CN105918312A - 一种新型纳米防霉抗菌剂 - Google Patents
一种新型纳米防霉抗菌剂 Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/48—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —S—C≡N groups
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- General Health & Medical Sciences (AREA)
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- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
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- Toxicology (AREA)
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Abstract
本发明的提供一种安全高效，制备简单，具有超长的抗菌效果的新型防霉抗菌剂组合物，包括1‑5质量份具有核壳结构的纳米颗粒、1‑3质量份的杀菌剂、0.5‑1.5质量份的表面活性剂、15‑30质量份的有机溶剂。本发明的防霉抗菌剂包含具有核壳结构的纳米颗粒，具有长效的抗菌性能，与细菌接触6h以后，杀菌率可以达到100％，且经过10天以后，依然具有很好的杀菌率。
Description
技术领域
本发明属于防霉抗菌剂领域，具体的说是一种具有核壳结构的纳米防霉抗菌剂及其制备方法。
背景技术
纳米材料是一种广泛使用的新型防霉抗菌剂，其化学稳定性较好，对环境影响小，抗菌性强，对多种微生物都有抑制作用，越来越广泛的应用于人们的生活中。目前常见的纳米防霉抗菌剂主要有无机纳米材料如纳米金属，纳米无机氧化物，纳米无机盐等。纳米材料的杀菌机理存在三种作用，包括：一是纳米银颗粒本身可以吸附并在细菌细胞壁表面富集，引起菌体细胞裂解；二是纳米颗粒可以释放出金属离子，银离子可以穿透细胞壁进入细胞内，与微生物体内的蛋白质、核酸中存在的巯基(-SH)、氨基(-NH2)等含硫、氮的官能团发生反应，破坏酶和遗传物质的活性，引起细菌死亡；三是纳米材料可以产生高氧化性的活性氧基团，像超氧离子、过氧化氢和氢氧自由基等，与细菌体内的物质发生反应氧化反应，引起细菌死亡。
纳米防霉抗菌剂虽然抗菌性能优良，但是存在易团聚，对某些微生物的抗菌效果不佳的问题。本发明对传统的纳米防霉抗菌剂进行改良，不仅对纳米颗粒的表面进行了改性，改善了其容易团聚的问题，还以纳米材料为核心制备出具有核壳结构的纳米防霉抗菌剂，将有机杀菌剂负载于纳米颗粒材料上，并包裹一层有机聚合物，使杀菌剂可以缓慢释放，大大延长纳米防霉抗菌剂的有效抗菌寿命。所述纳米抗菌材料还可以与其它防霉抗菌剂混合使用，以增强其抗菌效果。
本发明还通过多年的研究优选出具有较好抗菌性能的三嗪衍生物用于制备核壳结构的纳米防霉抗菌剂，三嗪衍生物具有良好的生物活性。
CN1426683A公开了一种耐高温抗变色无机抗菌防霉剂的制备方法，该防霉抗菌剂是以银为活性组分或以银锌为活性组分，以羟基磷灰石或其分解产物为载体。该防霉抗菌剂是纳米至微米的粉末，具有耐高温、抗变色的优点。
CN101161336公布了一种负载纳米金属银粒子氧化石墨的制备方法，但是该方法需要在暗室条件下进行搅拌，条件较为苛刻，且制备过程中使用较多的有机溶剂，不够环保。
CN101116446A公开了一种抗菌防霉剂的制备方法，将多聚糖类水溶性粘合剂溶于酸性溶液中，然后加入纳米二氧化钛，纳米二氧化钛的加入量与粘合剂的用量比为0.01-10g/g，混合后加入有机交联剂，得到抗菌防霉剂。该杀菌剂经表面涂敷，风干成膜后即可起到抗菌防霉效果，4h杀菌率几乎达到100％。
发明内容
本发明的目的在于提供一种安全高效，制备简单，具有超长的抗菌效果的防霉抗菌剂组合物。本发明的防霉抗菌剂组合物包含具有独特核壳结构的纳米颗粒，创造性的提出将噻二唑均三嗪吸附于含有微孔的纳米颗粒上，噻二唑均三嗪具有较好的吸附和穿透性能，不仅可以吸附于纳米颗粒的表面而且可以部分进入其孔道结构中，负载了噻二唑均三嗪的纳米颗粒再通过高分子有机聚合物的包裹，表面的高分子聚合物在自然环境下缓慢降解，逐渐释放出负载的噻二唑均三嗪，就可以发挥长久的抗菌作用，同时防霉抗菌剂组合物中还包括有短效的杀菌剂，以弥补防霉抗菌剂组合物在使用初期的抗菌效果，并且具有核壳结构的纳米颗粒本身作为纳米材料也可以具有一定的抗菌效果，可以杀灭绝大多数的菌类微生物。
一种新型防霉抗菌剂组合物，包括1-5质量份具有核壳结构的纳米颗粒、1-3质量份的杀菌剂、0.5-1.5质量份的表面活性剂、15-30质量份的有机溶剂；优选含有3-5质量份具有核壳结构的纳米颗粒、2-3质量份的杀菌剂、0.5-1质量份的表面活性剂、20-25质量份的有机溶剂。
所述具有核壳结构的纳米颗粒是包埋在有机高分子聚合物中，负载了噻二唑均三嗪的纳米颗粒，所述有机高分子聚合物是羧甲基纤维素钠或聚甲基丙烯酸酯；
所述表面活性剂是壬基酚聚氧乙烯醚，烷基酚聚氧乙烯醚磷酸酯中的一种或多种；
所述有机溶剂是乙醇，碳酸二甲酯，甲苯中的一种或多种；
所述杀菌剂是氨基甲基正丁基碘代炔丙酯、二硫氰基乙烷、2-甲基-4-异噻唑晽-3-酮中的一种或多种。
所述纳米微粒是碳纳米管、沸石、磷酸锌、碳酸钙、氧化锌、氧化钛中的一种或多种，优选是沸石和碳纳米管。
所述纳米粒子的平均粒径是50-1000nm，优选是100-300nm。
所述防霉抗菌剂组合物中还可以含有成膜助剂，所述成膜助剂是醇胺类或醇脂类成膜助剂。
所述噻二唑均三嗪的化学结构通式如下所示：
其中R1、R2、R3独立的选自C1-C6的烷基，烷羟基或烷基羧基。
所述核壳结构纳米颗粒的制备方法，包括如下步骤，将纳米颗粒浸渍在六氢三嗪衍生物的溶液中3-12h；将上述经过浸渍后的纳米颗粒进行干燥；将经过干燥后的纳米颗粒浸渍在有机高分子聚合物的溶液1-3h，将前一步得到的纳米颗粒干燥。所述浸渍可以反复进行1-3次
所述复合杀菌剂可以单独使用，也可以作为添加剂加入到涂料中使用。
所述包含核壳结构纳米颗粒的防霉抗菌剂组合物的制备方法，按照质量份数将所述具有核壳结构的纳米颗粒、杀菌剂、表面活性剂、有机溶剂依次加入到反应釜中，在40-60℃下搅拌，并用超声波进行辅助粉碎处理，即可得到所述防霉抗菌剂组合物。
具体实施方式
实施例1
配制浓度为10wt％的噻二唑均三嗪水溶液，将粒径为50-100nm的沸石纳米颗粒混合在水溶液中浸渍12h，将浸渍后的沸石纳米颗粒取出在110℃下干燥2h，然后将浸渍过的沸石纳米颗粒加入到5wt％的羧甲基纤维素钠溶液中浸渍3h后取出，在150℃下干燥5h，得到所述具有核壳结构的纳米颗粒。
取5kg制备好的具有核壳结构的纳米颗粒、2kg的氨基甲基正丁基碘代炔丙酯、1kg的烷基酚聚氧乙烯醚磷酸酯、20kg的乙醇经过搅拌和超声波粉碎即可得到所述防霉抗菌剂组合物。
实施例2
配制浓度为15wt％的噻二唑均三嗪水溶液，将粒径为50-100nm的碳纳米管颗粒混合在水溶液中浸渍6h，将浸渍后的碳纳米管颗粒取出在110℃下干燥1h，然后将浸渍过的沸石纳米颗粒加入到5wt％的聚甲基丙烯酸酯溶液中浸渍2h后取出，在130℃下干燥5h，得到所述具有核壳结构的纳米颗粒。
取3kg制备好的具有核壳结构的纳米颗粒、3kg的二硫氰基乙烷、1kg的壬基酚聚氧乙烯醚、20kg的碳酸二甲酯经过搅拌和超声波粉碎即可得到所述防霉抗菌剂组合物。
以实施例1得到的防霉抗菌剂组合物为例对本发明的防霉抗菌剂进行抗菌性能测试，测试的菌种包括大肠杆菌和金黄色葡萄球菌两种，这两种细菌是具有代表性的细菌。测定方法是将防霉抗菌剂加入两种细菌的培养液中，其中每种细菌培养液的菌种浓度为0.1-5×107，防霉抗菌剂的加入量为100-1000ppm，接触6h后实验的结果如下所示，接触24h抗菌率基本都达到100％。
表1防霉抗菌剂接触6h后的抗菌效果
为了验证本发明所述防霉抗菌剂的长效抗菌效果，将保持了所述防霉抗菌剂经过初次抗菌实验后，保存10d，再次加入细菌培养液，接触6h后，再次测定抗菌效果，实验结果如表2所示，接触超过24h后，抗菌效果基本达到100％。
表2 10d后抗菌效果
从上述实验结果我们不难看出，所述防霉抗菌剂对细菌有明显的杀菌抑制作用，尤其是在接触24小时以后更为明显。本发明所述防霉抗菌剂还具有长效杀菌抑制效果，在经过10d的放置后，依然具有很强的抗菌效果。
Claims (9)
1.一种新型防霉抗菌剂组合物，包括1-5质量份具有核壳结构的纳米颗粒、1-3质量份的杀菌剂、0.5-1.5质量份的表面活性剂、15-30质量份的有机溶剂；所述具有核壳结构的纳米颗粒是将负载了噻二唑均三嗪的纳米颗粒包埋在有机高分子聚合物中制得，所述有机高分子聚合物是羧甲基纤维素钠或聚甲基丙烯酸酯。
2.如权利要求1所述的防霉抗菌剂组合物，其特征在于所述组合物包括3-5质量份具有核壳结构的纳米颗粒、2-3质量份的杀菌剂、0.5-1质量份的表面活性剂、20-25质量份的有机溶剂。
3.如权利要求1所述的防霉抗菌剂组合物，其特征在于所述表面活性剂是壬基酚聚氧乙烯醚，烷基酚聚氧乙烯醚磷酸酯中的一种或多种。
4.如权利要求1所述的防霉抗菌剂组合物，其特征在于所述有机溶剂是乙醇，碳酸二甲酯，甲苯中的一种或多种。
5.如权利要求1所述的防霉抗菌剂组合物，其特征在于所述杀菌剂是氨基甲基正丁基碘代炔丙酯、二硫氰基乙烷、2-甲基-4-异噻唑晽-3-酮中的一种或多种。
6.如权利要求1所述的防霉抗菌剂组合物，其特征在于所述纳米微粒是碳纳米管、沸石、磷酸锌、碳酸钙、氧化锌、氧化钛中的一种或多种，优选是沸石或碳纳米管，所述纳米粒子的平均粒径是50-1000nm。
7.如权利要求1所述的防霉抗菌剂组合物，其特征在于所述防霉抗菌剂组合物中还可以含有成膜助剂，所述成膜助剂是醇胺类或醇脂类成膜助剂。
8.如权利要求1所述的防霉抗菌剂组合物，其特征在于所述噻二唑均三嗪的化学结构通式如下所示：
其中R1、R2、R3独立的选自C1-C6的烷基，烷羟基或烷基羧基。
9.制备如权利要求1-8任一项所述的防霉抗菌剂组合物的方法，包括如下步骤，将纳米颗粒浸渍在六氢三嗪衍生物的溶液中3-12h；将上述经过浸渍后的纳米颗粒进行干燥；将经过干燥后的纳米颗粒浸渍在有机高分子聚合物的溶液1-3h，将前一步得到的纳米颗粒干燥。
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