CN110028770A - 一种可全降解的复合膜及其制备方法 - Google Patents
一种可全降解的复合膜及其制备方法 Download PDFInfo
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- CN110028770A CN110028770A CN201910351156.7A CN201910351156A CN110028770A CN 110028770 A CN110028770 A CN 110028770A CN 201910351156 A CN201910351156 A CN 201910351156A CN 110028770 A CN110028770 A CN 110028770A
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Abstract
本发明公开了一种可全降解的复合膜,由包括以下重量份数组分制成:聚乙醇酸、聚羟基丁酸酯、聚(L‑丙交酯‑ε‑己内酯)、脂肪酸甘油酯、爽滑剂、阻水剂、增强纤维、滑石粉、季戊四醇二亚磷酸酯、壳聚糖和淀粉等材料制成。本发明还提供所述可全降解的复合膜的制备方法。本发明具有以下优点:具有良好的微生物降解性和水解性,完全生物降解材料分解后的最终形态是水和二氧化碳,对环境无污染;安全无毒,对动物及人体不存在潜在健康威胁;具有良好力学性能,充分满足包装材料的各种应用需求;在不影响力学性能的情况下,增加廉价且无环境污染的填料,有效的降低成本;制备工艺简单。
Description
技术领域
本发明涉及医疗和包装材料领域,具体为一种成本低、韧性好且制备简单的可全降解的复合膜及其制备方法。
背景技术
塑料包装袋已经成为日常生活中的必需品,使用量大且废弃量同样也巨大。塑料包装袋多以聚乙烯薄膜或聚氯乙烯辅佐一些改善性能的添加剂制成,其对人体可能存在损害外,最关键的是自然降解慢,且因为使用量巨大,回收利用少,废弃的塑料包装袋往往形成越来越严重“白色污染”。“白色污染”不仅给生活造成视觉污染,还危及农业生产以及生态循环等方面。
随着塑料产量不断增长,用途不断扩大,其废弃物也日益增多。由于塑料用后在自然环境中难以降解、腐烂,产生严重的环境污染。由大量的废弃塑料袋引起的“白色垃圾”问题已成为“百年难题”,严重污染环境,影响人们的生活。难以降解的塑料混入土壤能够影响作物吸收水分和养分,导致农作物减产;就算填埋起来,也占用土地并且上百年才可以完全降解。大量散落的塑料材料还容易造成动物误食致死。废弃的塑料易成团成捆,它甚至能堵塞水流,造成水利设施、引起城市设施故障,酿成灾害。
可降解塑料可以避免了二次污染,作为高科技产品和环保产品正成为当今世界瞩目的研发热点,其发展不仅扩大了塑料的功能,而且一定程度上缓解了环境矛盾,对日益枯竭的石油资源是一个补充,因此可降解塑料的研究开发和推广应用适应了人类可持续发展的要求。
聚乙醇酸(PolyglycolicAcid,PGA)具有简单规整的线性分子结构,是简单的线性脂肪族聚酯,有较高的结晶度,形成结晶状聚合物,结晶度一般为40%~80%,熔点在225℃左右,不溶于常用的有机溶剂,只溶于像六氟代异丙醇这样的强极性有机溶剂。高分子量的聚乙醇酸是通过开环聚合得到的,分子量达10000以上的聚乙醇酸,其强度完全能满足可吸收缝合线的使用要求,但用在骨折或其它内固定物方面,强度还不够;当聚乙醇酸平均分子量达到20000~145000时,聚合物可以拉成纤维状,并且可以使聚合物的分子排列具有方向性,也增强了聚乙醇酸的强度,这样的聚乙醇酸能做成薄膜或其他不同的形状。聚乙醇酸的生物医学应用主要表现在医用缝合线、药物控释载体、骨折固定材料、组织工程支架、缝合补强材料。聚乙醇酸可以在动物和人体中,在活性酶的作用下分子链产生裂解、解聚、侧基分裂等,被快速降解为水和二氧化碳等无害,并可随体内的循环系统排出体外,对动物和人体无毒副作用。因此,在医学领域常常被用于制造手术缝;合线、人造皮肤等,可以大大减少术后并发症的出现。
申请公布号为CN101333330,申请号为200810041435.5的中国专利申请公开一种可完全生物降解的聚乳酸复合材料及其制备方法,该复合材料由经过表面改性的编织或未编织的天然纤维、聚乳酸和硅烷偶联剂组成。虽然该聚乳酸复合材料的力学性能和热性能均有所提高,且使用废弃后可在自然环境中完全降解,但是需要从农作物中提取,取材受到限制,成本也比较高。
申请公布号CN101792591A,申请号为CN200910214402.0的中国专利申请公开一种一种全生物降解塑料薄膜及其制备方法,该材料由以下按重量份数计的组分组成:聚碳酸亚乙酯聚氨酯20-90份、热塑性淀粉1-50份、相容改性5-10份、纳米无机增强成分3-5份、复合增塑成分2-20份和润滑成分10-30份。采用本发明制备的全生物降解塑料薄膜不仅具有优良的生物降解性能,具有良好的韧性,较高的抗撕裂强度。但是其具有一定的化学毒性,且稳定性差,不利于推广实用。
发明内容
本发明的目的是针对以上所述现有技术存在的不足,提供一种成本低、力学性能好、安全无毒且可以完全生物降解的可全降解的复合膜。
本发明的另一目的是提供成本低、工序简单的可全降解的复合膜的制备方法。
为了实现本发明目的,本发明采用的技术方案是:一种可全降解的复合膜,由包括以下重量份数组分制成:
所述聚乙醇酸可以是为平均粒径1-5mm的颗粒,特性粘数[η]为1~5g/dl,分子量为20-30万。
所述聚(L-丙交酯-ε-己内酯)(poly(L-lactide-co-ε-caprolactone),PLLCA)的重均分子量(Mw)为20-50万,聚(L-丙交酯-ε-己内酯)中ε-己内酯单元摩尔百分比为20%~25%,用于显著提高拉伸率和拉伸强度。
所述脂肪酸甘油酯用于提高薄膜的抗张强度和低温柔性,以满足薄膜的使用要求。
所述聚羟基丁酸酯的酸酯黏均分子量大于22万,保持了聚乙醇酸树脂的优异气体阻隔性,同时显著改善了树脂耐湿稳定性和热熔融加工性。
所述季戊四醇二亚磷酸酯可以选用山东省临沂市三丰化工有限公司的抗氧剂SONOX 627A,用于提高聚合物稳定性,特别是加工成型的热稳定性,减少产品提前降解状况,提高产品降解前的耐用性。
所述淀粉可以玉米淀粉、大豆淀粉、红薯淀粉、马铃薯淀粉中的一种或两种以上的组合,用于作为有机填料,降低成本,且可以生物降解,安全无毒。
所述阻水剂可以是动物类阻水剂或者植物类阻水剂,其中所述动物类阻水剂为蜂蜡、牛油、鲸油、羊毛蜡或者鲸蜡中的一种或两种以上的组合;所述植物类阻水剂为棕榈蜡、花生油、蓖麻蜡、棕榈酸、大豆油、环氧大豆油、杨梅蜡、霍霍巴油或者氢化植物油中的一种或两种以上的组合。原材料来自于常规动物或者是植物,可以生物降解,环保,对环境不产生影响;具有良好的水汽阻隔性和断裂强度,且透明性好。
所述爽滑剂可以是油酸酰胺、硬脂酰胺或者芥酸酰胺,用于减小薄膜表面的摩擦系数,从而确保良好的后续加工性,比如在包装机上的走机性能;爽滑剂由于带有极性基团,与聚乙醇酸不相容的脂肪酸酰胺会迁移到薄膜表层,固化结晶后形成平滑的表面从而降低薄膜的摩擦系数。
所述壳聚糖具有良好的生物相容性和可生物降解,降解产物无毒,可以提高抗菌,抗微生物性,延缓聚乙醇酸快速降解,提高产品耐用性。
所述增强纤维可以是木纤维、麻纤维、棉纤维、竹纤维等多种天然高分子植物纤维中的一种或者两种以上的组合,他们强度和刚度比较高并且比重小,且可以在自然环境中降解并且来源比较广泛,没有污染;具有良好抗弯强度低伸长率特性。
还可以添加1-5重量份数的增韧剂。所述增韧剂1-5可以是杜邦公司的DuPontBiomax Strong,用于提高PGA材料的韧性,降低其脆性;另外可以提高PGA材料的冲击强度和熔融稳定性,且对透明性影响最小。所述增韧剂也可以是复合增韧剂,所述复合增韧剂可以是纳米方解石、纳米滑石粉和亚纳米脂肪酸稀土盐按30~50∶10~20∶1~5重量份组配而成,优选按35~45∶13~18∶2~3重量份组配而成。
上述可全降解的复合膜的制备方法,其包括的步骤如下:
(1)将聚乙醇酸、聚羟基丁酸酯、聚(L-丙交酯-ε-己内酯)和季戊四醇二亚磷酸酯在低温超微粉碎机下粉碎,得到平均粒径60~80μm的颗粒,并混合均匀,形成混合主料;
(2)加入爽滑剂、阻水剂、增强纤维、滑石粉、壳聚糖和淀粉在低温超微粉碎机下研磨粉碎得到平均粒径60~80μm的颗粒,并混合均匀,形成混合辅料;
(3)将混合主料、混合辅料和脂肪酸甘油酯混合均匀,通过挤出机在温度为170-230℃下挤出,然后形成薄膜。
所述挤出机内导入超声波处理,所述超声波处理功率为300-800W,频率为50-150KHz,可以有效的将各种组分在超声波的作用下相互迁移,形成紧密结构,提升有韧性和强度,且透明效果更好。
优选的,超声波功率为550W,频率为110KHz,可以有效的进行声波震荡搅拌,同时可以避免声波过强导致空化作用而产生气泡。所述超声波可以是超声波产生装置通过贴壁式的固定在挤出机的外侧板内,通过侧壁向腔内物料传递超声波。
所述(3)步骤中,可以通过挤出成膜系统来形成薄膜。所述挤出成膜系统,包括挤出机、吹胀成型环模、导向板和夹棍,所述挤出机通过连接头与吹胀成型环模连接,所述吹胀成型环模成膜出口方向设置导向板,所述导向板出口端设置夹棍;在所述吹胀成型环模的成膜出口处设置用于冷却的气环。
所述气环为环绕在所述吹胀成型环模的成膜出口处的环状吹风管,其风口方向向下与成膜出口方向形成30-45度夹角。
所述挤出机包括加料斗、筒体、驱动装置和机座,所述筒体固定在机座上,所述加料斗安装在筒体的进料口处,所述筒体内设置螺杆,所述螺杆与固定在所述筒体一端的驱动装置连接;所述筒体另一端设置挤出口与连接头连接;在所述筒体外侧壁上均匀的排布若干超声波换能器。
与现有技术相比,本发明具有以下优点:具有良好的微生物降解性和水解性,在适当和可表明期限的自然环境条件下,能够被微生物(细菌、真菌和藻类等)完全分解变成低分子化合物,最后完全生物降解材料分解后的最终形态是水和二氧化碳,对环境无污染;安全无毒,对动物及人体不存在潜在健康威胁;具有良好力学性能,充分满足包装材料的各种应用需求;在不影响力学性能的情况下,增加廉价且无环境污染的填料,有效的降低成本;制备工艺简单,超声波的导入,提高了产品力学性能;安全无毒,能满足各种领域需求。
具体实施方式
以下结合具体实施例对本发明进行详细的说明。
一种可全降解的复合膜,优选的,由包括以下重量份数组分制成:
上述可全降解的复合膜的制备方法,其包括的步骤如下:
(1)将聚乙醇酸、聚羟基丁酸酯、聚(L-丙交酯-ε-己内酯)和季戊四醇二亚磷酸酯在低温超微粉碎机下粉碎,得到平均粒径60~80μm的颗粒,并混合均匀,形成混合主料;
(2)加入爽滑剂、阻水剂、增强纤维、滑石粉、壳聚糖和淀粉在低温超微粉碎机下研磨粉碎得到平均粒径60~80μm的颗粒,并混合均匀,形成混合辅料;
(3)将混合主料、混合辅料和脂肪酸甘油酯混合均匀,通过挤出机在温度为170-230℃下挤出,然后形成薄膜。所述膜厚度在30~200μm之间,厚度精度为±20μm。
所述挤出机内导入超声波处理,所述超声波处理功率为400-600W,频率为80-120KHz,可以有效的将各种组分在超声波的作用下相互迁移,形成紧密结构,提升有韧性和强度,且透明效果更好。
优选的,超声波功率为550W,频率为110KHz,可以有效的进行声波震荡搅拌,同时可以避免声波过强导致空化作用而产生气泡。所述超声波可以是超声波产生装置通过贴壁式的固定在挤出机的外侧板内,通过侧壁向腔内物料传递超声波。
所述(3)步骤中,可以通过挤出成膜系统来形成薄膜。所述挤出成膜系统,如图1所示,其包括挤出机14、吹胀成型环模12、导向板7、夹棍8和卷取装置11,所述挤出机14通过连接头13与吹胀成型环模12连接,所述吹胀成型环模12成膜出口方向设置导向板7,所述导向板7出口端设置夹棍8。吹胀成型环模12出来的增塑膜通过导向板7被拉伸后通过夹棍8形成初膜,然后通过导向棍9引导最少通过一套二级夹棍10后被卷取装置11卷成卷。在所述吹胀成型环模12的成膜出口处设置用于冷却的气环5。所述气环5为环绕在所述吹胀成型环模12成膜出口处的环状吹风管,其风口方向向下与成膜出口方向成30-45°夹角,所述气环5与冷却风管连接,风冷代替水冷,提高制膜稳定性。优选的,夹角为40°。所述挤出机14包括加料斗2,筒体4、驱动装置1和机座,所述筒体4固定在机座上,所述加料斗2安装在筒体4的进料口处,用于方便进料。所述筒体4内设置螺杆,优选设置双螺杆,所述螺杆与固定在所述筒体4一端的驱动装置1连接,螺杆由驱动装置1驱动。所述筒体4另一端设置挤出口与连接头13连接。所述筒体4上设置加热器,用于调节温度。在所述筒体4外侧壁上均匀的排布若干超声波换能器3。所述超声波换能器3可以为贴壁式超声波换能器或者钳式超声波换能器。所述贴壁式超声波换能器为超声波发生器以其超声辐照方向垂直于筒体4上中轴线并通过一适配前置附块装设于筒体4外壁上,超声波换能器向筒体4内辐照超声波。所述超声波换能器通过一适配前置附块与所述筒体4外壁紧牢地连接安装。所述钳式超声波处理器包括换能器组件和功能夹具,换能器组件包括换能器和变幅杆,换能器与变幅杆连接,最少一个换能器组件与功能夹具连接。功能夹具可以包括辐照前沿近杆块和辐照前沿托管块,辐照前沿近杆块和辐照前沿托管块内设置容纳接受超声辐照筒体4的功能夹具腔,辐照前沿近杆块连接将接受超声辐照罐管夹紧;辐照前沿近杆块和/或辐照前沿托管块与变幅杆通过接驳螺杆连接。超声波换能器可以是压电式或者磁致式的。换能器与变幅杆通过接驳螺杆将其组合而成的换能器组件,换能器通过导线与超声波发射电器连接,超声波发射电器产生的超声波通过功能夹具向接受超声辐照筒体4内辐照,可以显著增强超声功能。在挤出成型加热搅拌过程中,可以有效的将各种组分在超声波的作用下相互迁移,形成紧密结构,提升有韧性和强度,且透明效果更好。
本发明可全降解的复合膜的具体实施例以及其对于的试验检测数据,去下表所示,其中拉伸强度和断裂伸长率力学性能按照GB/T4456-1996的方法测试,其它性能参数均采用相应的现有标准进行测试,其中完全完全降解为所得材料经完全生物及环境降解的天数,可以是在降解促进剂作用下进行,所述降解促进剂可以是低分子量的聚乙醇酸(分子量为5000以下)。具体参见下表1所示。
上表中,杜邦为杜邦公司的DuPont Biomax Strong
所述聚(L-丙交酯-ε-己内酯)可以是L-丙交酯与ε-己内酯按75:25的摩尔比在甲苯中,在辛酸亚锡的催化下,在40℃,133Pa的条件下干燥24h;然后将压强下降到小于0.5Pa恒温融化共聚而成,在本发明工,其少量的加入,在不改变生物降解性能的情况下,可以显著提高聚乙醇酸伸长率和弹性强度等力学性能。
聚乙醇酸主要通过乙醇酸、乙醇酸酯、乙交酯等原料在催化剂作用下缩聚而得。目前可以通过乙二醇项目的中间产品草酸二甲酯,通过加氢水解法,生产成乙醇酸,在煤制乙二醇快速规模化推进中,可以极低成本的得到性能优良的聚乙醇酸。
通过上述实施例我们可以看出,本发明可全降解的复合膜具有优良的力学性能和具有良好的微生物降解性和水解性,另外材料和制备工艺成本低,具有广泛的用途。
以上所述者,仅为本发明的较佳实施例而已,当不能以此限定本发明实施的范围,即大凡依本发明申请专利范围及发明说明内容所作的简单等效变化与修饰,皆仍属本发明专利涵盖的范围内。
Claims (10)
1.一种可全降解的复合膜,其特征在于,由包括以下重量份数组分制成:
2.根据权利要求1所述的一种可全降解的复合膜,其特征在于,所述淀粉玉米淀粉、大豆淀粉、红薯淀粉、马铃薯淀粉中的一种或两种以上的组合。
3.根据权利要求1所述的一种可全降解的复合膜,其特征在于,所述阻水剂是动物类阻水剂或者植物类阻水剂,其中所述动物类阻水剂为蜂蜡、牛油、鲸油、羊毛蜡或者鲸蜡中的一种或两种以上的组合;所述植物类阻水剂为棕榈蜡、花生油、蓖麻蜡、棕榈酸、大豆油、环氧大豆油、杨梅蜡、霍霍巴油或者氢化植物油中的一种或两种以上的组合。
4.根据权利要求1所述的一种可全降解的复合膜,其特征在于,所述爽滑剂是油酸酰胺、硬脂酰胺或者芥酸酰胺。
5.根据权利要求1所述的一种可全降解的复合膜,其特征在于,所述增强纤维是木纤维、麻纤维、棉纤维、竹纤维等多种天然高分子植物纤维中的一种或者两种以上的组合。
6.根据权利要求1-5任一所述的一种可全降解的复合膜的制备方法,其特征在于,其包括的步骤如下:
(1)将聚乙醇酸、聚羟基丁酸酯、聚(L-丙交酯-ε-己内酯)和季戊四醇二亚磷酸酯粉碎,得到平均粒径60~80μm的颗粒,并混合均匀,形成混合主料;
(2)加入爽滑剂、阻水剂、增强纤维、滑石粉、壳聚糖和淀粉在低温超微粉碎机下研磨粉碎得到平均粒径60~80μm的颗粒,并混合均匀,形成混合辅料;
(3)将混合主料、混合辅料和脂肪酸甘油酯混合均匀,通过挤出机在温度为170-230℃下挤出,然后形成薄膜。
7.根据权利要求6所述的一种可全降解的复合膜的制备方法,其特征在于,所述挤出机内导入超声波处理,所述超声波处理功率为300-800W,频率为50-150KHz。
8.根据权利要求7所述的一种可全降解的复合膜的制备方法,其特征在于,所述(3)步骤中,通过挤出成膜系统来形成薄膜;所述挤出成膜系统,包括挤出机、吹胀成型环模、导向板和夹棍,所述挤出机通过连接头与吹胀成型环模连接,所述吹胀成型环模成膜出口方向设置导向板,所述导向板出口端设置夹棍;在所述吹胀成型环模的成膜出口处设置用于冷却的气环。
9.根据权利要求8所述的一种可全降解的复合膜的制备方法,其特征在于,所述气环为环绕在所述吹胀成型环模的成膜出口处的环状吹风管,其风口方向向下与成膜出口方向形成30-45度夹角。
10.根据权利要求8所述的一种可全降解的复合膜的制备方法,其特征在于,所述挤出机包括加料斗、筒体、驱动装置和机座,所述筒体固定在机座上,所述加料斗安装在筒体的进料口处,所述筒体内设置螺杆,所述螺杆与固定在所述筒体一端的驱动装置连接;所述筒体另一端设置挤出口与连接头连接;在所述筒体外侧壁上均匀的排布若干超声波换能器。
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