CN107531890A - 用于制备聚对苯二甲酸乙二醇酯聚合物的方法、聚对苯二甲酸乙二醇酯聚合物纱线和包含该纱线的汽车垫 - Google Patents
用于制备聚对苯二甲酸乙二醇酯聚合物的方法、聚对苯二甲酸乙二醇酯聚合物纱线和包含该纱线的汽车垫 Download PDFInfo
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- polyethylene terephthalate
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 39
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Abstract
本发明涉及通过除了形成常规聚对苯二甲酸乙二醇酯键的乙二醇(EG,Ethyleneglycol)和对苯二甲酸(TPA,terephthalic acid)以外还引入无机颗粒(金属)来制造具有改善的耐磨性的聚对苯二甲酸乙二醇酯聚合物的方法,以及通过使用由上述制造方法制造的聚对苯二甲酸乙二醇酯聚合物而制造的纱线和汽车垫。当通过使用上述聚对苯二甲酸乙二醇酯聚合物制造纱线和汽车垫时,纱线的密度提高,并且可以改善汽车垫的耐磨性。
Description
技术领域
本发明涉及通过除了构成常规聚对苯二甲酸乙二醇酯键的乙二醇(EG,Ethyleneglycol)和对苯二甲酸(TPA,terephthalic acid)以外还引入无机颗粒(金属)来制造耐磨性改善的聚对苯二甲酸乙二醇酯聚合物的方法,以及通过使用由上述制造方法制造的聚对苯二甲酸乙二醇酯聚合物而制造的纱线和汽车垫。
背景技术
通常,聚酯树脂,特别是聚对苯二甲酸乙二醇酯树脂是由二羧酸或其成酯衍生物和二醇或其成酯衍生物合成的线性聚合物,并且因为其成本低,机械性能和化学性能优异以及阻气性优异,而广泛用于诸如容器、膜和纤维等各种制品。同时,通过缩聚法制造聚酯。在根据外部条件的平衡反应中,在高温和高真空的条件下获得可商用的粘度,并且在最终聚合物中残留有一定量的低聚物。
同时,目前汽车垫市场主要由包括PET针刺棉和尼龙BCF的市场组成。在传统的PET汽车垫的情况下,其价格与尼龙汽车垫相比较低,但是由于汽车垫要求的耐磨性低(300次水平),它仅被用于小型汽车。
为了扩大PET汽车垫的市场,我们开发了本发明,以在PET汽车垫中发展尼龙水平的耐磨性,并且通过实现尼龙水平的1000次以上的耐磨性而成功地商业化。
发明内容
技术问题
本发明涉及提供一种通过在聚对苯二甲酸乙二醇酯聚合物的制造中另外引入无机颗粒而改善耐磨性的聚对苯二甲酸乙二醇酯聚合物,以及使用该聚合物制造纱线和汽车垫的方法。
技术方案
根据本发明的示例性实施方式,制备聚对苯二甲酸乙二醇酯聚合物的方法可以包括通过混合乙二醇(EG,Ethyleneglycol)和对苯二甲酸(TPA,Terephthalic acid)制备浆料的步骤;使所述浆料酯化的步骤;以及使所述浆料缩聚的步骤,其中,在酯化步骤之后或之前,或者在缩聚步骤之前,添加包含无机颗粒的母料。
无机颗粒优选为选自包含硫酸钡、二氧化硅、高岭土、氧化铝(Al2O3)、TiO2、碳酸钙(CaCO3)、云母、沸石、滑石、玻璃珠粉末和磷酸钙的组中的至少一种。
同时,无机颗粒的添加量优选为0.01重量%~5重量%。
在这种情况下,硫酸钡的含量小于0.01重量%,耐磨性下降。如果硫酸钡含量大于5重量%,则机械性能下降。
另外,无机颗粒的平均粒径优选为0.1μm~10μm。在这种情况下,如果平均粒径小于0.1μm,由于细颗粒的凝聚而导致分散性下降,并且耐磨性下降。如果平均粒径大于10μm,则机械性能下降。
另外,聚对苯二甲酸乙二醇酯聚合物的本征粘度(I.V.)优选为0.8以上。
另外,本发明提供了聚对苯二甲酸乙二醇酯纱线,其使用通过所述制造方法制造的聚对苯二甲酸乙二醇酯聚合物制造,且纱线的纤度为800d~1500d以下,优选为850d~1350d。
同时,本发明提供了包含所述聚对苯二甲酸乙二醇酯纱线的汽车垫。
有益效果
在使用聚对苯二甲酸乙二醇酯聚合物制造纱线和汽车垫的情况下,本发明在制造聚对苯二甲酸乙二醇酯聚合物时,可以通过添加无机颗粒来提高纱线的密度,而改善汽车垫的耐磨性。
具体实施方式
本发明的聚对苯二甲酸乙二醇酯聚合物的制造方法的特征在于,其包括通过混合乙二醇(EG,Ethyleneglycol)和对苯二甲酸(TPA,Terephthalic acid)而制造浆料的步骤;使所述浆料酯化的步骤;以及使所述浆料缩聚的步骤,其中,在酯化步骤之后或之前,或者在缩聚步骤之前,添加包含无机颗粒的母料。
在本发明中,在酯化反应之后和缩聚步骤之前引入无机颗粒,以实现聚对苯二甲酸乙二醇酯的耐磨性改善效果,并使无机颗粒凝聚和分散在聚对苯二甲酸乙二醇酯聚合物中。
此处,无机颗粒优选为选自包含硫酸钡、二氧化硅、高岭土、氧化铝(Al2O3)、TiO2、碳酸钙(CaCO3)、云母、沸石、滑石、玻璃珠粉末和磷酸钙的组中的一种或多种,但不限于此。
根据本发明,对于无机颗粒,硫酸钡和二氧化硅是更优选使用的。硫酸钡和二氧化硅用于无机颗粒的原因是它们具有较高的硬度,并且折射率与聚对苯二甲酸乙二醇酯类似,当添加硫酸钡作为无机颗粒时,可以使纱线的光泽变化最小化。
本发明在酯化之后或缩聚之前引入包含无机颗粒的母料。在这种情况下,引入的无机颗粒的平均粒径(D50)优选为0.1μm~10μm,更优选为1.0μm~5.0μm。如果无机颗粒的平均粒径小于0.1μm,由于细颗粒之间的凝聚难以确保分散性,因此耐磨性的改善效果低,而如果平均粒径大于10μm,存在可纺性的问题,且生产率下降。同时,由于细颗粒凝聚而导致的可纺性下降和压力上升的问题主要是因为粒径、形状、表面积、电荷和化学性质,其中,粒径分散直接影响分散性。
在这种情况下,本发明包括两种以上不同种类的无机颗粒的粒径以改善耐磨性。相对于使用相同尺寸的颗粒的情况,在使用相对不同尺寸的颗粒的情况下,由于通过较大颗粒在聚合物和纱线的表面上形成微细突起,可以额外地改善耐磨性。
在低于平均粒径的分布小于50%的情况下,由于分子之间的分子力,而非常迅速地发生凝聚,从而大大下降了可纺性。因此,根据本发明,使用平均粒径分布为50%以上的硫酸钡颗粒以防止凝聚。
同时,相对于聚对苯二甲酸乙二醇酯聚合物的总重量,无机颗粒的添加量优选为0.01重量%~5重量%,更优选为0.1重量%~1.5重量%。
在无机颗粒含量小于0.01重量%的情况下,耐磨性的改善效果轻微。如果该含量大于5重量%,则功能性的改善不大,且可纺性和性能下降。
如上所述制造的聚对苯二甲酸乙二醇酯聚合物的本征粘度(I.V.)优选为0.8以上。
在通过使用本征粘度为0.8以上的聚对苯二甲酸乙二醇酯聚合物制造纱线的情况下,纱线的纤度优选为800d~1500d,更优选为850d~1350d。
在纱线的纤度在上述范围内的情况下,可以使用该纱线生产耐磨性改善的汽车垫。
在下文中,详细描述使用根据本发明制造的聚对苯二甲酸乙二醇酯聚合物制造纱线的方法。
首先,将根据本发明制造的聚对苯二甲酸乙二醇酯聚合物在245℃~335℃下熔融纺丝并通过喷丝头。
作为本发明基础的聚对苯二甲酸乙二醇酯树脂包含90摩尔%以上的对苯二甲酸乙二醇酯重复单元。
然后,在冷却区以0.2米/秒~1.0米/秒的速度冷却。在这种情况下,将冷却温度调节至10℃~35℃。如果冷却空气的速度小于0.2米/秒,则冷却效果不够。如果冷却空气的速度大于1.0米/秒,则纱线的晃动很多,从而导致纺丝加工性的问题。如果冷却温度低于10℃,则在经济上是不利的,如果冷却温度高于35℃,则冷却效果下降。
本发明经过在冷却后进行加油的纺丝修整步骤。在修整涂布器中,在两个步骤中使用不掺水型乳液或水溶性乳液进行油的一次和二次润滑,从而提高纱线的收集能力、润滑性和光滑度。
然后,以100米/分~1,000米/分(优选为400米/分~800米/分)的速度从进料辊向拉伸辊提供长丝,其中,拉伸辊的温度为100℃~230℃,且为2.5倍~6.0倍、优选为3.5倍~5.0倍的进料辊速度。如果拉伸速度小于2.5倍,则不能充分进行拉伸。如果拉伸速度大于6.0倍,聚对苯二甲酸乙二醇酯长丝不能承受拉伸并且由于聚对苯二甲酸乙二醇酯材料的特性而折叠。
经过拉伸辊的长丝通过具有变形喷嘴的变形单元以提供蓬松性,其中,通过在所述变形单元内以3kg/cm2~10kg/cm2的压力喷射150℃~270℃的加热液体,所述长丝卷曲为不规则的三维形状,其中,卷曲率为3%~50%。
在这种情况下,加热液体的温度优选为150℃~270℃。如果温度低于150℃,变形效果下降。如果温度高于270℃,则长丝损坏。此外,加热液体的压力优选为3kg/cm2~10kg/cm2,如果其小于3kg/cm2,则变形效果下降。如果其大于10kg/cm2,则长丝损坏。
经过变形单元的长丝通过冷却部,其被冷却并通过交缠装置。在此部分中,为了改善纱线的收集能力,在2.0kg/m2~8.0kg/m2的压力下提供轻微的扭曲和打结,并且在0次/分~40次/米的范围内,优选为10次~25次。在交缠超过40次的情况下,即使在染色和后加工之后,交缠部分不会解开,并且损坏毡毯的外部。
然后,以拉伸辊的速度的0.65倍~0.95倍的速度从松弛辊通过,使松弛率为5%~35%,然后在最终卷绕装置中进行卷绕。通常将卷绕装置的速度调节为使纱线的张力在50g~350g的范围内。在这种情况下,如果卷绕装置中的张力小于50g,则不能进行卷绕。如果张力大于350g,蓬松度下降,并且在很大程度上导致纱线收缩,并引起高张力和工作问题。同时,如果松弛辊的速度小于拉伸辊的速度的0.65倍,则不会发生卷绕。如果速度大于0.95倍,则蓬松度下降,并且很大程度上导致纱线收缩,并引起高张力和工作问题。
上述方法涉及仅由聚对苯二甲酸乙二醇酯树脂制造的BCF,并且当根据毡毯的用途制造涂料染色纱线时,加工步骤与上述相同。此外,可以通过将一定量的着色剂引入供给原料的基础碎片输入中并纺丝来制造涂料染色纱线。
如上所述,根据本发明制备的聚对苯二甲酸乙二醇酯复丝经过后加工并制成毡毯。由本发明的BCF纱线制成的毡毯可以以本领域技术人员已知的任何方法制造。优选地,将多根BCF纱线制成缆绳并热固定,然后与主衬里一起编织。然后施加胶乳粘合剂和次级底片。可以制造具有约2mm~20mm的绒毛高度的割绒型毡毯或圈绒型毡毯。
在下文中,参考以下实施例更详细地描述本发明。然而,以下实施例是对本发明的说明,不应解释为限制本发明的范围。以下列方式评价在本发明的实施例和比较例中制备的纱线的性能。
1.如何测量纱线的强度和伸长率
纱线处在标准状态条件下,即在25℃的温度和65%RH的相对湿度的稳定温度湿度室中24小时,然后通过拉伸测试机按照ASTM 2256方法测量样品。
2.卷曲率和标准偏差
通过TYT-EW(变形纱线测试机)测量仪测量卷曲率和标准偏差,测量长度为20米,并以2米间隔测量5次。加热区的温度为130℃,测量速度为20米/分。
3.汽车垫的耐磨性评价方法
汽车垫的耐磨性在以下条件下测量,基于在汽车垫底部暴露于对应于外部评价水平2.5的水平时的最终磨损次数来评价汽车垫的耐磨性的数量。
相关测试方法规格:ASTM D3884
测试方法:Hyundai Motor MS300-35
测试设备:Taber磨损测试机
样品尺寸:直径130mm的圆形样品
测试条件
1)砂轮:H-18
2)转速:70次/分
3)负荷:1000g
4)评价方法:外部评价1~5级(通过Hyundai Motor公司的MS343-15的3级以上(3、4、5级))
5)评价标准:5级 根本没有显示磨损
4级 磨损略微可见或几乎看不见。
3级 磨损略微存在,但可见
2级 磨损略微严重
1级 很严重
实施例1
将通过相对于100重量份的对苯二甲酸混合50重量份的乙二醇而制备的浆料引入酯化反应器中,并在0.5托的压力下在250℃下加压4小时以使水流出反应器,以进行酯化反应,产生对苯二甲酸二(2-羟乙基)酯。在这种情况下,在酯化反应结束时加入300ppm的磷系热稳定剂。同时,在酯化反应后,在该聚合物中加入0.1重量%的90%的平均粒径为1.4μm的硫酸钡颗粒和10%的粒径为4.2μm的硫酸钡颗粒。此后,在缩聚反应的初始阶段加入300ppm锑催化剂作为聚合催化剂,以60℃/小时将温度从250℃升至285℃,并将压力降至0.5托,进行缩聚反应。
通过具有128孔和Y形横截面的喷丝头,将聚对苯二甲酸乙二醇酯聚合物在290℃熔融纺丝。离开喷丝头的聚合物在喷嘴底部通过0.5米/秒和20℃的冷却空气冷却,然后通过乳液供给装置。赋予纱线的乳液以598米/分的速度经过保持在90℃的进料辊,然后在拉伸辊中在190℃下以2,840米/分的速率拉伸。经过拉伸辊的纱线通过变形喷嘴,纱线被赋予卷曲。在这种情况下,热空气的温度为200℃,压力为7kg/cm2,背压为5kg/cm2。在通过冷却水冷却的收集器中,在4.0kg/m2的压力下以20次/米的比例进行交缠。纱线以2250米/分通过松弛辊,松弛约21%,并在卷绕机中卷绕。测量通过该方法制造的聚对苯二甲酸乙二醇酯BCF纱线的纤度、强度和卷曲值,并示于表1中。
使用聚对苯二甲酸乙二醇酯BCF纱线制造汽车垫,并测量其耐磨性。结果示于表1。
实施例2~4
以与实施例1相同的方法制备聚合物、纱线和汽车垫,不同之处在于,如表1所示改变聚对苯二甲酸乙二醇酯聚合物的本征粘度和纱线的纤度。
实施例5
以与实施例1相同的方法制备聚合物、纱线和汽车垫,不同之处在于,如表1所示改变聚对苯二甲酸乙二醇酯聚合物的本征粘度和纱线的纤度,并且在聚对苯二甲酸乙二醇酯聚合物的制造中引入0.1重量%的90%的平均粒径为1.4μm的二氧化硅颗粒和10%的平均粒径为4.2μm的二氧化硅颗粒来代替硫酸钡。
实施例6
以与实施例5相同的方法制备聚合物、纱线和汽车垫,不同之处在于,如表1所示改变聚对苯二甲酸乙二醇酯聚合物纱线的纤度。
实施例7~10
以与实施例1相同的方法制备聚合物、纱线和汽车垫,不同之处在于,如表1所示改变聚对苯二甲酸乙二醇酯聚合物的本征粘度、纱线的纤度和硫酸钡含量。
比较例1
以与实施例1相同的方法制备聚合物、纱线和汽车垫,不同之处在于,在聚对苯二甲酸乙二醇酯聚合物的制造过程中不加入硫酸钡,并且如表1所示改变聚合物的粘度和纱线的纤度。
比较例2
以与实施例1相同的方法制备聚合物、纱线和汽车垫,不同之处在于,如表1所示改变聚对苯二甲酸乙二醇酯聚合物的本征粘度和纱线的纤度。
比较例3
以与比较例1相同的方法制备聚合物、纱线和汽车垫,不同之处在于,如表1所示改变聚对苯二甲酸乙二醇酯聚合物的本征粘度和纱线的纤度。
表1
如表1所示,在酯化反应后引入硫酸钡或二氧化硅,在聚合物的本征粘度为0.8以上,且纱线的纤度为850~1350旦的情况下,制造的汽车垫(实施例1~10)的耐磨性改善。
同时发现,当在聚合物的制造中不引入无机颗粒(比较例3)时,所制造的汽车垫的耐磨性下降。还发现,当在聚合物的制造过程中在不添加无机颗粒的情况下聚合物的本征粘度小于0.8(比较例1)时,汽车垫的耐磨性下降。同时发现,在聚合物的制备中引入无机颗粒,但是当聚合物的本征粘度小于0.8时(比较例2),汽车垫的耐磨性也下降。
虽然已经结合目前被认为是实用的示例性实施方式的情况描述了本发明,但应当理解的是,本发明不限于所公开的实施方式,相反,其旨在覆盖包括在所附权利要求的精神和范围内的各种修改和等同设置。
Claims (8)
1.一种制备聚对苯二甲酸乙二醇酯聚合物的方法,其特征在于包括以下步骤:
通过混合乙二醇(EG,Ethyleneglycol)和对苯二甲酸(TPA,Terephthalic acid)制备浆料;
使所述浆料酯化;和
使所述浆料缩聚,
其中,在所述酯化之后或之前,或者在所述缩聚之前,引入包含无机颗粒的母料或无机颗粒。
2.如权利要求1所述的制备聚对苯二甲酸乙二醇酯聚合物的方法,
其中,所述无机颗粒是选自包含硫酸钡、二氧化硅、高岭土、氧化铝(Al2O3)、TiO2、碳酸钙(CaCO3)、云母、沸石、滑石、玻璃珠粉末和磷酸钙的组中的至少一种。
3.如权利要求1所述的制备聚对苯二甲酸乙二醇酯聚合物的方法,
其中,所述无机颗粒的添加量为0.01重量%~5重量%。
4.如权利要求1所述的制备聚对苯二甲酸乙二醇酯聚合物的方法,
其中,所述无机颗粒的平均粒径为0.1μm~10μm。
5.如权利要求1所述的制备聚对苯二甲酸乙二醇酯聚合物的方法,
其中,所述聚对苯二甲酸乙二醇酯聚合物的本征粘度(IV)为0.8以上。
6.通过权利要求1~5中任一项所述的方法制造的聚对苯二甲酸乙二醇酯聚合物。
7.由权利要求6所述的聚对苯二甲酸乙二醇酯聚合物制造的聚对苯二甲酸乙二醇酯纱线,
其中,所述纱线的纤度为800旦~1,500旦。
8.包含权利要求7所述的聚对苯二甲酸乙二醇酯纱线的汽车垫。
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CN201680002997.1A Pending CN107531890A (zh) | 2016-04-19 | 2016-08-24 | 用于制备聚对苯二甲酸乙二醇酯聚合物的方法、聚对苯二甲酸乙二醇酯聚合物纱线和包含该纱线的汽车垫 |
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US (1) | US20180094101A1 (zh) |
EP (1) | EP3447079A4 (zh) |
JP (1) | JP2018516997A (zh) |
KR (1) | KR101767900B1 (zh) |
CN (1) | CN107531890A (zh) |
MX (1) | MX2017004289A (zh) |
WO (1) | WO2017183771A1 (zh) |
Cited By (4)
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CN110396181A (zh) * | 2018-04-24 | 2019-11-01 | 中国石油化工股份有限公司 | 一种快速结晶聚酯及其热灌装聚酯瓶片的制备方法 |
CN110607571A (zh) * | 2019-09-24 | 2019-12-24 | 东莞市博斯蒂新材料有限公司 | 一种涤纶丝及其制备方法 |
CN110972484A (zh) * | 2018-08-09 | 2020-04-07 | 晓星高新材料株式会社 | 包含聚对苯二甲酸乙二醇酯膨体连续纤丝的簇绒地毯 |
CN117384469A (zh) * | 2023-10-16 | 2024-01-12 | 台州天奇鞋业股份有限公司 | 一种透气性耐磨鞋面材料及制备方法 |
Families Citing this family (2)
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KR102274875B1 (ko) * | 2018-04-24 | 2021-07-08 | 효성화학 주식회사 | 필름용 폴리에틸렌 테레프탈레이트 중합물의 제조방법 |
EP3620557A1 (en) | 2018-09-05 | 2020-03-11 | Hyosung Advanced Materials Corporation | Polyethyleneterephthalate bulked continuous filament and tufted carpet including the same |
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CN110396181A (zh) * | 2018-04-24 | 2019-11-01 | 中国石油化工股份有限公司 | 一种快速结晶聚酯及其热灌装聚酯瓶片的制备方法 |
CN110396181B (zh) * | 2018-04-24 | 2021-12-07 | 中国石油化工股份有限公司 | 一种快速结晶聚酯及其热灌装聚酯瓶片的制备方法 |
CN110972484A (zh) * | 2018-08-09 | 2020-04-07 | 晓星高新材料株式会社 | 包含聚对苯二甲酸乙二醇酯膨体连续纤丝的簇绒地毯 |
CN110972484B (zh) * | 2018-08-09 | 2021-05-18 | 晓星高新材料株式会社 | 包含聚对苯二甲酸乙二醇酯膨体连续纤丝的簇绒地毯 |
CN110607571A (zh) * | 2019-09-24 | 2019-12-24 | 东莞市博斯蒂新材料有限公司 | 一种涤纶丝及其制备方法 |
CN117384469A (zh) * | 2023-10-16 | 2024-01-12 | 台州天奇鞋业股份有限公司 | 一种透气性耐磨鞋面材料及制备方法 |
CN117384469B (zh) * | 2023-10-16 | 2024-05-07 | 台州天奇鞋业股份有限公司 | 一种透气性耐磨鞋面材料及制备方法 |
Also Published As
Publication number | Publication date |
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EP3447079A1 (en) | 2019-02-27 |
WO2017183771A1 (ko) | 2017-10-26 |
US20180094101A1 (en) | 2018-04-05 |
EP3447079A4 (en) | 2019-10-02 |
MX2017004289A (es) | 2017-12-08 |
JP2018516997A (ja) | 2018-06-28 |
KR101767900B1 (ko) | 2017-08-16 |
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