或作为纤维的涂料施加、然后除去水性聚烯烃分散体中的水进行。
12.根据权利要求11的产品,其中通过干燥除去所述水性聚烯烃分散体中的水,这优选在75℃以上的温度下进行。
13.根据权利要求11或12的产品,该产品由纸或纸板提供。
14.如权利要求1-10之一中规定的水性聚烯烃分散体作为粘合剂和/或作为涂料组合物用于纤维型基底的用途,优选用于纸或纸板。
15.根据权利要求14的用途,用于改善纤维型基底的与耐油性、防水性和/或防水蒸气性相关的阻隔性能。
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