CN113679620A - 一种含有胶态银的抗菌防腐组合物及其制备方法 - Google Patents
一种含有胶态银的抗菌防腐组合物及其制备方法 Download PDFInfo
- Publication number
- CN113679620A CN113679620A CN202110632033.8A CN202110632033A CN113679620A CN 113679620 A CN113679620 A CN 113679620A CN 202110632033 A CN202110632033 A CN 202110632033A CN 113679620 A CN113679620 A CN 113679620A
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- Prior art keywords
- antiseptic
- colloidal silver
- antibacterial
- component
- silver
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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Abstract
本发明涉及抗菌防腐技术领域,具体涉及一种含有胶态银的抗菌防腐组合物及其制备方法。按重量份计,包括胶态银,防腐成分和分散剂。所述胶态银,防腐成分和分散剂的重量比为(1‑5):(3‑8):(5‑20)。本发明提供了一种含有胶态银的抗菌防腐组合物及其制备方法抗菌速度快,防腐效果好,广谱性高,适用范围广泛。
Description
技术领域
本发明涉及抗菌防腐技术领域,具体涉及一种含有胶态银的抗菌防腐组合物及其制备方法。
背景技术
微生物与人类关系密切,生活中细菌无处不在,这些微生物既能造福于人类,也能给人类带来毁灭性的灾难。比如食物,化妆品,医药等变质。不仅给人们的生活带来严重的经济损失,更会危及人们的生命健康,因此关于抗菌防腐产品的研制势在必行。
专利201810772629.6提供了一种含有辛酰羟肟酸的复配防腐剂及其制备方法,包括辛酰羟肟酸,对羟基苯乙酮,乙基己基甘油等物质,对许多细菌都具有抗菌效果,但该方法提供的防腐剂短时间内杀菌抑菌效果差,不能快速有效的抑菌。因此本发明提供一种抗菌防腐组合物在短时间和长期都有显著的抑菌效果。
发明内容
为了解决上述技术问题,本发明的第一个方面提供了一种含有胶态银的抗菌防腐组合物,按重量份计,包括胶态银,防腐成分和分散剂。所述胶态银,防腐成分和分散剂的重量比为(1-5):(3-8):(5-20)。
优选的,所述胶态银的制备原料包括银盐,还原剂和稳定剂。
优选的,所述银盐和稳定剂的重量比为(3-4):(6-7.5)。
优选的,所述胶态银的粒径为1-50nm。
优选的,所述防腐成分包括有机酸及其盐类防腐成分,醇类防腐成分,酚类防腐成分,酯类防腐成分,氯苯甘醚的至少一种。
优选的,所述酯类防腐成分包括尼泊金酯类防腐成分,甘油辛酸酯,碘丙炔醇丁基氨甲酸酯,山梨坦辛酸酯的一种或几种。
优选的,所述分散剂为聚乙烯吡咯烷酮。
优选的,所述聚乙烯吡咯烷酮的重均分子量为3500-1500000。
优选的,所述原料还包括抗菌剂和助剂。
本发明的第二个方面提供了一种含有胶态银的抗菌防腐组合物的制备方法,包括以下步骤:将防腐成分,分散剂,抗菌剂和助剂混合,加热到40-60℃,搅拌至溶解,然后加入胶态银,搅拌分散均匀,冷却出料即得抗菌防腐组合物。
有益效果:
1)本发明提供了一种含有胶态银的抗菌防腐组合物及其制备方法具有高效的抗菌效果,抗菌速度快,防腐效果好。
2)本发明提供了一种含有胶态银的抗菌防腐组合物及其制备方法稳定性好,广谱性高,对细菌,真菌,霉菌都具有抑菌效果。
3)本发明提供了一种含有胶态银的抗菌防腐组合物及其制备方法适用范围广泛,可应用于食品,医药,化妆品等行业领域,尤其是化妆品行业。
具体实施方式
为了解决上述问题,本发明提供了一种含有胶态银的抗菌防腐组合物,按重量份计,包括胶态银,防腐成分和分散剂。所述胶态银,防腐成分和分散剂的重量比为(1-5):(3-8):(5-20)。
胶态银
所述胶态银的粒径范围通常在1-100nm之间,由于其独特的表面效应等特殊性质,抗菌效果等性能极为优异,被人们广泛应用。优选的,所述胶态银的制备原料包括银盐,还原剂和稳定剂。
优选的,所述银盐为硝酸盐及其配合物。
优选的,所述还原剂包括水合肼,硼氢化钠,次亚磷酸钠,柠檬酸,维生素,甲醛,多元醇,双氧水的至少一种。
优选的,所述稳定剂包括十六烷基三甲基溴化铵,聚乙烯吡咯烷酮,聚乙二醇,聚丙二醇,聚醋酸乙烯酯,甲基纤维素,六偏磷酸钠,二(2-乙基)己基磺基琥珀酸钠的至少一种。
优选的,所述聚乙烯吡咯烷酮的重均分子量为30000-350000。
进一步优选的,所述银盐和稳定剂的重量比为(3-4):(6-7.5)。
优选的,所述胶态银的制备方法,包括以下步骤:将还原剂平均分为两份,一份与稳定剂搅拌混合均匀得到混合物A,另一份与银盐搅拌混合均匀得到混合物B。将混合物A加入至120-150℃后保持恒温,加入混合物B充分搅拌混合均匀,反应0.8-1.5h,冷却至常温。使用超声波超声分散10-20min,静置得到胶态银。
优选的,所述胶态银的粒径为1-50nm。
进一步优选的,所述胶态银的粒径为2-20nm。
防腐成分
所述防腐成分不仅能够起到防腐作用,还能与体系内的胶态银协同作用,增强菌防腐组合物的抗菌的广谱性。
优选的,所述防腐成分包括有机酸及其盐类防腐成分,醇类防腐成分,酚类防腐成分,酯类防腐成分的至少一种。
优选的,所述酯类防腐成分包括尼泊金酯类防腐成分,甘油辛酸酯,碘丙炔醇丁基氨甲酸酯,山梨坦辛酸酯的一种或几种。
在一种优选的实施方式中,所述防腐成分为为氯苯甘醚。
在一种优选的实施方式中,所述防腐成分包括有机酸及其盐类防腐成分和酯类防腐成分。所述有机酸及其盐类防腐成分和酯类防腐成分的重量比为(5-15):(2-7)。
优选的,所述有机酸及其盐类防腐成分为辛酰羟肟酸;所述酯类防腐成分为甘油辛酸酯。
在一种优选的实施方式中,所述防腐成分为尼泊金酯类防腐成分。
优选的,所述尼泊金酯类防腐成分包括尼泊金甲酯,尼泊金甲酯,尼泊金乙酯,尼泊金丙酯,尼泊金丁酯,尼泊金异丙酯,尼泊金异丁酯的至少两种。
优选的,所述防腐成分为尼泊金丁酯和尼泊金异丙酯。所述尼泊金丁酯和尼泊金异丙酯的重量比为(3-5):(2-4)。
分散剂
所述分散剂能够帮助体系内各物质分散均匀,防止团聚,增加体系的稳定性,帮助改善菌防腐组合物的抗菌性能。
优选的,所述分散剂为聚乙烯吡咯烷酮。
优选的,所述聚乙烯吡咯烷酮的重均分子量为3500-1500000。
进一步优选的,所述聚乙烯吡咯烷酮的重均分子量为40000-650000。
进一步优选的,所述聚乙烯吡咯烷酮的重均分子量为150000-600000。
优选的,所述一种含有胶态银的抗菌防腐组合物原料还包括抗菌剂和助剂。
优选的,所述抗菌剂包括壳聚糖,甲壳素,氨基酸类抗菌剂的至少一种。
优选的,所述壳聚糖为改性壳聚糖,所述改性壳聚糖为羧基化壳聚糖。
进一步优选的,所述羧基化壳聚糖的取代度≥60%,所述羧基化壳聚糖在20℃条件下的粘度为5-150mPa·s。
优选的,所述助剂包括多元醇类化合物,络合剂至少一种。
本发明所述多元醇类化合物不做限制,所述多元醇类化合物可以选自甘油,丙二醇,二丙丙二醇,丁二醇,山梨醇,葡萄糖,聚乙二醇,1,2-戊二醇,双甘油。
本发明所述络合剂不做限制,所述络合剂可以选自EDTA,EDTP等。
本发明的第二个方面提供了一种含有胶态银的抗菌防腐组合物的制备方法,包括以下步骤:将防腐成分,分散剂,抗菌剂和助剂混合,加热到40-60℃,搅拌至溶解,然后加入胶态银,搅拌分散均匀,冷却出料即得抗菌防腐组合物。
由于胶态银粒径小,比表面积高,在热力学上不稳定,容易发生团聚,导致制备的抗菌防腐组合物不够稳定。本发明意外研究发现当体系中加入特定分子量的聚乙烯吡咯烷酮可以增强体系中的稳定性,制备的防腐组合物具有更高的抗菌防腐效果。推测是由于聚乙烯吡咯烷酮是具有柔性链状结构的聚合物,加入后引起空间位阻效应,同时聚乙烯吡咯烷酮可以吸附胶态银表面,阻隔胶粒之间相互碰撞,防止团聚。同时特定分子量的聚乙烯吡咯烷酮亲水亲油性好,促进体系中防腐成分等物质混合均匀,使得胶态银与体系中防腐成分协同作用,不仅能够抑制细菌真菌等繁殖,对霉菌等也具有较好的杀菌效果,增强抗菌防腐组合物抗菌的广谱性。
下面通过实施例对本发明进行具体描述。有必要在此指出的是,以下实施例只用于对本发明作进一步说明,不能理解为对本发明保护范围的限制,该领域的专业技术人员根据上述本发明的内容做出的一些非本质的改进和调整,仍属于本发明的保护范围。
另外,如果没有其它说明,所用原料都是市售得到的。
实施例
实施例1
一种含有胶态银的抗菌防腐组合物,按重量份计,包括胶态银,防腐成分和分散剂。所述胶态银,防腐成分和分散剂的重量比为3:5:10。
所述胶态银的制备原料包括银盐,还原剂和稳定剂。
所述银盐为硝酸银。所述还原剂为乙二醇。所述稳定剂为聚乙烯吡咯烷酮。所述聚乙烯吡咯烷酮的重均分子量为152000。所述聚乙烯吡咯烷酮购自Gobekie公司,牌号:PVPK45。
所述银盐和稳定剂的重量比为3.5:6.5。
所述胶态银的制备方法,包括以下步骤:将200份还原剂平均分为两份,一份与0.65份稳定剂搅拌混合均匀得到混合物A,另一份与0.35份银盐搅拌混合均匀得到混合物B。将混合物A加入至130℃后保持恒温,加入混合物B充分搅拌混合均匀,反应1.2h,冷却至常温。使用超声波超声分散15min,静置得到胶态银。
所述胶态银的粒径为2-20nm。
所述防腐成分为尼泊金酯类防腐成分。所述防腐成分为尼泊金丁酯和尼泊金异丙酯。所述尼泊金丁酯(CAS号:94-26-8)和尼泊金异丙酯(CAS号:4191-73-5)的重量比为4:3。
所述分散剂为聚乙烯吡咯烷酮。所述聚乙烯吡咯烷酮的重均分子量为216000。所述聚乙烯吡咯烷酮购自Gobekie公司,牌号:PVPK60。
所述一种含有胶态银的抗菌防腐组合物原料还包括抗菌剂和助剂。所述抗菌剂为壳聚糖。所述壳聚糖为改性壳聚糖,所述改性壳聚糖为羧基化壳聚糖。所述羧基化壳聚糖的取代度约为80%,所述羧基化壳聚糖在20℃条件下的粘度为10-80mPa·s。所述壳聚糖购自南通飞宇生物科技有限公司,牌号:FY36191。
所述助剂为多元醇类化合物和络合剂。所述多元醇类化合物为甘油。所述络合剂为EDTA。
所述胶态银,抗菌剂,多元醇类化合物和络合剂的重量比为3:1:30:0.8。
一种含有胶态银的抗菌防腐组合物的制备方法,包括以下步骤:将防腐成分,分散剂,抗菌剂和助剂混合,加热到55℃,搅拌至溶解,然后加入胶态银,搅拌分散均匀,冷却出料即得抗菌防腐组合物。
实施例2
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于所述防腐成分包括有机酸及其盐类防腐成分和酯类防腐成分。所述有机酸及其盐类防腐成分和酯类防腐成分的重量比为8:5。所述有机酸及其盐类防腐成分为辛酰羟肟酸(CAS号:7377-3-9);所述酯类防腐成分为甘油辛酸酯(CAS号:26402-26-6)。
实施例3
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于所述防腐成分为氯苯甘醚(CAS号:104-29-0)。
实施例4
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于所述聚乙烯吡咯烷酮的重均分子量为37900。所述聚乙烯吡咯烷酮购自Gobekie公司,牌号:PVPK30。
实施例5
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于所述壳聚糖为未改性壳聚糖,所述壳聚糖购自山东奥康生物科技有限公司。
对比例1
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于所述银盐和稳定剂的重量比为3.5:1。
对比例2
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于所述聚乙烯吡咯烷酮的重均分子量为1760000。所述聚乙烯吡咯烷酮购自Gobekie公司,牌号:PVPK150。
对比例3
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于按重量份计,原料包括胶态银,分散剂,抗菌剂和助剂。所述胶态银和分散剂的重量比为3:10。所述胶态银,抗菌剂,多元醇类化合物和络合剂的重量比为3:1:30:0.8。
对比例4
一种含有胶态银的抗菌防腐组合物,具体实施方式同实施例1相同,不同之处在于按重量份计,原料包括防腐成分,分散剂,抗菌剂和助剂。所述防腐成分和分散剂的重量比为5:10。所述防腐成分,抗菌剂,多元醇类化合物和络合剂的重量比为10:1:30:0.8。
性能测试
1.抗菌防腐性测试:在37℃条件下进行采用抑菌圈法进行测试,测试菌种为金黄色葡萄球菌,白假丝酵母菌,黄曲霉;所述金黄色葡萄球菌和白假丝酵母菌菌种浓度均为5*106cfu/g,所述黄曲霉菌菌种浓度为3*104cfu/g,分别测试5min后的抑菌率,24h,7天,30天后的含菌量,设置三个平行试样,测试结果取平均值。
2.稳定性测试:将实施例及对比例制备的含有胶态银的抗菌防腐组合物放入离心机中,转速为2000r/min,离心30min,观察是否有沉淀分层现象。
表1金黄色葡萄球菌抗菌防腐性能测试结果
表2白假丝酵母菌抗菌防腐性能测试结果
表3黄曲霉抗菌防腐性能测试结果
表4稳定性测试结果
稳定性 | |
实施例1 | 无分层,无沉淀 |
实施例2 | 无分层,无沉淀 |
实施例3 | 无分层,无沉淀 |
实施例4 | 无分层,有沉淀 |
实施例5 | 无分层,无沉淀 |
对比例1 | 有分层,有沉淀 |
对比例2 | 无分层,有沉淀 |
对比例3 | 有分层,无沉淀 |
以上所述,仅是本发明的较佳实施例而已,并非是对发明作其他形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或更改为等同变化的等效实施例,但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改,等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (10)
1.一种含有胶态银的抗菌防腐组合物,其特征在于,按重量份计,包括胶态银,防腐成分和分散剂;所述胶态银,防腐成分和分散剂的重量比为(1-5):(3-8):(5-20)。
2.根据权利要求1所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述胶态银的制备原料包括银盐,还原剂和稳定剂。
3.根据权利要求2所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述银盐和稳定剂的重量比为(3-4):(6-7.5)。
4.根据权利要求1-3任一项所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述胶态银的粒径为1-50nm。
5.根据权利要求1所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述防腐成分包括有机酸及其盐类防腐成分,醇类防腐成分,酚类防腐成分,酯类防腐成分,氯苯甘醚的至少一种。
6.根据权利要求5所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述酯类防腐成分包括尼泊金酯类防腐成分,甘油辛酸酯,碘丙炔醇丁基氨甲酸酯,山梨坦辛酸酯的一种或几种。
7.根据权利要求1所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述分散剂为聚乙烯吡咯烷酮。
8.根据权利要求7所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述聚乙烯吡咯烷酮的重均分子量为3500-1500000。
9.根据权利要求1-8任一项所述的一种含有胶态银的抗菌防腐组合物,其特征在于,所述一种含有胶态银的抗菌防腐组合物原料还包括抗菌剂和助剂。
10.根据权利要求9所述的一种含有胶态银的抗菌防腐组合物的制备方法,其特征在于,包括以下步骤:将防腐成分,分散剂,抗菌剂和助剂混合,加热到40-60℃,搅拌至溶解,然后加入胶态银,搅拌分散均匀,冷却出料即得抗菌防腐组合物。
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