CN116277843B - 一种防光防腐蚀的黑膜制备工艺 - Google Patents
一种防光防腐蚀的黑膜制备工艺 Download PDFInfo
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Abstract
本发明公开了一种防光防腐蚀的黑膜制备工艺，包括以下步骤：表层挤出料的制备：将淀粉、低聚乳酸、多元酸和增塑剂投入高混机中混匀，得到第一混合物；将第一混合物与硅粉、炭黑混合，得到第二混合物；将第二混合物与防腐蚀剂、第一紫外线吸收剂、第二紫外线吸收剂在高混机中于80~90℃下混合搅拌10~12小时，得到表层挤出料；中层挤出料的制备：用电晕或表面活性剂对PET膜进行表面处理，得到中层挤出料；内层挤出料的制备：将多糖溶液、增塑剂、分散剂和明胶溶液在高混机中于40~50℃下混合均匀，得到内层挤出料；成膜。本发明采用上述的黑膜制备工艺，制备的黑膜防光照、防腐蚀，具有抑菌性和较高的力学性能，可以广泛应用于食品包装领域。
Description
技术领域
本发明属于包装袋技术领域，具体涉及一种防光防腐蚀的黑膜制备工艺。
背景技术
目前，包装袋主要以塑料材质为主，其力学性能好，具有隔水隔气特性，适用范围较广，具有明显的优势。但是因塑料本身不可降解，对环境产生不利影响。现有技术中针对上述问题开发了大量的生物质可降解基料，但是综合来看还具有以下缺点：
（1）力学性能较弱，不能满足日常生活中对包装袋的要求；
（2）不具有防光和防腐蚀的功能；
（3）虽然采用包装袋包装食品，但是其不具有抗菌功能，食品易发生变质。
发明内容
本发明的目的是提供一种防光防腐蚀的黑膜制备工艺，以解决上述包装袋力学性能较弱、功能较为单一的问题。
为实现上述目的，本发明提供了一种防光防腐蚀的黑膜制备工艺，包括以下步骤：
（1）表层挤出料的制备：将淀粉、低聚乳酸、多元酸和增塑剂投入高混机中混匀，得到第一混合物；
将第一混合物与硅粉、炭黑在高混机中混合，得到第二混合物；
将第二混合物与防腐蚀剂、第一紫外线吸收剂、第二紫外线吸收剂在高混机中于80~90℃下混合搅拌10~12小时，得到表层挤出料；
（2）中层挤出料的制备：用电晕或表面活性剂对PET膜进行表面处理，得到中层挤出料；
（3）内层挤出料的制备：将多糖溶液、增塑剂、分散剂和明胶溶液在高混机中于40~50℃下混合均匀，得到内层挤出料；
（4）成膜：将表层挤出料、中层挤出料和内层挤出料分别加入三层共挤挤出三层共挤吹膜机得到黑膜。
优选的，步骤（1）中第一紫外线吸收剂为聚硅氧烷-15，第二紫外线吸收剂为氯代苯并三唑类紫外线吸收剂。其中第一紫外线吸收剂和第二紫外线吸收剂均为直接购买所得，本发明未对其进行任何改进。
优选的，步骤（1）中防腐蚀剂包括硼酸锌、锡酸锌中的至少一种。
优选的，步骤（1）中多元有机酸为酒石酸、草酸、苹果酸、柠檬酸、对苯二甲酸中的一种或几种；步骤（1）和步骤（3）中的增塑剂包括乙二醇、木糖醇、甘油。
优选的，步骤（2）中的电晕处理条件：电压为10000伏，功率为100W；表面活性剂为CTAB，表面活性剂的加入量为PET膜质量的0.2%。
优选的，步骤（3）中的多糖包括海藻酸、壳聚糖中的一种或两种。
优选的，步骤（3）中称取多糖溶于蒸馏水中，搅拌均匀，制得4～6％的多糖溶液；称取明胶溶解在蒸馏水中，室温溶胀，然后45～50℃水浴条件下搅拌溶解后，制得10～12％的明胶溶液，然后将所述多糖溶液与所述明胶溶液混合均匀。
优选的，步骤（3）中分散剂包括硬脂酸酯和磺化改性聚乙烯醇中的一种或两种。
优选的，步骤（4）中三层共挤吹膜机的设置为：表、中、内层三层的挤出机筒温度设定为100℃、150℃、110℃，模头温度设置为150~170℃，制冷温度为15~20℃，吹胀比为1.3:1。
因此，本发明采用上述结构的一种防光防腐蚀的黑膜制备工艺，具有以下有益效果：
（1）黑膜的表层和内层分别采用淀粉和多糖作为原料，黑膜容易被环境降解，不易对环境产生影响。
（2）表层含有防腐蚀剂、第一紫外线吸收剂和第二紫外线吸收剂，可以有效抵御光照和降低外界环境对黑膜的影响，增加黑膜的使用寿命。
（3）采用对中层PET膜进行活化的方式，增加其表面的活性基团羟基的数量，进而增加其与表层和内层之间的粘接强度，避免在黑膜拉伸过程中三层产生分离。
（4）内层采用的多糖均为具有抗菌性能的多糖，同时具有能够与中层的羟基产生化学键力的基团，降低了黑膜表面和黑膜包装的食品的菌种数量，增加了黑膜的使用时间和延长了食品的储存时间，还通过氨基或羟基增加了与中层的粘接力，保证了三层黑膜的整体性。
下面通过实施例，对本发明的技术方案做进一步的详细描述。
具体实施方式
以下将对本发明进行进一步的描述，需要说明的是，本实施例以本技术方案为前提，给出了详细的实施方式和具体的操作过程，但本发明并不限于本实施例。
实施例1
一种防光防腐蚀的黑膜制备工艺，包括以下步骤：
（1）表层挤出料的制备：将淀粉、低聚乳酸、酒石酸和甘油投入高混机中混匀，得到第一混合物；
将第一混合物与硅粉、炭黑在高混机中混合，得到第二混合物；
将第二混合物与硼酸锌、聚硅氧烷-15，氯代苯并三唑类紫外线吸收剂在高混机中于80℃下混合搅拌12小时，得到表层挤出料；
（2）中层挤出料的制备：用电晕对PET膜进行表面处理，电晕处理条件：电压为10000伏，功率为100W，得到中层挤出料；
（3）内层挤出料的制备：称取海藻酸溶于蒸馏水中，搅拌均匀，制得6％的多糖溶液；称取明胶溶解在蒸馏水中，室温溶胀，然后50℃水浴条件下搅拌溶解后，制得10％的明胶溶液，然后将甘油、硬脂酸酯、所述多糖溶液与所述明胶溶液在45℃下混合均匀，得到内层挤出料；
（4）成膜：将表层挤出料、中层挤出料和内层挤出料分别加入三层共挤挤出三层共挤吹膜机，三层共挤吹膜机的设置为：表、中、内层三层的挤出机筒温度设定为100℃、150℃、110℃，模头温度设置为150℃，制冷温度为17℃，吹胀比为1.3:1，得到黑膜。
实施例2
一种防光防腐蚀的黑膜制备工艺，包括以下步骤：
（1）表层挤出料的制备：将淀粉、低聚乳酸、柠檬酸和乙二醇投入高混机中混匀，得到第一混合物；
将第一混合物与硅粉、炭黑在高混机中混合，得到第二混合物；
将第二混合物与硼酸锌、聚硅氧烷-15，氯代苯并三唑类紫外线吸收剂在高混机中于80℃下混合搅拌12小时，得到表层挤出料；
（2）中层挤出料的制备：用表面活性剂对PET膜进行表面处理，表面活性剂为CTAB，表面活性剂的加入量为PET膜质量的0.2%，得到中层挤出料；
（3）内层挤出料的制备：称取壳聚糖溶于蒸馏水中，搅拌均匀，制得4％的多糖溶液；称取明胶溶解在蒸馏水中，室温溶胀，然后45℃水浴条件下搅拌溶解后，制得12％的明胶溶液，然后将甘油、硬脂酸酯、所述多糖溶液与所述明胶溶液在50℃下混合均匀，得到内层挤出料；
（4）成膜：将表层挤出料、中层挤出料和内层挤出料分别加入三层共挤挤出三层共挤吹膜机，三层共挤吹膜机的设置为：表、中、内层三层的挤出机筒温度设定为100℃、150℃、110℃，模头温度设置为150℃，制冷温度为17℃，吹胀比为1.3:1，得到黑膜。
实施例3
一种防光防腐蚀的黑膜制备工艺，包括以下步骤：
（1）表层挤出料的制备：将淀粉、低聚乳酸、草酸和乙二醇投入高混机中混匀，得到第一混合物；
将第一混合物与硅粉、炭黑在高混机中混合，得到第二混合物；
将第二混合物与锡酸锌、聚硅氧烷-15，氯代苯并三唑类紫外线吸收剂在高混机中于90℃下混合搅拌10小时，得到表层挤出料；
（2）中层挤出料的制备：用表面活性剂对PET膜进行表面处理，表面活性剂为CTAB，表面活性剂的加入量为PET膜质量的0.2%，得到中层挤出料；
（3）内层挤出料的制备：称取海藻酸溶于蒸馏水中，搅拌均匀，制得6％的多糖溶液；称取明胶溶解在蒸馏水中，室温溶胀，然后50℃水浴条件下搅拌溶解后，制得12％的明胶溶液，然后将甘油、硬脂酸酯、所述多糖溶液与所述明胶溶液在50℃下混合均匀，得到内层挤出料；
（4）成膜：将表层挤出料、中层挤出料和内层挤出料分别加入三层共挤挤出三层共挤吹膜机，三层共挤吹膜机的设置为：表、中、内层三层的挤出机筒温度设定为100℃、150℃、110℃，模头温度设置为150℃，制冷温度为17℃，吹胀比为1.3:1，得到黑膜。
需要说明的是实施例1-3中各组分的重量份数：
步骤（1）中淀粉100份、低聚乳酸100份、多元酸10份、增塑剂5份、硅粉0.6份、炭黑1.0份、第一紫外线吸收剂16份、第二紫外线吸收剂12份；
步骤（3）中多糖溶液50份、增塑剂2份、分散剂1份、明胶溶液100份。
对比例1
与实施例1的区别在于：省略步骤（2），直接制备两层共挤挤出三层共挤吹膜机获得黑膜。
对比例2
与实施例1的区别在于：步骤（2）直接采用PET膜制备中层挤出料，未进行表面处理。
对比例3
与实施例1的区别在于：多糖为半乳糖。
实施例4
实施例1-3和对比例1-3制备的黑膜进行表征。
（1）膜抗拉强度和伸长率的测定
将膜裁成5.5cm×1.5cm的长条，用游标卡尺测定膜的厚度，两端各取0.5cm用于两端的固定，用自制测试仪器作拉伸测定，有效拉伸长度为4.5cm，记录膜断裂时伸长的距离和所挂物体的质量。每组做三个平行实验，取三者的平均值作为结果。
抗拉强度计算：
其中F＝mg，S＝dh；
伸长率的计算：
式中：TS-抗拉强度(MPa)；F-膜断裂时的拉力(N)；S-被测膜的横截面积(mm)；m-所挂物体的质量(kg)；g-重力加速度，取值9.81N/kg；d-被测膜的宽度，取值15mm；h-被测膜的厚度；U-膜伸长率(％)；L1-膜断裂时的长度(mm)；L1-膜原来的长度(mm)。
（2）膜透光率的测定
将膜样剪成1cm×4.5cm的长条状，紧贴于比色皿的一侧内表面，用分光光度计在350nm和500nm波长下，以空比色皿为参照物，分别测定膜样的透光率，并测定膜样厚度，每个样品做3组平行实验取均值。
（3）膜的阻氧性测定
按GB/T5009.37-2003方法测定。称取2g左右的食用油置于聚乙烯塑料杯中，用所制备的膜封口，再用保鲜膜贴合密封。置于常温环境下，5d后揭膜测定油样的过氧化值(POV值)，同时用敞口的油样作对照组。
（4）膜抗菌性测试
利用打孔器得到直径约为6mm的滤纸圆片，在灭菌处理后将其放入复合膜液中浸泡24h，然后将滤纸圆片贴在已接种大肠杆菌或金黄色葡萄球菌的培养基表面，将培养皿置于37℃培养箱中培养24h，观察培养基表面菌落的生长情况，测量各样品的抑菌圈直径大小。
测试结果见表1。
从表1中可以看出当中层的PET膜不存在和不进行表面处理时，对黑膜的抗拉伸强度和伸长率影响较大，两者显著降低，对于透射比、过氧化值和抑菌性的影响较小，说明表面处理的PET膜可以显著增加黑膜的力学性能。
从表1中还可以看出将海藻糖转变为半乳糖，由于半乳糖只有羟基，不具有与羟基进行化合反应的羧基和氨基，黑膜的力学性能明显有下降的趋势，说明多糖上增加与羟基能够反应的基团可以增加抗拉伸强度和伸长率，保证整个黑膜的力学性能较高。
实施例5
黑膜猪肉保鲜应用：选取外观均匀的猪肉，分割成约15g的小块，选取其中一块新鲜猪肉装入食品级PE自封袋中作为空白组，其它分别用实施例1-3和对比例1-3制备的黑膜包裹，并装入PE自封袋以隔绝外界环境影响，再把上述处理后的猪肉放入4℃冰箱中冷藏，在0、2、4、6、8天取出，分别测定猪肉样品的菌落总数。
菌落总数的测定：称1g样品与9mL生理盐水均质1-2min，得到样品匀液(1:10)，取1:10的样品匀液1mL，加入9mL生理盐水中，振摇均匀制成1:100的样品匀液，依次进行10倍递增稀释，选择2-3个稀释度适宜的样品匀液，吸取1mL样品匀液于无菌平皿内，并将固体培养基倾注于平皿中，待凝固后于36℃培养48h，同时吸取1mL生理盐水于无菌平皿内作空白对照，用肉眼观察并记录菌落数量，按照公式计算菌落总数。
用实施例1和对比例1-3制备的黑膜对新鲜猪肉进行包裹，测试结果如表2。
菌落总数(TVC)测定是用来判定食品被细菌污染的程度及卫生质量，猪肉初始菌落数为4.0(lg(CFU/g))，空白组和黑膜处理组包裹猪肉的TVC值随天数增加均不断上升，TVC值超过6.00(lg(CFU/g))说明猪肉已不再新鲜，空白组的TVC值在第六天的时候达到6.49(lg(CFU/g))，实施例1制备的黑膜的TVC值在第六天的时候为5.53(lg(CFU/g))，仍处在次新鲜的级别，说明黑膜能够减少肉类的腐败，这与其抑菌活性强的结果一致。
从表2中可以看出中层PET膜的存在与否与菌落数的影响不大，但是对比例3将多糖从海藻酸变为半乳糖，由于半乳糖不具有抑菌性能，菌落总数明显上升，在第六天的时候达到6.27(lg(CFU/g))，这与空白组的数据相差无几，说明半乳糖不具有抑菌性能。
因此，本发明采用上述结构的一种防光防腐蚀的黑膜制备工艺，内层采用的多糖均为具有抗菌性能的多糖，同时具有能够与中层的羟基产生化学键力的基团，降低了黑膜表面和黑膜包装的食品的菌种数量，增加了黑膜的使用时间和延长了食品的储存时间，还通过氨基或羟基增加了与中层的粘接力，保证了三层黑膜的力学性能。
最后应说明的是：以上实施例仅用以说明本发明的技术方案而非对其进行限制，尽管参照较佳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：其依然可以对本发明的技术方案进行修改或者等同替换，而这些修改或者等同替换亦不能使修改后的技术方案脱离本发明技术方案的精神和范围。
Claims (8)
1.一种防光防腐蚀的黑膜制备工艺，其特征在于，包括以下步骤：
（1）表层挤出料的制备：将淀粉、低聚乳酸、多元酸和增塑剂投入高混机中混匀，得到第一混合物；多元酸为酒石酸、草酸、苹果酸、柠檬酸、对苯二甲酸中的一种或几种；
将第一混合物与硅粉、炭黑在高混机中混合，得到第二混合物；
将第二混合物与防腐蚀剂、第一紫外线吸收剂、第二紫外线吸收剂在高混机中于80~90℃下混合搅拌10~12小时，得到表层挤出料；
（2）中层挤出料的制备：用电晕或表面活性剂对PET膜进行表面处理，得到中层挤出料；
（3）内层挤出料的制备：将多糖溶液、增塑剂、分散剂和明胶溶液在高混机中于40~50℃下混合均匀，得到内层挤出料；多糖包括海藻酸、壳聚糖中的一种或两种;
（4）成膜：将表层挤出料、中层挤出料和内层挤出料分别加入三层共挤挤出三层共挤吹膜机得到黑膜。
2.根据权利要求1所述的一种防光防腐蚀的黑膜制备工艺，其特征在于，步骤（1）中第一紫外线吸收剂为聚硅氧烷-15，第二紫外线吸收剂为氯代苯并三唑类紫外线吸收剂。
3.根据权利要求1所述的一种防光防腐蚀的黑膜制备工艺，其特征在于，步骤（1）中防腐蚀剂包括硼酸锌、锡酸锌中的至少一种。
4.根据权利要求1所述的一种防光防腐蚀的黑膜制备工艺，其特征在于，步骤（1）和步骤（3）中的增塑剂包括乙二醇、木糖醇、甘油。
5.根据权利要求1所述的一种防光防腐蚀的黑膜制备工艺，其特征在于，步骤（2）中的电晕处理条件：电压为10000伏，功率为100W；表面活性剂为CTAB，表面活性剂的加入量为PET膜质量的0.2%。
6.根据权利要求1所述的一种防光防腐蚀的黑膜制备工艺，其特征在于，步骤（3）中称取多糖溶于蒸馏水中，搅拌均匀，制得4～6％的多糖溶液；称取明胶溶解在蒸馏水中，室温溶胀，然后45～50℃水浴条件下搅拌溶解后，制得10～12％的明胶溶液，然后将所述多糖溶液与所述明胶溶液混合均匀。
7.根据权利要求1所述的一种防光防腐蚀的黑膜制备工艺，其特征在于，步骤（3）中分散剂包括硬脂酸酯和磺化改性聚乙烯醇中的一种或两种。
8.根据权利要求1所述的一种防光防腐蚀的黑膜制备工艺，其特征在于，步骤（4）中三层共挤吹膜机的设置为：表、中、内层三层的挤出机筒温度设定为100℃、150℃、110℃，模头温度设置为150~170℃，制冷温度为15~20℃，吹胀比为1.3:1。
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