CN112590346A - 一种抗菌高阻隔共挤复合膜及其制备方法 - Google Patents
一种抗菌高阻隔共挤复合膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种抗菌高阻隔共挤复合膜及其制备方法。该薄膜包括5层结构,由上至下依次为聚酰胺上表层、抗菌阻燃共聚聚酰胺层、EVOH阻隔层、阻燃聚酰胺层、聚酰胺下表层;其中,所述抗菌阻燃聚酰胺层组份按照质量百分比由共聚聚酰胺62‑82%、载锌蒙脱土复合抗菌剂3‑8%、纳米氢氧化镁15‑30%组成。本发明提供的抗菌高阻隔共挤复合膜阻燃性和抗菌性能优异,阻隔性好,可高温杀菌,特别适合在食品、药品及电子产品的包装,具备广阔的市场应用前景。
Description
技术领域
本发明属于薄膜包装技术领域,具体涉及一种抗菌高阻隔共挤复合膜及其制备方法。
背景技术
力学性能优异的软包装高阻隔功能性薄膜势必成为未来软包装的一个新的增长点,例如双向拉伸PA6/EVOH共挤复合薄膜,既具备的双向拉伸尼龙薄膜优异的拉伸强度、耐穿刺性能及耐化学性能,有具备的EVOH的高阻隔特性,在食品、日用品、药品及电子产品等领域逐步得以应用,具备旷阔的市场前景。例如将双向拉伸PA6/EVOH共挤复合薄膜应用于糕点、干果及酱料类产品的包装,可提供良好的保香保鲜效果,并延长产品的保质期,获得一致好评;同时在农药等领域也有应用,可解决复铝箔类包装袋不耐折导致阻隔性能降低等问题。
但是现有的PA6/EVOH共挤复合薄膜的阻隔性能受到温、湿度影响比较大,在23℃,85%RH的高湿环境下氧气透过率高达20.2cc/m2˙day,限制了其应用领域,尤其在电子产品领域或一些特定的食药品、日化用品等对阻隔和阻燃性能比普通日化产品要求高的领域,现有的PA6/EVOH共挤复合薄膜往往难以符合要求。
发明内容
本发明的目的在于克服现有技术的不足之处,提供了一种抗菌高阻隔共挤复合膜及其制备方法,解决了上述背景技术中高湿条件下阻隔性降低、不具备抗菌和阻燃性的问题。
本发明解决其技术问题所采用的技术方案之一是:提供了一种抗菌高阻隔共挤复合膜,由上至下依次设置为聚酰胺上表层、抗菌阻燃共聚聚酰胺层、EVOH阻隔层、阻燃聚酰胺层和聚酰胺下表层;其中,
所述抗菌阻燃共聚聚酰胺层按照质量百分比由共聚聚酰胺62-82%、载锌蒙脱土复合抗菌剂3-8%和纳米氢氧化镁15-30%组成;
所述EVOH阻隔层为聚乙烯-乙烯醇共挤物;
所述阻燃聚酰胺层按照质量百分比由聚酰胺91-96%、有机蒙脱土3-6%和氨基硅油1-3%组成。
在本发明一较佳实施例中,所述载锌蒙脱土复合抗菌剂,按照如下步骤制备而成:
步骤a、将钠基蒙脱土添加到去离子水中,用搅拌机搅拌均匀,得到2-5wt%的钠基蒙脱土悬浮液;
步骤b、往钠基蒙脱土悬浮液中添加30-60mmol的硝酸锌在40-60℃条件下恒温搅拌2-4h,得到载锌蒙脱土悬浮液;
步骤C、往载锌蒙脱土悬浮液中继续添加40-80mmol季铵盐,在40-60℃条件下恒温搅拌2-4h,抽滤,得到白色沉淀物;
步骤d、将白色沉淀物在80℃下干燥24h,研磨,过400筛,即得到载锌蒙脱土复合抗菌剂。
在本发明一较佳实施例中,所述聚酰胺上表层和聚酰胺下表层按照质量百分比由聚酰胺98-99.8%、开口剂0.1-1%和爽滑剂0.1-1%组成。所述聚酰胺为尼龙6、尼龙46、尼龙56、尼龙66、尼龙610、尼龙612、尼龙1010、尼龙1212的至少一种。所述开口剂为二氧化硅、碳酸钙、磷石膏粉、空心玻璃微珠、亚克力、PS交联颗粒、有机硅交联颗粒的至少一种。所述爽滑剂为酰胺类爽滑剂、蜡类爽滑剂、硅酮类爽滑剂的至少一种。
在本发明一较佳实施例中,所述共聚聚酰胺的熔点为160-190℃,所述共聚聚酰胺由尼龙6、尼龙66、尼龙11、尼龙12、尼龙1010、尼龙1212中的至少两种单体共聚而成。
在本发明一较佳实施例中,复合膜的总厚度为15-25μm,所述聚酰胺上表层和聚酰胺下表层的厚度均为1-2μm,所述EVOH阻隔层的厚度为3-5μm。
本发明解决其技术问题所采用的技术方案之二是:提供了上述抗菌高阻隔共挤复合膜的制备方法,包括如下步骤:
步骤一、将聚酰胺上表层、聚酰胺下表层的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的表层母粒烘干,备用;
步骤二、将抗菌阻燃共聚聚酰胺层中的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的抗菌母粒烘干,备用;
步骤三、将阻燃聚酰胺层中的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的阻燃母粒烘干,备用;
步骤四、将上述表层母粒、抗菌母粒、阻燃母粒分别投入挤出机,分别制备得到聚酰胺上表层和聚酰胺下表层、抗菌阻燃共聚聚酰胺层、阻燃聚酰胺层;制备聚乙烯-乙烯醇共挤物的EVOH阻隔层;其中,聚酰胺上表层和聚酰胺下表层、阻燃聚酰胺层的挤出机温度及其T型模头的温度控制在220-240℃之间,抗菌阻燃共聚聚酰胺层和EVOH阻隔层的挤出机温度及其T型模头的温度控制在160-210℃之间;
步骤五、采用LISIM同步拉伸法,将各层挤出、急冷铸片,经60-80℃热蒸槽调湿、清洁表面,用热风清除铸片表面蒸分后,然后进行双向拉伸,拉伸温度为160-190℃,定型温度为180-210℃,拉伸倍率为3.0*3.0-3.8*3.8,即得到抗菌高阻隔共挤复合膜。
本技术方案与背景技术相比,它具有如下优点:
1.本发明采用的纳米片层MMT可以提高薄膜的阻隔性能,降低水分子对EVOH层的影响,提高共挤复合薄膜的对温、湿度的适应能力;同时纳米氢氧化镁中的镁离子,在高温高湿条件下可转移到EVOH中,并与EVOH中的羟基发生离子结合,提高薄膜的阻隔性能;
2.本发明的抗菌阻燃共聚聚酰胺层以共聚聚酰胺作为载体:①降低MMT与氢氧化镁无卤阻燃对薄膜柔韧性的影响;②降低加工温度,防止抗菌性在高温(210℃以上)开始分解导致抗菌性能降低;
3.本发明采用载锌蒙脱土复合抗菌剂,具备高效、光谱、长效的抗菌性能;季铵盐离子和锌离子交替插层在MMT中,不易发生转移,满足食品包装要求;
4.本发明复合膜在高湿条件下仍能保持良好的阻隔性,同时兼具抗菌性和阻燃性,在各领域中具有很强的适配性和利用效果。
附图说明
图1为实施例1抗菌高阻隔共挤复合膜的层结构图。
其中,10-聚酰胺上表层,20-抗菌阻燃共聚聚酰胺层,30-EVOH阻隔层,40-阻燃共聚酰胺层,50-聚酰胺下表层。
具体实施方式
术语“上”、“下”为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。
下述实施例中使用的载锌蒙脱土复合抗菌剂的制备方法为:
步骤a、先将钠基蒙脱土添加到去离子水中,用搅拌机搅拌均匀,得到3%的钠基蒙脱土悬浮液;
步骤b、往钠基蒙脱土悬浮液中添加50mmol的硝酸锌在50℃条件下恒温搅拌3h,得到载锌蒙脱土悬浮液;
步骤C、往得到的载锌蒙脱土悬浮液中继续添加60mmol季铵盐,在50℃条件下恒温搅拌3h,抽滤,得到白色沉淀物;
步骤d、将白色沉淀物在80℃下干燥24h,研磨,过400筛,即得到载锌蒙脱土复合抗菌剂。
实施例中其余未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件或者按照产品说明书进行,所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规产品。
实施例1
本实施例一种抗菌高阻隔共挤复合膜,包括5层结构,由上至下依次为聚酰胺上表层、抗菌阻燃共聚聚酰胺层、EVOH阻隔层、阻燃聚酰胺层、聚酰胺下表层;其中,
所述聚酰胺上表层、聚酰胺下表层的厚度为1.5μm,其组份按照质量百分比包括:PA6 99%、二氧化硅0.5%、芥酸酰胺0.5%;
所述抗菌阻燃共聚聚酰胺层的厚度为4μm,其组份按照质量百分比包括:PA6/PA66/PA12共聚物75%、载锌蒙脱土复合抗菌剂5%、纳米氢氧化镁20%;
所述EVOH阻隔层的厚度为4μm,组份按照质量百分比包括:聚乙烯-乙烯醇共挤物100%;
所述阻燃聚酰胺层的厚度为4μm,组份按照质量百分比包括:PA6 93%、有机蒙脱土5%、氨基硅油2%。
本实施例抗菌高阻隔共挤复合膜的制备方法为:
步骤一、将聚酰胺上表层、聚酰胺下表层中的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的表层母粒烘干,备用;
步骤二、将抗菌阻燃共聚聚酰胺层中的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的抗菌母粒烘干,备用;
步骤三、将阻燃聚酰胺层中的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的阻燃母粒烘干,备用;
步骤四、将步骤一中得到的表层母粒分别投入10挤出机和50挤出机,制作聚酰胺上表层、聚酰胺下表层;将步骤二和步骤三得到的母料分别投入20挤出机和40挤出机,制作抗菌阻燃共聚聚酰胺层和阻燃聚酰胺层;将EVOH投入30挤出机,制作EVOH阻隔层;其中聚酰胺上表层、聚酰胺下表层和阻燃聚酰胺层的挤出机温度及其T型模头的温度控制在220-240℃之间,抗菌阻燃共聚聚酰胺层和EVOH阻隔层的挤出机温度及其T型模头的温度控制在160-210℃之间;
步骤五、采用LISIM同步拉伸法,将步骤三中各层挤出、急冷铸片,经60-80℃热蒸槽调湿、清洁表面,用热风清除铸片表面蒸分后,然后进行双向拉伸,拉伸温度为160-190℃,定型温度为180-210℃,拉伸倍率为3.0*3.0-3.8*3.8,即得到抗菌高阻隔共挤复合膜。
实施例2
实施例2与实施例1的区别在于:
所述聚酰胺表层的厚度为1.5μm,其组份按照质量百分比包括:PA6 99.8%、二氧化硅0.1%、芥酸酰胺0.1%;
所述抗菌阻燃共聚聚酰胺层的厚度为4μm,其组份按照质量百分比包括:PA6/PA66/PA12共聚物83%、载锌蒙脱土复合抗菌剂3%、纳米氢氧化镁15%;
所述EVOH阻隔层的厚度为4μm,组份按照质量百分比包括:聚乙烯-乙烯醇共挤物100%;
所述阻燃聚酰胺层的厚度为4μm,组份按照质量百分比包括:PA6 96%、有机蒙脱土3%、氨基硅油1%。
实施例3
实施例3与实施例1的区别在于:
所述聚酰胺表层的厚度为1.5μm,其组份按照质量百分比包括:PA6 98%、二氧化硅1%、芥酸酰胺1%;
所述抗菌阻燃共聚聚酰胺层的厚度为4μm,其组份按照质量百分比包括:PA6/PA66/PA12共聚物62%、载锌蒙脱土复合抗菌剂8%、纳米氢氧化镁30%;
所述EVOH阻隔层的厚度为4μm,组份按照质量百分比包括:聚乙烯-乙烯醇共挤物100%;
所述阻燃聚酰胺层的厚度为4μm,组份按照质量百分比包括:PA6 89%、有机蒙脱土8%、氨基硅油3%。
对比例1
市售15μm双向拉伸尼龙薄膜。
对比例2
市售15μm双向拉伸EVOH/尼龙共挤薄膜。
将实施例和对比例所制得的薄膜进行性能测试,拉伸性能:按GB/T1040.3-2006标准测试;垂直燃烧:按ANSL-UL94-2009标准测试;抗菌性能:按《GB/T 31402-2015塑料、塑料表面抗菌性能试验方法》测试。其测试评价结果如表1所示:
表1
由表1可以中的实施1-3与对比例1-2可以看出,制备的抗菌高阻隔共挤复合薄膜抗菌性能和阻燃性能优异,高湿条件下阻隔性好。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (10)
1.一种抗菌高阻隔共挤复合膜,其特征在于:由上至下依次设置为聚酰胺上表层、抗菌阻燃共聚聚酰胺层、EVOH阻隔层、阻燃聚酰胺层和聚酰胺下表层;其中,
所述抗菌阻燃共聚聚酰胺层按照质量百分比由共聚聚酰胺62-82%、载锌蒙脱土复合抗菌剂3-8%和纳米氢氧化镁15-30%组成;
所述EVOH阻隔层为聚乙烯-乙烯醇共挤物;
所述阻燃聚酰胺层按照质量百分比由聚酰胺91-96%、有机蒙脱土3-6%和氨基硅油1-3%组成。
2.根据权利要求1所述的一种抗菌高阻隔共挤复合膜,其特征在于:所述载锌蒙脱土复合抗菌剂,按照如下步骤制备而成:
步骤a、将钠基蒙脱土添加到去离子水中,用搅拌机搅拌均匀,得到2-5wt%的钠基蒙脱土悬浮液;
步骤b、往钠基蒙脱土悬浮液中添加30-60mmol的硝酸锌在40-60℃条件下恒温搅拌2-4h,得到载锌蒙脱土悬浮液;
步骤C、往载锌蒙脱土悬浮液中继续添加40-80mmol季铵盐,在40-60℃条件下恒温搅拌2-4h,抽滤,得到白色沉淀物;
步骤d、将白色沉淀物在80℃下干燥24h,研磨,过400筛,即得到载锌蒙脱土复合抗菌剂。
3.根据权利要求1所述的一种抗菌高阻隔共挤复合膜,其特征在于:所述聚酰胺上表层和聚酰胺下表层按照质量百分比由聚酰胺98-99.8%、开口剂0.1-1%和爽滑剂0.1-1%组成。
4.根据权利要求3所述的一种抗菌高阻隔共挤复合膜,其特征在于:所述聚酰胺为尼龙6、尼龙46、尼龙56、尼龙66、尼龙610、尼龙612、尼龙1010、尼龙1212的至少一种。
5.根据权利要求3所述的一种抗菌高阻隔共挤复合膜,其特征在于:所述开口剂为二氧化硅、碳酸钙、磷石膏粉、空心玻璃微珠、亚克力、PS交联颗粒、有机硅交联颗粒的至少一种。
6.根据权利要求3所述的一种抗菌高阻隔共挤复合膜,其特征在于:所述爽滑剂为酰胺类爽滑剂、蜡类爽滑剂、硅酮类爽滑剂的至少一种。
7.根据权利要求1所述的一种抗菌高阻隔共挤复合膜,其特征在于:所述共聚聚酰胺的熔点为160-190℃。
8.根据权利要求1所述的一种抗菌高阻隔共挤复合膜,其特征在于:所述共聚聚酰胺由尼龙6、尼龙66、尼龙11、尼龙12、尼龙1010、尼龙1212中的至少两种单体共聚而成。
9.根据权利要求1所述的一种抗菌高阻隔共挤复合膜,其特征在于:复合膜的总厚度为15-25μm,所述聚酰胺上表层和聚酰胺下表层的厚度均为1-2μm,所述EVOH阻隔层的厚度为3-5μm。
10.如权利要求1~9任一项所述一种抗菌高阻隔共挤复合膜的制备方法,其特征在于:包括如下步骤:
步骤一、将聚酰胺上表层、聚酰胺下表层的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的表层母粒烘干,备用;
步骤二、将抗菌阻燃共聚聚酰胺层中的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的抗菌母粒烘干,备用;
步骤三、将阻燃聚酰胺层中的组分按比例掺混,经双螺杆挤出机熔融共混、挤出、造粒,将得到的阻燃母粒烘干,备用;
步骤四、将上述表层母粒、抗菌母粒、阻燃母粒分别投入挤出机,分别制备得到聚酰胺上表层和聚酰胺下表层、抗菌阻燃共聚聚酰胺层、阻燃聚酰胺层;制备聚乙烯-乙烯醇共挤物的EVOH阻隔层;其中,聚酰胺上表层和聚酰胺下表层、阻燃聚酰胺层的挤出机温度及其T型模头的温度控制在220-240℃之间,抗菌阻燃共聚聚酰胺层和EVOH阻隔层的挤出机温度及其T型模头的温度控制在160-210℃之间;
步骤五、采用LISIM同步拉伸法,将各层挤出、急冷铸片,经60-80℃热蒸槽调湿、清洁表面,用热风清除铸片表面蒸分后,然后进行双向拉伸,拉伸温度为160-190℃,定型温度为180-210℃,拉伸倍率为3.0*3.0-3.8*3.8,即得到抗菌高阻隔共挤复合膜。
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