CN115091831B - 阻隔瓶及其制备方法 - Google Patents
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Abstract
本发明属于阻隔瓶制备技术领域,具体的涉及一种阻隔瓶及其制备方法。所述的阻隔瓶为五层共挤瓶,最外层和最内侧为基础树脂层,中间层为阻隔树脂层,基础树脂层和阻隔树脂层之间为胶黏剂层。其中:所述的阻隔树脂层,以质量份数计,原料组成如下:乙烯‑乙烯醇共聚物15‑18份、聚羟基乙酸35‑38份、聚萘二甲酸乙二醇酯40‑45份、乙烯‑甲基丙烯酸共聚物5‑8份、改性微晶纤维素1.5‑2.0份。本发明所述的阻隔瓶不仅实现了对气体和水汽的阻隔,还实现了对有机溶剂的阻隔,大大延长了阻隔瓶的使用寿命。
Description
技术领域
本发明属于阻隔瓶制备技术领域,具体的涉及一种阻隔瓶及其制备方法。
背景技术
产品在贮存、运输等流通过程中常会受到各种不利因素的破坏和影响,采用合理的包装可使产品免受或减少这些影响。通过阻隔材料包装产品可实现对包装内气体成分及含量的控制,从而有效地延长产品的保质期,因此阻隔材料成为重要的功能包装材料之一。阻隔瓶主要是在普通的塑料瓶中加入阻隔性树脂,从而广泛地应用于医药、食品与化工等高要求的特殊包装行业。
单纯的PE、PET、PP等单层阻隔瓶存在诸多缺陷:PE以及PP单层阻隔瓶对于乳油农药不适用,乳油农药中的有机溶剂会通过塑料瓶壁分子间隙渗透逃逸;PET单层阻隔瓶存在不耐碱性和酚类物质的缺陷,从而导致单层阻隔瓶阻隔性能欠佳,使其在气密性要求高的领域使用受到极大地限制,所以多层共挤阻隔瓶的发展日益受到重视。在多层共挤阻隔瓶领域中,为了增强对氧气、水汽的阻隔能力,目前,常对阻隔瓶的内外层进行化学物理处理,涂覆致密的阻隔层。然而,上述处理往往工艺精密复杂,成本高昂,不易大规模工业化应用。因此,有必要探索一种新型的阻隔瓶制备工艺,使得制备的阻隔瓶无需在成型后再经过物理或化学处理涂覆致密阻隔层。
发明内容
本发明的目的是:提供一种阻隔瓶。所述的阻隔瓶不仅能够对气体和水汽具有阻隔作用,还实现了对有机溶剂的阻隔;本发明同时提供了其制备方法。
本发明所述的阻隔瓶为五层共挤瓶,最外层和最内侧为基础树脂层,中间层为阻隔树脂层,基础树脂层和阻隔树脂层之间为胶黏剂层;其中:所述的阻隔树脂层,以质量份数计,原料组成如下:
乙烯-乙烯醇共聚物15-18份
聚羟基乙酸 35-38份
聚萘二甲酸乙二醇酯40-45份
乙烯-甲基丙烯酸共聚物5-8份
改性微晶纤维素 1.5-2.0份。
其中:
所述的改性微晶纤维素的制备方法为:将硅烷偶联剂KH550与乙醇溶液混合均匀,然后加入微晶纤维素进行搅拌反应,反应完毕后静置沉淀去除上清液;对沉淀物进行离心处理,最后将沉淀物进行干燥固化,制备得到改性微晶纤维素。
乙醇溶液的质量浓度为70%;搅拌反应的温度为63-65℃,搅拌反应时间为2.2-2.5h;干燥固化的温度为100-102℃,时间为10-13min;硅烷偶联剂KH550与微晶纤维素的质量比为4-4.5:1。
所述的阻隔树脂层,将乙烯-乙烯醇共聚物、聚羟基乙酸和聚萘二甲酸乙二醇酯复配使用;其中,由于乙烯-乙烯醇共聚物分子结构中存在羟基,因此,在乙烯-乙烯醇共聚物体系中存在着相邻羟基间的分子内和分子间氢键的相互作用,粘聚力较强,分子链堆积紧密,小分子不能透过,它既可以有效的阻止氧气、二氧化碳、氮气等气体的渗透,还对非极性的油类、有机溶剂也有极好的阻隔性能;但是乙烯-乙烯醇共聚物脆性大、耐冲击性能较差且具有吸湿性。复配聚萘二甲酸乙二醇酯(PEN)使用,增加其性能稳定性,不仅对有机溶剂和化学药品稳定,且具有很好的气密性、耐酸碱性和耐热性,其阻隔性能不受环境湿度的影响,增加了制备的阻隔瓶的力学性能。聚羟基乙酸对二氧化碳和氧气的阻隔性能优异,不溶于丙酮、二氯甲烷、氯仿、四氢呋喃等有机溶剂,且其自身具有很好的机械性能和生物相容性。在阻隔树脂层中创造性的添加改性微晶纤维素,通过改性微晶纤维素的添加,对聚萘二甲酸乙二醇酯进行改性处理,提高阻隔树脂层的耐水性。
所述的基础树脂层,以质量份数计,原料组成如下:
高密度聚乙烯60-65份
聚丙烯15-20份
聚碳酸亚丙酯2-3份
聚甲基丙烯酸甲酯5-7份
乙烯-丙烯酸共聚物6-8份。
其中:基础树脂层中,选用高密度聚乙烯和聚丙烯为基体树脂,高密度聚乙烯具有很好的化学稳定性、耐热性、耐寒性、抗老化性能和韧性,但是其刚性和强度较差,因此,复配聚丙烯使用来提高基础树脂层的强度;且高密度聚乙烯和聚丙烯自身均具有很好的耐溶剂性和耐湿性,使得基础树脂层能够起到很好的阻湿性能;添加少量的聚碳酸亚丙酯和聚甲基丙烯酸甲酯是因为聚碳酸亚丙酯由于酯键的存在对有机溶剂具有很好的阻隔性,而聚甲基丙烯酸甲酯的添加则大大提高了基础树脂层的疏水性;将聚甲基丙烯酸甲酯和聚碳酸亚丙酯作为分散相分散在高密度聚乙烯和聚丙烯基体树脂中,形成阻隔带,通过增加小分子经过材料的曲折路径,从而进一步提高其阻隔性能;将乙烯-丙烯酸共聚物作为相容剂,一方面,乙烯-丙烯酸共聚物分子链中的羧基能够与聚碳酸亚丙酯和聚甲基丙烯酸甲酯分子链中的酯基形成氢键;另外一方面,由于乙烯-丙烯酸共聚物的分子主链是非极性,因此与高密度聚乙烯和聚丙烯本身就具有很好的相容性;综上所述,所述的基础树脂层中,各个原料之间相互配合,使得基础树脂层具有很好的疏水性能。
所述的胶黏剂层,以质量份数计,原料组成如下:
线性低密度聚乙烯23-25份
马来酸酐接枝聚乙烯 16-18份
乙烯-丙烯酸酯-马来酸酐三元共聚物23-28份
磺化三元乙丙橡胶10-13份。
其中:
所述的胶黏剂层中,乙烯-丙烯酸酯-马来酸酐三元共聚物(EMH粘结树脂)的热稳定性能优异且兼容性好;磺化三元乙丙橡胶(SEPDM)除了具有优良的粘结性能外,还具有很好的耐介质、耐水性能和耐候性,此外,磺化三元乙丙橡胶对醇和氧化剂也有很好的抗耐性;线性低密度聚乙烯自身具有很好的抗冲击强度、抗穿刺性、拉伸强度和耐环境应力开裂性;马来酸酐接枝聚乙烯不仅起到相容剂的作用,它自身还是一种粘合树脂。所述的胶黏剂层不仅具有很好的粘合性,还具有对氧气、水汽和溶剂的阻隔性能以及很好的机械性能;且所述的胶黏剂层中的粘合树脂在高温下能与基础树脂层和阻隔树脂层中树脂的相应的基团发生化学反应,通过化学键形成牢固的粘结。由此可知,所述的胶黏剂层不仅对基础树脂层和阻隔树脂层均具有很好的粘结性能,还具有耐水性、耐介质性以及对氧气的阻隔性能。
本发明所述的阻隔瓶的制备方法,由以下步骤组成:
(1)将基础树脂层用到的原料高密度聚乙烯、聚丙烯、聚碳酸亚丙酯、聚甲基丙烯酸甲酯和乙烯-丙烯酸共聚物按比例混合均匀;
(2)将胶黏剂层用到的原料线性低密度聚乙烯、马来酸酐接枝聚乙烯、乙烯-丙烯酸酯-马来酸酐三元共聚物和磺化三元乙丙橡胶按比例混合均匀;
(3)将阻隔树脂层用到的原料乙烯-乙烯醇共聚物、聚羟基乙酸、聚萘二甲酸乙二醇酯、乙烯-甲基丙烯酸共聚物和改性微晶纤维素按配比混合均匀;
(4)将步骤(1)-步骤(3)混合均匀的各层原料放入相应的挤出机中,通过五层共挤吹塑成型工艺制备得到包含基础树脂层、胶黏剂层、阻隔树脂层、胶黏剂层和基础树脂层的阻隔瓶。
其中:
在步骤(4)中挤出时,步骤(1)中混合均匀的原料的挤出温度为180-185℃;步骤(2)中混合均匀的原料的挤出温度为200-210℃;步骤(3)中混合均匀的原料的挤出温度为250-255℃。
本发明与现有技术相比,具有以下有益效果:
(1)本发明所述的阻隔瓶,基础树脂层具有很好的阻湿性能,胶黏剂层不仅对基础树脂层和阻隔树脂层均具有很好的粘结性能,其自身还具有耐水性、耐介质性以及对氧气的阻隔性能,阻隔树脂层不仅具有很好的机械性能,还具有对氧气、二氧化碳、氮气等气体的阻隔性以及对有机溶剂也具有很好的阻隔性,此外,经过改性处理大大提高了阻隔树脂层的疏水性;由此可知,由基础树脂层、胶黏剂层和阻隔树脂层共挤得到的阻隔瓶不仅实现了对气体和水汽的阻隔,还实现了对有机溶剂的阻隔,大大延长了阻隔瓶的使用寿命。
(2)本发明所述的阻隔瓶的制备方法,制备工艺简单,参数易于控制,制备的阻隔瓶的阻隔性能优异。
具体实施方式
以下结合实施例对本发明作进一步描述。
实施例1
本实施例1所述的阻隔瓶为五层共挤瓶,最外层和最内侧为基础树脂层,中间层为阻隔树脂层,基础树脂层和阻隔树脂层之间为胶黏剂层;其中:所述的阻隔树脂层,以质量份数计,原料组成如下:
乙烯-乙烯醇共聚物17份
聚羟基乙酸 36份
聚萘二甲酸乙二醇酯43份
乙烯-甲基丙烯酸共聚物 7份
改性微晶纤维素1.8份。
其中:
所述的改性微晶纤维素的制备方法为:将硅烷偶联剂KH550与乙醇溶液混合均匀,然后加入微晶纤维素进行搅拌反应,反应完毕后静置沉淀去除上清液;对沉淀物进行离心处理,最后将沉淀物进行干燥固化,制备得到改性微晶纤维素。
其中:乙醇溶液的质量浓度为70%;搅拌反应的温度为64℃,搅拌反应时间为2.3h;干燥固化的温度为101℃,时间为12min;硅烷偶联剂KH550与微晶纤维素的质量比为4.5:1。
所述的基础树脂层,以质量份数计,原料组成如下:
高密度聚乙烯60份
聚丙烯20份
聚碳酸亚丙酯2.5份
聚甲基丙烯酸甲酯6份
乙烯-丙烯酸共聚物7份。
所述的胶黏剂层,以质量份数计,原料组成如下:
线性低密度聚乙烯24份
马来酸酐接枝聚乙烯 17份
乙烯-丙烯酸酯-马来酸酐三元共聚物23份
磺化三元乙丙橡胶 13份。
本实施例1所述的阻隔瓶的制备方法,由以下步骤组成:
(1)将基础树脂层用到的原料高密度聚乙烯、聚丙烯、聚碳酸亚丙酯、聚甲基丙烯酸甲酯和乙烯-丙烯酸共聚物按比例混合均匀;
(2)将胶黏剂层用到的原料线性低密度聚乙烯、马来酸酐接枝聚乙烯、乙烯-丙烯酸酯-马来酸酐三元共聚物和磺化三元乙丙橡胶按比例混合均匀;
(3)将阻隔树脂层用到的原料乙烯-乙烯醇共聚物、聚羟基乙酸、聚萘二甲酸乙二醇酯、乙烯-甲基丙烯酸共聚物和改性微晶纤维素按配比混合均匀;
(4)将步骤(1)-步骤(3)混合均匀的各层原料放入相应的挤出机中,通过五层共挤吹塑成型工艺制备得到包含基础树脂层、胶黏剂层、阻隔树脂层、胶黏剂层和基础树脂层的阻隔瓶。
其中:
在步骤(4)中挤出时,步骤(1)中混合均匀的原料的挤出温度为183℃;步骤(2)中混合均匀的原料的挤出温度为210℃;步骤(3)中混合均匀的原料的挤出温度为253℃。
实施例2
本实施例2所述的阻隔瓶为五层共挤瓶,最外层和最内侧为基础树脂层,中间层为阻隔树脂层,基础树脂层和阻隔树脂层之间为胶黏剂层;其中:所述的阻隔树脂层,以质量份数计,原料组成如下:
乙烯-乙烯醇共聚物15份
聚羟基乙酸 38份
聚萘二甲酸乙二醇酯40份
乙烯-甲基丙烯酸共聚物 5份
改性微晶纤维素1.5份。
其中:
所述的改性微晶纤维素的制备方法为:将硅烷偶联剂KH550与乙醇溶液混合均匀,然后加入微晶纤维素进行搅拌反应,反应完毕后静置沉淀去除上清液;对沉淀物进行离心处理,最后将沉淀物进行干燥固化,制备得到改性微晶纤维素。
乙醇溶液的质量浓度为70%;搅拌反应的温度为63℃,搅拌反应时间为2.2h;干燥固化的温度为100℃,时间为10min;硅烷偶联剂KH550与微晶纤维素的质量比为4.3:1。
所述的基础树脂层,以质量份数计,原料组成如下:
高密度聚乙烯63份
聚丙烯 15份
聚碳酸亚丙酯3份
聚甲基丙烯酸甲酯7份
乙烯-丙烯酸共聚物8份。
所述的胶黏剂层,以质量份数计,原料组成如下:
线性低密度聚乙烯 23份
马来酸酐接枝聚乙烯 16份
乙烯-丙烯酸酯-马来酸酐三元共聚物 25份
磺化三元乙丙橡胶 12份。
本实施例2所述的阻隔瓶的制备方法,由以下步骤组成:
(1)将基础树脂层用到的原料高密度聚乙烯、聚丙烯、聚碳酸亚丙酯、聚甲基丙烯酸甲酯和乙烯-丙烯酸共聚物按比例混合均匀;
(2)将胶黏剂层用到的原料线性低密度聚乙烯、马来酸酐接枝聚乙烯、乙烯-丙烯酸酯-马来酸酐三元共聚物和磺化三元乙丙橡胶按比例混合均匀;
(3)将阻隔树脂层用到的原料乙烯-乙烯醇共聚物、聚羟基乙酸、聚萘二甲酸乙二醇酯、乙烯-甲基丙烯酸共聚物和改性微晶纤维素按配比混合均匀;
(4)将步骤(1)-步骤(3)混合均匀的各层原料放入相应的挤出机中,通过五层共挤吹塑成型工艺制备得到包含基础树脂层、胶黏剂层、阻隔树脂层、胶黏剂层和基础树脂层的阻隔瓶。
其中:
在步骤(4)中挤出时,步骤(1)中混合均匀的原料的挤出温度为185℃;步骤(2)中混合均匀的原料的挤出温度为200℃;步骤(3)中混合均匀的原料的挤出温度为250℃。
实施例3
本实施例3所述的阻隔瓶为五层共挤瓶,最外层和最内侧为基础树脂层,中间层为阻隔树脂层,基础树脂层和阻隔树脂层之间为胶黏剂层;其中:所述的阻隔树脂层,以质量份数计,原料组成如下:
乙烯-乙烯醇共聚物18份
聚羟基乙酸 35份
聚萘二甲酸乙二醇酯45份
乙烯-甲基丙烯酸共聚物8份
改性微晶纤维素2.0份。
其中:
所述的改性微晶纤维素的制备方法为:将硅烷偶联剂KH550与乙醇溶液混合均匀,然后加入微晶纤维素进行搅拌反应,反应完毕后静置沉淀去除上清液;对沉淀物进行离心处理,最后将沉淀物进行干燥固化,制备得到改性微晶纤维素。
乙醇溶液的质量浓度为70%;搅拌反应的温度为65℃,搅拌反应时间为2.5h;干燥固化的温度为102℃,时间为13min;硅烷偶联剂KH550与微晶纤维素的质量比为4:1。
所述的基础树脂层,以质量份数计,原料组成如下:
高密度聚乙烯65份
聚丙烯 17份
聚碳酸亚丙酯2份
聚甲基丙烯酸甲酯5份
乙烯-丙烯酸共聚物6份。
所述的胶黏剂层,以质量份数计,原料组成如下:
线性低密度聚乙烯25份
马来酸酐接枝聚乙烯 18份
乙烯-丙烯酸酯-马来酸酐三元共聚物 28份
磺化三元乙丙橡胶 10份。
本实施例3所述的阻隔瓶的制备方法,由以下步骤组成:
(1)将基础树脂层用到的原料高密度聚乙烯、聚丙烯、聚碳酸亚丙酯、聚甲基丙烯酸甲酯和乙烯-丙烯酸共聚物按比例混合均匀;
(2)将胶黏剂层用到的原料线性低密度聚乙烯、马来酸酐接枝聚乙烯、乙烯-丙烯酸酯-马来酸酐三元共聚物和磺化三元乙丙橡胶按比例混合均匀;
(3)将阻隔树脂层用到的原料乙烯-乙烯醇共聚物、聚羟基乙酸、聚萘二甲酸乙二醇酯、乙烯-甲基丙烯酸共聚物和改性微晶纤维素按配比混合均匀;
(4)将步骤(1)-步骤(3)混合均匀的各层原料放入相应的挤出机中,通过五层共挤吹塑成型工艺制备得到包含基础树脂层、胶黏剂层、阻隔树脂层、胶黏剂层和基础树脂层的阻隔瓶。
其中:
在步骤(4)中挤出时,步骤(1)中混合均匀的原料的挤出温度为180℃;步骤(2)中混合均匀的原料的挤出温度为205℃;步骤(3)中混合均匀的原料的挤出温度为255℃。
对比例1
本对比例1所述的阻隔瓶为五层共挤瓶,与实施例3所述的阻隔瓶的结构和制备方法相同,且基础树脂层和胶黏剂层的原料组成也相同,唯一的不同点在于,阻隔树脂层的原料组成不同:
所述的阻隔树脂层,以质量份数计,原料组成如下:
聚羟基乙酸35份
聚萘二甲酸乙二醇酯45份。
对比例2
本对比例2所述的阻隔瓶为五层共挤瓶,与实施例3所述的阻隔瓶的结构和制备方法相同,且阻隔树脂层和胶黏剂层的原料组成也相同,唯一的不同点在于,基础树脂层的原料组成不同:
所述的基础树脂层,以质量份数计,原料组成如下:
高密度聚乙烯65份
聚丙烯 17份
聚碳酸亚丙酯2份
乙烯-丙烯酸共聚物6份。
对比例3
本对比例3所述的阻隔瓶为五层共挤瓶,与实施例3所述的阻隔瓶的结构和制备方法相同,且阻隔树脂层和基础树脂层的原料组成也相同,唯一的不同点在于,胶黏剂层的原料组成不同:
所述的胶黏剂层,以质量份数计,原料组成如下:
线性低密度聚乙烯25份
马来酸酐接枝聚乙烯 18份
乙烯-丙烯酸酯-马来酸酐三元共聚物 28份。
对实施例1-3以及对比例1-3制备的阻隔瓶进行性能测试,结果如下表1所示:
表1 阻隔瓶测试结果
Claims (7)
1.一种阻隔瓶,其特征在于:阻隔瓶为五层共挤瓶,最外层和最内侧为基础树脂层,中间层为阻隔树脂层,基础树脂层和阻隔树脂层之间为胶黏剂层;其中:所述的阻隔树脂层,以质量份数计,原料组成如下:
乙烯-乙烯醇共聚物 15-18份
聚羟基乙酸 35-38份
聚萘二甲酸乙二醇酯 40-45份
乙烯-甲基丙烯酸共聚物 5-8份
改性微晶纤维素 1.5-2.0份;
所述的基础树脂层,以质量份数计,原料组成如下:
高密度聚乙烯 60-65份
聚丙烯 15-20份
聚碳酸亚丙酯 2-3份
聚甲基丙烯酸甲酯 5-7份
乙烯-丙烯酸共聚物 6-8份;
所述的胶黏剂层,以质量份数计,原料组成如下:
线性低密度聚乙烯 23-25份
马来酸酐接枝聚乙烯 16-18份
乙烯-丙烯酸酯-马来酸酐三元共聚物 23-28份
磺化三元乙丙橡胶 10-13份;
改性微晶纤维素的制备方法为:将硅烷偶联剂KH550与乙醇溶液混合均匀,然后加入微晶纤维素进行搅拌反应,反应完毕后静置沉淀去除上清液;对沉淀物进行离心处理,最后将沉淀物进行干燥固化,制备得到改性微晶纤维素。
2.根据权利要求1所述的阻隔瓶,其特征在于:乙醇溶液的质量浓度为70%;搅拌反应的温度为63-65℃,搅拌反应时间为2.2-2.5h。
3.根据权利要求1所述的阻隔瓶,其特征在于:干燥固化的温度为100-102℃,时间为10-13min;硅烷偶联剂KH550与微晶纤维素的质量比为4-4.5:1。
4.一种权利要求1所述的阻隔瓶的制备方法,其特征在于:由以下步骤组成:
(1)将基础树脂层用到的原料高密度聚乙烯、聚丙烯、聚碳酸亚丙酯、聚甲基丙烯酸甲酯和乙烯-丙烯酸共聚物按比例混合均匀;
(2)将胶黏剂层用到的原料线性低密度聚乙烯、马来酸酐接枝聚乙烯、乙烯-丙烯酸酯-马来酸酐三元共聚物和磺化三元乙丙橡胶按比例混合均匀;
(3)将阻隔树脂层用到的原料乙烯-乙烯醇共聚物、聚羟基乙酸、聚萘二甲酸乙二醇酯、乙烯-甲基丙烯酸共聚物和改性微晶纤维素按配比混合均匀;
(4)将步骤(1)-步骤(3)混合均匀的各层原料放入相应的挤出机中,通过五层共挤吹塑成型工艺制备得到包含基础树脂层、胶黏剂层、阻隔树脂层、胶黏剂层和基础树脂层的阻隔瓶。
5.根据权利要求4所述的阻隔瓶的制备方法,其特征在于:在步骤(4)中挤出时,步骤(1)中混合均匀的原料的挤出温度为180-185℃。
6.根据权利要求4所述的阻隔瓶的制备方法,其特征在于:在步骤(4)中挤出时,步骤(2)中混合均匀的原料的挤出温度为200-210℃。
7.根据权利要求4所述的阻隔瓶的制备方法,其特征在于:在步骤(4)中挤出时,步骤(3)中混合均匀的原料的挤出温度为250-255℃。
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