CN116289183B - 一种抑菌抗老化无纺布及其制备方法 - Google Patents
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Abstract
本发明公开了一种抑菌抗老化无纺布,以重量份数计,由以下组分制成:聚丙烯无纺布0.5~1份、甲基丙烯酸80~100份、改性SiO24~6份、木犀草素2~5份;一种抑菌抗老化无纺布的制备方法,包括如下步骤:取二苯甲酮溶于丙酮溶液中,然后加入甲基丙烯酸,得到处理液,然后将聚丙烯无纺布加入到处理液中浸渍;取出浸渍好的聚丙烯无纺布,在氮气气氛下,用紫外灯辐射,得到甲基丙烯酸接枝无纺布;将改性纳米SiO2分散入丁酮中,搅拌下加入木犀草素,然后将甲基丙烯酸接枝无纺布浸渍到分散液中,反应结束后洗涤、烘干得到抑菌抗老化无纺布。
Description
技术领域
本发明涉及无纺布技术领域,具体涉及一种抑菌抗老化无纺布及其制备方法。
背景技术
无纺布,又称非织造布或不织布,是由定向或随机排列的纤维通过粘合等不同方法组合而结合而成的,为柔软、质轻、透气和平面结构的新型纤维结构产品,还具有工艺流程短、生产效率高、经济效益显著、产品品种丰富和使用范围广等特点,已成为纺织工业的新兴产业。用于无纺布的纤维原料可以是棉等天然纤维和聚丙烯、聚酯、粘胶等化学纤维,但目前化学纤维占有支配地位。聚丙烯无纺布由于其具有无毒、色彩丰富、耐酸碱、耐化学腐蚀、耐磨性较好,抗微生物性能好和不霉不蛀等优势,成为无纺布生产中总量最大的品种。按照聚丙烯无纺布的功能进行分类,主要有亲水型、抗菌型、抗静电型、阻燃型和抗老化型等,广泛应用于过滤、医疗、卫生、保健、工业、农业、土木水利工程、建筑、家庭装饰及生活的各个领域。
中国专利CN1346905A提供了一种载银抗菌复合无纺布制造方法,包括以下工序:1)抗菌母粒制作:按载银抗菌材料25-50%重量份、纤维树脂40-75%重量份、塑料助剂0-10%重量份,经螺杆挤出造粒机进行混熔造粒机混熔,制成抗菌母粒;2)抗菌纺粘网制作:按抗菌母粒2-4%重量份与纤维树脂96-98%重量份进行混合后,按常规纺粘工艺制成抗菌纺粘网;3)复合抗菌无纺布制作:将抗菌纺粘网和棉纤维网或木浆纤维网进行复合水刺处理后,进行烘干,即成为复合抗菌无纺布。但该方法制成的抗菌复合无纺布成本较高,且抗老化性能较差。
中国专利文献200610104887.4公开了一种纤维无纺布果蔬保鲜膜系列制品,选择化纤无纺布、植物纤维无纺布、化纤与植物纤维复合无纺布为基础材料;将其单层或复合层制成保鲜膜卷材;经裁剪、热封等制成果蔬贮藏运输保鲜袋、塑料筐或篮、木条箱、包装箱的内衬以及各种形状的保鲜帐。上述基础材料可先用硅烷偶联剂、纳米SiO2及水溶性硅油混合配制成的纳米SiO2乳化分散液涂于基料表面,常温晾干或烘干,再制作成纤维无纺布保鲜膜系列制品。使用前,用杀菌剂、保鲜剂喷洒或浸蘸处理。但该无纺布果蔬保鲜膜系列制品是在使用前采用杀菌剂、保鲜剂喷洒或浸蘸处理无纺布材料,杀菌、保鲜效果持续时间较短。
因此急需提供一种制备工艺简单,成本低廉,抗菌性能好,抗老化性能优异的无纺布。
发明内容
为了解决现有技术存在的不足,本发明的目的在于提供一种抑菌抗老化无纺布及其制备方法,制备工艺简单,制备成本低廉,抗菌性能好,抗老化性能优异。
为了实现上述目的,本发明采用如下技术方案:
一种抑菌抗老化无纺布,以重量份数计,由以下组分制成:聚丙烯无纺布0.5~1份、甲基丙烯酸80~100份、改性SiO24~6份、木犀草素2~5份。
优选的,所述聚丙烯无纺布克重为50~100g/m2。
优选的,所述改性SiO2的制备方法如下:将纳米SiO2在120℃下烘干3~4h,将纳米SiO2、丙酮和γ-氨丙基三甲氧基硅烷加入到反应容器中,打开磁力搅拌和加热,110℃回流反应2h,反应结束后洗涤、干燥,得到氨基化纳米SiO2;将氨基化纳米SiO2、丙酮、有机锡和二苯基甲烷二异氰酸酯加入反应容器中,超声分散30~60min,缓慢升温到70℃,恒温搅拌3~5h,反应结束后离心,将沉淀物洗涤、干燥,得到改性纳米SiO2。
优选的,纳米SiO2、甲苯和γ-氨丙基三甲氧基硅烷的重量比为4~6:100:8~10。
优选的,氨基化纳米SiO2、甲苯、有机锡和二苯基甲烷二异氰酸酯的重量比为4~6:100:0.1:3.2~4.8。
本发明还要求保护一种所述抑菌抗老化无纺布的制备方法,包括如下步骤:
(1)用无水乙醇、0.5mol/LNaOH溶液洗涤聚丙烯无纺布,烘干备用;取二苯甲酮溶于丙酮溶液中,然后加入甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍70~90min;
(2)取出浸渍好的聚丙烯无纺布沥干液体,在氮气气氛下,用紫外灯辐射,得到甲基丙烯酸接枝无纺布;
(3)将改性纳米SiO2分散入丁酮中,将步骤(2)所得甲基丙烯酸接枝无纺布浸渍到分散液中,然后加入有机锡、木犀草素,磁力搅拌下反应4~6h,反应结束后洗涤、干燥,得到抑菌抗老化无纺布。
优选的,步骤(1)中,丙酮溶液体积浓度为50%;二苯甲酮、丙酮溶液与甲基丙烯酸的重量比为1~2:150~200:80~100。
优选的,步骤(2)中,紫外灯功率为400~500W,辐射反应温度为50~60℃,聚丙烯无纺布正反面各辐射60~90min。
优选的,步骤(3)中,反应温度为75℃,改性纳米SiO2、有机锡、丁酮的质量体积比为4~6:0.1:160~200。
本发明还要求保护一种所述抑菌抗老化无纺布在水果包装中的应用。
与现有技术相比,本发明具有如下有益效果:
1)本发明提供的抑菌抗老化无纺布,首先通过辐射交联将甲基丙烯酸接枝到聚丙烯无纺布上,然后利用γ-氨丙基三甲氧基硅烷处理纳米SiO2得到氨基化纳米SiO2,然后通过二苯基甲烷二异氰酸酯对氨基化纳米SiO2进行改性,引入苯基和异氰酸酯基团,然后通过脱水缩合将改性纳米二氧化硅接枝到甲基丙烯酸链上,使纳米二氧化硅能够稳固附着在无纺布主体上同时引入氨基甲基酯基团,SiO2与苯基、氨基甲基酯基团协同,能够显著提高聚丙烯无纺布的抗氧化、抗老化性能。
2)本发明提供的抑菌抗老化无纺布,利用甲基丙烯酸将羧基引入聚丙烯无纺布,又通过γ-氨丙基三甲氧基硅烷引入氨基,使得改性后无纺布与木犀草素分子之间能形成多点位的氢键,从而增强聚丙烯无纺布对木犀草素的负载能力,能够有效延长木犀草素的作用效果;木犀草素具有抗氧化、抑菌、抗病毒等生理活性,可使微生物细胞蛋白质变性、能量合成受阻,且安全无毒、生物相容性好,将其对聚丙烯无纺布进行浸渍改性,可以大大提高无纺布的抗菌性能,扩大聚丙烯无纺布的应用范围和应用前景。
3)本发明提供的抑菌抗老化无纺布,能够作为水果保鲜抑菌包装材料,保护水果在储运、销售等过程中免受各种微生物以及环境因素的影响,在保持水果色香味的基础上同时延长水果保质期,而且本发明提供的制备方法工艺简单、造价低廉,适合工业化生产。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚,以下结合实施例,对本发明作进一步的详细说明。当然,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
如无特殊说明外,本发明中的化学试剂和材料均通过市场途径购买或通过市场途径购买的原料合成。
无纺布购自广州市溢和泰无纺布有限公司,克重50~100g/m2;
木犀草素购自陕西瑞沃生物科技有限公司,CAS:491-70-3,纯度98%;
有机锡购自新典化学材料(上海)有限公司,CAS:77-58-7;
纳米SiO2购自浙江弘晟材料科技股份有限公司,型号SS1,比表面积120m2/g,平均粒径20nm,纯度99%。
实施例1
一种抑菌抗老化无纺布的制备方法,包括如下步骤:
(1)取克重为100g/m2、大小为10cm×10cm的聚丙烯无纺布,用无水乙醇、0.5mol/LNaOH溶液洗涤,烘干备用;取2g二苯甲酮溶于200g体积浓度50%丙酮溶液中,然后加入100g甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍90min;
(2)取出浸渍好的聚丙烯无纺布沥干液体,在氮气气氛下,用500W紫外灯在60℃下将聚丙烯无纺布正反面各辐射90min,得到甲基丙烯酸接枝无纺布;
(3)将纳米SiO2在120℃下烘干4h,将6g纳米SiO2、100g甲苯和10gγ-氨丙基三甲氧基硅烷加入反应容器中,打开磁力搅拌和加热,110℃下回流反应2h,反应结束后洗涤、干燥,得到氨基化纳米SiO2;将氨基化纳米SiO2、100g甲苯、0.1g二月桂酸二丁锡和4.8g二苯基甲烷二异氰酸酯加入反应容器中,超声分散60min,缓慢升温到70℃,恒温搅拌5h,反应结束后离心,将沉淀物洗涤、干燥,得到改性纳米SiO2;
(4)将6g改性纳米SiO2分散到200mL丁酮中得到分散液,将步骤(2)所得甲基丙烯酸接枝无纺布浸渍到分散液中,然后加入0.1g二月桂酸二丁锡、5g木犀草素,开启磁力搅拌,75℃下反应6h,反应结束后洗涤、干燥,得到抑菌抗老化无纺布。
实施例2
一种抑菌抗老化无纺布的制备方法,包括如下步骤:
(1)取克重为50g/m2、大小为10cm×10cm的聚丙烯无纺布,用无水乙醇、0.5mol/LNaOH溶液洗涤,烘干备用;取1g二苯甲酮溶于150g体积浓度50%丙酮溶液中,然后加入80g甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍70min;
(2)取出浸渍好的聚丙烯无纺布沥干液体,在氮气气氛下,用400W紫外灯在50℃下将聚丙烯无纺布正反面各辐射60min,得到甲基丙烯酸接枝无纺布;
(3)将纳米SiO2在120℃下烘干3~4h,将4g纳米SiO2、100g甲苯和8gγ-氨丙基三甲氧基硅烷加入反应容器中,打开磁力搅拌和加热,110℃下回流反应2h,反应结束后洗涤、干燥,得到氨基化纳米SiO2;将氨基化纳米SiO2、100g甲苯、0.1g二月桂酸二丁锡和3.2g二苯基甲烷二异氰酸酯加入反应容器中,超声分散30min,缓慢升温到70℃,恒温搅拌3h,反应结束后离心,将沉淀物洗涤、干燥,得到改性纳米SiO2;
(4)将4g改性纳米SiO2分散到160mL丁酮中得到分散液,将步骤(2)所得甲基丙烯酸接枝无纺布浸渍到分散液中,然后加入0.1g二月桂酸二丁锡、2g木犀草素,开启磁力搅拌,75℃下反应4h,反应结束后洗涤、干燥,得到抑菌抗老化无纺布。
实施例3
一种抑菌抗老化无纺布的制备方法,包括如下步骤:
(1)取克重为80g/m2、大小为10cm×10cm的聚丙烯无纺布,用无水乙醇、0.5mol/LNaOH溶液洗涤,烘干备用;取1.5g二苯甲酮溶于180g体积浓度50%丙酮溶液中,然后加入90g甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍80min;
(2)取出浸渍好的聚丙烯无纺布沥干液体,在氮气气氛下,用450W紫外灯在55℃下将聚丙烯无纺布正反面各辐射80min,得到甲基丙烯酸接枝无纺布;
(3)将纳米SiO2在120℃下烘干3.5h,将5g纳米SiO2、100g甲苯和9gγ-氨丙基三甲氧基硅烷加入反应容器中,打开磁力搅拌和加热,110℃下回流反应2h,反应结束后洗涤、干燥,得到氨基化纳米SiO2;将氨基化纳米SiO2、100g甲苯、0.1g二月桂酸二丁锡和4.0g二苯基甲烷二异氰酸酯加入反应容器中,超声分散50min,缓慢升温到70℃,恒温搅拌4h,反应结束后离心,将沉淀物洗涤、干燥,得到改性纳米SiO2;
(4)将5g改性纳米SiO2分散到180mL丁酮中得到分散液,将步骤(2)所得甲基丙烯酸接枝无纺布浸渍到分散液中,然后加入0.1g二月桂酸二丁锡、4g木犀草素,开启磁力搅拌,75℃下反应5h,反应结束后洗涤、干燥,得到抑菌抗老化无纺布。
对比例1
一种无纺布的制备方法,包括如下步骤:
(1)取克重为100g/m2、大小为10cm×10cm的聚丙烯无纺布,用无水乙醇、0.5mol/LNaOH溶液洗涤,烘干备用;取2g二苯甲酮溶于200g体积浓度50%丙酮溶液中,然后加入100g甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍90min;
(2)将纳米SiO2在120℃下烘干4h,将6g纳米SiO2、100g甲苯和10gγ-氨丙基三甲氧基硅烷加入反应容器中,打开磁力搅拌和加热,110℃下回流反应2h,反应结束后洗涤、干燥,得到氨基化纳米SiO2;将氨基化纳米SiO2、100g甲苯、0.1g二月桂酸二丁锡和4.8g二苯基甲烷二异氰酸酯加入反应容器中,超声分散60min,缓慢升温到70℃,恒温搅拌5h,反应结束后离心,将沉淀物洗涤、干燥,得到改性纳米SiO2;
(3)将6g改性纳米SiO2分散到200mL丁酮中得到分散液,将步骤(1)所得无纺布浸渍到分散液中,然后加入0.1g二月桂酸二丁锡、5g木犀草素,开启磁力搅拌,75℃下反应6h,反应结束后用水洗涤5次,烘干得到一种无纺布。
对比例2
一种无纺布的制备方法,包括如下步骤:
(1)取克重为100g/m2、大小为10cm×10cm的聚丙烯无纺布,用无水乙醇、0.5mol/LNaOH溶液洗涤,烘干备用;取2g二苯甲酮溶于200g体积浓度50%丙酮溶液中,然后加入100g甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍90min;
(2)取出浸渍好的聚丙烯无纺布沥干液体,在氮气气氛下,用500W紫外灯在60℃下将聚丙烯无纺布正反面各辐射90min,得到甲基丙烯酸接枝无纺布;
(3)将6g纳米SiO2分散到200mL丁酮中得到分散液,将步骤(2)所得甲基丙烯酸接枝无纺布浸渍到分散液中,然后加入0.1g二月桂酸二丁锡、5g木犀草素,开启磁力搅拌,75℃下反应6h,反应结束后用水洗涤5次,烘干得到一种无纺布。
对比例3
一种无纺布的制备方法,包括如下步骤:
(1)取克重为100g/m2、大小为10cm×10cm的聚丙烯无纺布,用无水乙醇、0.5mol/LNaOH溶液洗涤,烘干备用;取2g二苯甲酮溶于200g体积浓度50%丙酮溶液中,然后加入100g甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍90min;
(2)取出浸渍好的聚丙烯无纺布沥干液体,在氮气气氛下,用500W紫外灯在60℃下将聚丙烯无纺布正反面各辐射90min,得到甲基丙烯酸接枝无纺布;
(3)将纳米SiO2在120℃下烘干4h,将6g纳米SiO2、100g甲苯和10gγ-氨丙基三甲氧基硅烷加入反应容器中,打开磁力搅拌和加热,110℃下回流反应2h,反应结束后洗涤、干燥,得到氨基化纳米SiO2;将氨基化纳米SiO2、100g甲苯、0.1g二月桂酸二丁锡和4.8g二苯基甲烷二异氰酸酯加入反应容器中,超声分散60min,缓慢升温到70℃,恒温搅拌5h,反应结束后离心,将沉淀物洗涤、干燥,得到改性纳米SiO2;
(4)将6g改性纳米SiO2分散到200mL丁酮中得到分散液,将步骤(2)所得甲基丙烯酸接枝无纺布浸渍到分散液中,然后加入0.1g二月桂酸二丁锡,开启磁力搅拌,75℃下反应6h,反应结束后用水洗涤5次,烘干得到一种无纺布。
依据实施例1~3、对比例1~3方法制备得到无纺布,各组裁剪成15mm×20mm的条样6个,按照GB/T 24218-2017《纺织品非织造布试验方法第3部分:断裂强力和断裂伸长率的测定(条样法)》用电子拉力试验机进行力学性能测试,随后将各样品参考GB/T16422.3-2022《塑料实验室光源暴露试验方法第3部分:荧光紫外灯》中循环序号1进行紫外光照试验,老化天数为14天,老化试验后对无纺布进行力学性能测试,试验结果见表1。
表1无纺布抗老化性能数据
对实施例1~3、对比例1~3制备所得无纺布材料进行抑菌性检测,参考标准GB/T21510-2008《纳米无机材料抗菌性能检测方法》进行测定,具体数据见表2。
表2无纺布抑菌性能数据
对比例1未利用甲基丙烯酸对聚丙烯无纺布进行接枝改性,对比例2未对纳米SiO2进行改性,二者制备得到的无纺布产品对木犀草素的负载作用均不佳,因而其抑菌效果要差于实施例制备所得无纺布,且水洗50次后的抑菌率下降较大;对比例3中未添加木犀草素,其制备所得无纺布产品抑菌效果及抑菌持续效果均最差。
利用实施例1方法制备得到抑菌抗老化无纺布,用热风机将其制成袋子(实验组),再取市售克重100g/m2无纺布制成包装袋(空白组),购买未经保鲜剂处理的新鲜草莓,挑选形状、大小、成熟度相近的草莓10颗,平均分为两组,分别装入实验组、空白组制成的包装袋中,用热风机封口,放于室内,每隔48h测草莓的失重率,具体数据见表3。
表3草莓失重率记录表(单位:%)
第2天 | 第4天 | 第6天 | 第8天 | |
实验组 | 8.2 | 17.6 | 21.5 | 28.1 |
空白组 | 11.5 | 23.7 | 26.8 | 52.4 |
从表3中试验数据可以看出,本发明提供的抑菌抗老化无纺布相较于市售普通无纺布,能够有效延长水果的保存时间。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种抑菌抗老化无纺布,其特征在于,以重量份数计,由以下组分制成:聚丙烯无纺布0.5~1份、甲基丙烯酸80~100份、改性SiO2 4~6份、木犀草素2~5份;
所述改性SiO2的制备方法如下:将纳米SiO2在120℃下烘干3~4h,将纳米SiO2、甲苯和γ-氨丙基三甲氧基硅烷加入到反应容器中,打开磁力搅拌和加热,110℃回流反应2h,反应结束后洗涤、干燥,得到氨基化纳米SiO2;将氨基化纳米SiO2、甲苯、有机锡和二苯基甲烷二异氰酸酯加入反应容器中,超声分散30~60min,缓慢升温到70℃,恒温搅拌3~5h,反应结束后离心,将沉淀物洗涤、干燥,得到改性纳米SiO2;
所述抑菌抗老化无纺布的制备方法,包括如下步骤:
(1)用无水乙醇、0.5mol/L NaOH溶液洗涤聚丙烯无纺布,烘干备用;取二苯甲酮溶于丙酮溶液中,然后加入甲基丙烯酸,混合均匀,得到处理液;然后将聚丙烯无纺布加入到处理液中,常温下浸渍70~90min;
(2)取出浸渍好的聚丙烯无纺布沥干液体,在氮气气氛下,用紫外灯辐射,得到甲基丙烯酸接枝无纺布;
(3)将改性纳米SiO2分散入丁酮中,将步骤(2)所得甲基丙烯酸接枝无纺布浸渍到分散液中,然后加入有机锡、木犀草素,磁力搅拌下反应4~6h,反应结束后洗涤、干燥,得到抑菌抗老化无纺布。
2.根据权利要求1所述的抑菌抗老化无纺布,其特征在于,所述聚丙烯无纺布克重为50~100g/m2。
3.根据权利要求1所述的抑菌抗老化无纺布,其特征在于,纳米SiO2、甲苯和γ-氨丙基三甲氧基硅烷的重量比为4~6:100:8~10。
4.根据权利要求1所述的抑菌抗老化无纺布,其特征在于,氨基化纳米SiO2、甲苯、有机锡和二苯基甲烷二异氰酸酯的重量比为4~6:100:0.1:3.2~4.8。
5.根据权利要求1所述的抑菌抗老化无纺布,其特征在于,步骤(1)中,丙酮溶液体积浓度为50%;二苯甲酮、丙溶液与甲基丙烯酸的重量比为1~2:150~200:80~100。
6.根据权利要求1所述的抑菌抗老化无纺布,其特征在于,步骤(2)中,紫外灯功率为400~500W,辐射反应温度为50~60℃,聚丙烯无纺布正反面各辐射60~90min。
7.根据权利要求1所述的抑菌抗老化无纺布,其特征在于,步骤(3)中,反应温度为75℃,改性纳米SiO2、有机锡、丁酮的质量体积比为4~6:0.1:160~200。
8.一种如权利要求1~7任一项所述抑菌抗老化无纺布在水果包装中的应用。
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