CN106243332B - 一种增强型阻燃抗老化聚酯膜的制造方法 - Google Patents
一种增强型阻燃抗老化聚酯膜的制造方法 Download PDFInfo
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Abstract
本发明涉及一种增强型阻燃抗老化聚酯膜的制造方法，将具有阻燃、增强材料功能的氢氧化镁晶须，碳酸钙晶须，流酸钡，微胶囊化红磷阻燃剂等与乙二醇，对羟基苯甲酸等研磨反应得到阻燃、增强功能醇；将抗老化材料三嗪‑5光稳定剂，金红石型钛白粉，高温抗氧剂，UV‑327紫外线吸收剂与乙二醇等混合，研磨反应得到复合抗老化剂；将一定比例的精对苯二甲酸与乙二醇，阻燃、增强功能醇混合共缩聚，并在酯化反应后期连续加入复合抗老化剂制成一种具有增强型阻燃抗老化聚酯；将增强型阻燃抗老化聚酯双轴拉伸、热定型制成增强型阻燃抗老化聚酯膜。
Description
技术领域
本发明涉及一种增强型阻燃抗老化聚酯膜的制造方法，属于塑料制品制造技术领域。
背景技术
聚对苯二甲酸乙二醇酯(聚酯)，是由对苯二甲酸(PTA)和乙二醇(EG)经过缩聚反应制得，因其具备较高的熔融温度(Tm)和玻璃化转变温度(Tg)，并且具有良好的加工流变性，力学性能，耐磨性，抗蠕变性及电绝缘性，被广泛应用在合成纤维、瓶片、薄膜等领域。聚酯老化一般指聚酯在加工、储存及使用过程中，在外界(风吹、日晒、雨淋、冷、热)条件下，发生分子链降解及交联反应，导致性能变差，影响产品正常使用，是一种不可逆的变化，户外用聚酯产品真的不是使用损坏的，而是老化损坏，特别是农用薄膜。由于常规PET抗老化性能差，在热氧环境中寿命短等缺陷，限制了其在户外领域的应用。
PET分为纤维级聚酯和非纤维级聚酯。①纤维级聚酯用于制造涤纶短纤维和涤纶长丝，是供给涤纶纤维企业加工纤维及相关产品的原料。②非纤维级聚酯用于制造聚酯瓶类、聚酯薄膜、聚酯型材等用途，聚酯薄膜广泛应用于包装业、农业、电子电器、医疗卫生、建筑等领域，其中包装、农业是聚酯薄膜最大的应用市场，同时也是PET增长最快的领域。
聚酯分子结构高度对称，具有一定的结晶取向能力，故而具有较高的成膜性。双轴拉伸薄膜是指用双轴拉伸工艺制备的薄膜。由平膜在膜面内两个互相垂直的轴向上同时拉伸或依次拉伸得到。拉伸薄膜的聚合物在应力作用下发生分子链的取向，双向拉伸聚酯薄膜中长链分子沿平面上各方向都平衡的双轴取向，这种薄膜在膜面内各方向上的模量和强度很高，刚性好、透明、光泽度高等特点；无嗅、无味、无色、无毒、突出的强韧性；其拉伸强度是PC膜、PA膜的3倍，冲击强度是双轴拉伸PP膜的3-5倍，有极好的耐磨性、耐折叠性、耐针孔性和抗撕裂性等。广泛应用在包装、农用领域。
聚酯的基础原料是石油，也给人类埋伏了很多的火灾隐患。为了安全，必须提高聚酯的阻燃性。聚酯被广泛用于产业和户外领域，为了延长使用寿命，必须对其进行抗老化处理。
无机纳米材料熔点很高，通常都在800℃以上，添加到聚酯中正好弥补了聚酯在耐热方面的不足，使体系的玻璃化转变温度和热变形温度均有升高，具有阻燃性能。
氢氧化镁晶须，是塑料、橡胶等高分子材料优良的阻燃剂，与基材有很好的相容性。氢氧化镁晶须是一种新型填充型绿色环保阻燃剂，通过受热分解时释放出结合水，吸收大量的潜热，来降低它所填充的合成材料在火焰中的表面温度，具有抑制聚合物分解和对所产生的可燃气体进行冷却的作用。分解生成的氧化镁又是良好的耐火材料，也能帮助提高合成材料的抗火性能，同时它放出的水蒸气也可作为一种抑烟剂。氢氧化镁晶须是公认的橡塑行业中具有阻燃、抑烟、填充三重功能的优秀阻燃剂。与同类无机阻燃剂相比，具有更好的阻燃抑烟效果，填充高分子材料还有较好的增强作用。
碳酸钙晶须用于改性塑料、橡胶、聚氯乙烯等热塑性材料表现出显著的增强、增韧作用。还可以改善产品的弯曲强度、尺寸稳定性、热稳定性、抗老化性能；还可提升加工性能及制品的表面光洁度。
白炭黑可以强烈地反射紫外线，添加到聚乙烯树脂中可大大减少紫外线对聚乙烯的降解作用，从而达到延缓材料老化的目的。白炭黑颗粒比SiO2要小100-1000倍，将其添加到聚乙烯树脂中，有利于熔融拉膜。由于白炭黑的高流动性和小尺寸效应，使材料表面更加致密细洁，加之纳米颗粒的高强度，使膜的强度大大增强。
金红石型钛白粉在橡胶、塑料中既作为着色剂，又具有补强、防老化、填充作用。在塑料中加入少量金红石型钛白粉，在日光照射下，耐日晒，不开裂、不变色。可以提高塑料制品的耐热性、耐光性、耐候性，使塑料制品的物理化学性能得到改善，增强制品的机械强度，延长使用寿命。
蒙脱土是一类由纳米厚度的表面带负电的硅酸盐片层，依靠层间的静电作用而堆积在一起构成的土状矿物，其晶体结构中的晶胞是由两层硅氧四面体中间夹一层铝氧八面体构成。具有独特的一维层状纳米结构和阳离子交换性特性，从而赋予蒙脱土诸多改性的可能和应用领域的扩大。经改性的蒙脱土具有很强的吸附能力，良好的分散性能，可以广泛应用高分子材料行业作为纳米聚合物高分子材料的添加剂，提高抗冲击、抗疲劳、尺寸稳定性及气体阻隔性能等，从而起到增强聚合物综合物理性能的作用，同时改善物料加工性能。
紫外线吸收剂UV－327是一种性能卓越的高效防老化助剂,具有色浅、无毒、相容性好、迁移性小、易于加工等特点。它对聚合物有最大的保护作用，并有助于减少色泽，同时延缓泛黄和阻滞物理性能损失。与高温抗氧剂1098并用为显著的协同效应，显著改善PET的热氧稳定性和抗氧化性能，可有效地延长PET制品的使用期限。三嗪-5光稳定剂，该品可用为PET光稳定剂，可赋予PET制品优良的户外防老化性能。
发明内容
本发明的目的在于克服现有技术存在的不足，提供一种增强型阻燃抗老化聚酯膜的制造方法。
本发明提供的一种增强型阻燃抗老化聚酯膜的制造方法，采用如下步骤：
A)将质量份数2-4份纳米级流酸钡，0.5-1.5份月桂胺，2-4份白炭黑，2-4份纳米级有机化氢氧化镁晶须，2-4份表征参数直径为1-3μm、长度为5-25μm的碳酸钙晶须，1-2份微胶囊化红磷阻燃剂，0.2-0.5份硅烷偶联剂，4-8份对羟基苯甲酸，40-50份乙二醇，5-10份1、3-丙二醇，混合后，在50-60℃搅拌球磨机密闭研磨反应8-12h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数2-4份金红石型钛白粉,2-4份纳米蒙脱土，4-8份硬脂酸钡，0.1-0.3份硅烷偶联剂，0.8-1.2份三嗪-5光稳定剂，0.8-1.2份高温抗氧剂，1-2份UV-327紫外线吸收剂,10-15份乙二醇，0.2-0.4份乙二醇锑，0.2-0.8份乙醇胺混合，在40-50℃密闭搅拌球磨机研磨反应8-12h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的3-5份阻燃、增强功能醇与8-12份乙二醇、22-30份精对苯二甲酸共混打浆，升温至60-80℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2-3份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
本发明提供的一种增强型阻燃抗老化聚酯膜的制造方法，采用如下步骤：
A)将质量份数3份纳米级流酸钡，1份月桂胺，3份白炭黑，3份纳米级有机化氢氧化镁晶须，3份表征参数直径为2μm、长度为15μm的碳酸钙晶须，1.5份微胶囊化红磷阻燃剂，0.3份硅烷偶联剂，6份对羟基苯甲酸，45份乙二醇，7.5份1、3-丙二醇，混合后，在55℃搅拌球磨机密闭研磨反应10h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数3份金红石型钛白粉，3份纳米蒙脱土，6份硬脂酸钡，0.2份硅烷偶联剂，1份三嗪-5光稳定剂，1份高温抗氧剂，1.5份UV-327紫外线吸收剂，12份乙二醇，0.3份乙二醇锑，0.5份乙醇胺混合，在45℃密闭搅拌球磨机研磨反应10h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的4份阻燃、增强功能醇与10份乙二醇、26份精对苯二甲酸共混打浆，升温至70℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2.5份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
通常在塑料中添加改性功能材料制备功能塑料都是以牺牲塑料原有强度、韧性等物理性能为代价，与现有技术相比，本发明在聚酯合成反应过程中添加阻燃、增强材料、抗老化改性剂参与聚合反应，因改性剂参与聚合反应，改性基团引入聚酯分子，其分散性能好，聚酯品质和加工性能均有提高，可制成高品质增强型阻燃抗老化聚酯膜。
具体实施方式
下面将结合具体实施例对本发明作详细的介绍：本发明所述的一种增强型阻燃抗老化聚酯膜的制造方法，采用如下步骤：
A)将质量份数2-4份纳米级流酸钡，0.5-1.5份月桂胺，2-4份白炭黑，2-4份纳米级有机化氢氧化镁晶须，2-4份表征参数直径为1-3μm、长度为5-25μm的碳酸钙晶须，1-2份微胶囊化红磷阻燃剂，0.2-0.5份硅烷偶联剂，4-8份对羟基苯甲酸，40-50份乙二醇，5-10份1、3-丙二醇，混合后，在50-60℃搅拌球磨机密闭研磨反应8-12h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数2-4份金红石型钛白粉,2-4份纳米蒙脱土，4-8份硬脂酸钡，0.1-0.3份硅烷偶联剂，0.8-1.2份三嗪-5光稳定剂，0.8-1.2份高温抗氧剂，1-2份UV-327紫外线吸收剂,10-15份乙二醇，0.2-0.4份乙二醇锑，0.2-0.8份乙醇胺混合，在40-50℃密闭搅拌球磨机研磨反应8-12h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的3-5份阻燃、增强功能醇与8-12份乙二醇、22-30份精对苯二甲酸共混打浆，升温至60-80℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2-3份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
实施例1：一种增强型阻燃抗老化聚酯膜的制造方法，采用如下步骤：
A)将质量份数2份纳米级流酸钡，0.5份月桂胺，2份白炭黑，2份纳米级有机化氢氧化镁晶须，2份表征参数直径为1μm、长度为5μm的碳酸钙晶须，1份微胶囊化红磷阻燃剂，0.2份硅烷偶联剂，4份对羟基苯甲酸，40份乙二醇，5份1、3-丙二醇，混合后，在50℃搅拌球磨机密闭研磨反应8h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数2份金红石型钛白粉,2份纳米蒙脱土，4份硬脂酸钡，0.1份硅烷偶联剂，0.8份三嗪-5光稳定剂，0.8份高温抗氧剂，1份UV-327紫外线吸收剂,10份乙二醇，0.2份乙二醇锑，0.2份乙醇胺混合，在40℃密闭搅拌球磨机研磨反应8h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的3份阻燃、增强功能醇与8份乙二醇、22份精对苯二甲酸共混打浆，升温至60℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
实施例2：一种增强型阻燃抗老化聚酯膜的制造方法，采用如下步骤：
A)将质量份数3份纳米级流酸钡，1份月桂胺，3份白炭黑，3份纳米级有机化氢氧化镁晶须，3份表征参数直径为2μm、长度为15μm的碳酸钙晶须，1.5份微胶囊化红磷阻燃剂，0.3份硅烷偶联剂，6份对羟基苯甲酸，45份乙二醇，7.5份1、3-丙二醇，混合后，在55℃搅拌球磨机密闭研磨反应10h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数3份金红石型钛白粉，3份纳米蒙脱土，6份硬脂酸钡，0.2份硅烷偶联剂，1份三嗪-5光稳定剂，1份高温抗氧剂，1.5份UV-327紫外线吸收剂，12份乙二醇，0.3份乙二醇锑，0.5份乙醇胺混合，在45℃密闭搅拌球磨机研磨反应10h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的4份阻燃、增强功能醇与10份乙二醇、26份精对苯二甲酸共混打浆，升温至70℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2.5份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
实施例3：一种增强型阻燃抗老化聚酯膜的制造方法，采用如下步骤：
A)将质量份数4份纳米级流酸钡，1.5份月桂胺，4份白炭黑，4份纳米级有机化氢氧化镁晶须，4份表征参数直径为3μm、长度为25μm的碳酸钙晶须，2份微胶囊化红磷阻燃剂，0.5份硅烷偶联剂，8份对羟基苯甲酸，50份乙二醇，10份1、3-丙二醇，混合后，在60℃搅拌球磨机密闭研磨反应12h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数4份金红石型钛白粉,4份纳米蒙脱土，8份硬脂酸钡，0.3份硅烷偶联剂，1.2份三嗪-5光稳定剂，1.2份高温抗氧剂，2份UV-327紫外线吸收剂,15份乙二醇，0.4份乙二醇锑，0.8份乙醇胺混合，在50℃密闭搅拌球磨机研磨反应12h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的5份阻燃、增强功能醇与12份乙二醇、30份精对苯二甲酸共混打浆，升温至80℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2-3份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
本发明所述的实施例并不限于以上所述实施例，通过前述公开的数值范围，在就具体实施例中进行任意替换，从而可以得到无数个实施例，对此不一一例举。
Claims (2)
1.一种增强型阻燃抗老化聚酯膜的制造方法，其特征在于该制造方法采用如下步骤：
A)将质量份数2-4份纳米级硫酸钡，0.5-1.5份月桂胺，2-4份白炭黑，2-4份纳米级有机化氢氧化镁晶须，2-4份表征参数直径为1-3μm、长度为5-25μm的碳酸钙晶须，1-2份微胶囊化红磷阻燃剂，0.2-0.5份硅烷偶联剂，4-8份对羟基苯甲酸，40-50份乙二醇，5-10份1,3-丙二醇，混合后，在50-60℃搅拌球磨机密闭研磨反应8-12h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数2-4份金红石型钛白粉,2-4份纳米蒙脱土，4-8份硬脂酸钡，0.1-0.3份硅烷偶联剂，0.8-1.2份三嗪-5光稳定剂，0.8-1.2份高温抗氧剂1098，1-2份UV-327紫外线吸收剂,10-15份乙二醇，0.2-0.4份乙二醇锑，0.2-0.8份乙醇胺混合，在40-50℃密闭搅拌球磨机研磨反应8-12h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的3-5份阻燃、增强功能醇与8-12份乙二醇、22-30份精对苯二甲酸共混打浆，升温至60-80℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2-3份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
2.一种增强型阻燃抗老化聚酯膜的制造方法，其特征在于该制造方法采用如下步骤：
A)将质量份数3份纳米级硫酸钡，1份月桂胺，3份白炭黑，3份纳米级有机化氢氧化镁晶须，3份表征参数直径为2μm、长度为15μm的碳酸钙晶须，1.5份微胶囊化红磷阻燃剂，0.3份硅烷偶联剂，6份对羟基苯甲酸，45份乙二醇，7.5份1,3-丙二醇，混合后，在55℃搅拌球磨机密闭研磨反应10h得到阻燃、增强功能醇，70℃保温48h内用完；
B)将质量份数3份金红石型钛白粉，3份纳米蒙脱土，6份硬脂酸钡，0.2份硅烷偶联剂，1份三嗪-5光稳定剂，1份高温抗氧剂1098，1.5份UV-327紫外线吸收剂，12份乙二醇，0.3份乙二醇锑，0.5份乙醇胺混合，在45℃密闭搅拌球磨机研磨反应10h得到复合抗老化剂，70℃真空脱水至含水量小于1％时保温48h内用完；
C)按质量份数，取步骤A)制备的4份阻燃、增强功能醇与10份乙二醇、26份精对苯二甲酸共混打浆，升温至70℃真空脱水，当含水量小于1％时加入到聚合装置并升温至250℃、压力0.15MPa进行酯化反应，酯化反应后期，伴随着酯化反应连续加入2.5份由步骤B)制备的复合抗老化剂，加热至270℃反应50min，再加热至285℃，抽真空度至100Pa以下进行共缩聚反应直至制成增强型阻燃抗老化聚酯；
D)将步骤C)制备的增强型阻燃抗老化聚酯由熔体泵从缩聚釜输出至熔体计量泵，经熔体计量泵计量从挤出模口挤出，连续双轴向拉伸、热定型制成增强型阻燃抗老化聚酯膜。
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