CN105012345B - 一种散射银离子化合物的制备方法 - Google Patents
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Abstract
本发明公开了一种散射银离子化合物的制备方法。银离子化合物是一类对细菌、病毒和真菌具有很好消杀作用的化学物质，对环境及人类安全。本发明公布了利用二级液态反应散射银离子化合物的技术，此方法合成的银离子散射分布，分散均匀，灭菌效果好，作用2分钟对大肠杆菌、白色念珠菌的杀菌率可达100%，作用10分钟对金黄色葡萄糖球菌的杀菌率可达100%；合成工艺环保简单，不需要精制，无废弃物，效率高。
Description
技术领域
本发明属于无机绿色化学合成领域，具体涉及一种合成散射银离子化合物的方法。
背景技术
在自然界中，有害细菌、真菌和病毒等是使人类传染、诱发疾病的重要原因。在公元14世纪中期引起欧洲三分之一人口死亡的黑死病和20世纪初致使全世界2000多万人死亡的流感。近年来随着人人类活动交流频繁，人口密度增大，不仅传统细菌引起病害增加，而且还出现了新的细菌引起流行病。《WHO》杂志1996年的统计数字表明，在1995年，全世界死亡5200万人，其中因细菌传染引起的死亡为1700万人，约占1/3。这些传染病包括霍乱、肺炎、疟疾、结核和肝炎等。
作为杀菌剂在2000年前即已为人所知，研究者根据实验对不同金属抗菌效能的相对效能进行了测定，抗菌能力为Ag>Hg>Cu>Cd>Ni>Co>Zn>Fe>Ca，银离子杀菌效能最高。
银离子杀菌剂被广泛应用于皮肤和粘膜组织的抗菌治疗过程，但是普遍存在银离子容易团聚、杀菌时间比较长的问题，降低了抗菌效果。中国专利申请CN101822850A、CN101062055A、CN104126611A等针对银离子团聚问题提出了解决方案，但是杀菌时间和效果有待提高。专利申请CN101062055A中测试了纳米银抗菌剂对大肠杆菌和白色念珠菌的杀菌效果，杀菌时间较长，作用10分钟时杀菌率在94%左右。中国专利申请CN10355225A中测试了银离子抗菌胶的杀菌效果，作用48小时后表面杀菌率才能达到99%。
发明内容
本发明提供一种银离子化合物的制备方法，其反应物处于完全溶解的液体状态，采用二级液态连续合成方式，得到散射银离子化合物。
本发明通过以下技术方案实现：
一种散射银离子化合物的制备方法，，包括如下步骤：
（1）按比例称取反应底物，纯水20份，硝酸银5-10份，散射剂10-20份，置入可调温反应釜，升温至60-90℃，保温25-30分钟；
（2）物料温度降至25-30℃，加入物料总体积3-4%的硝酸，物料总重量2-3%的聚乙二醇，电动搅拌30分钟，转速50-100r/s，得到散射银离子化合物。
步骤（1）中所述散射剂为聚萘甲醛磺酸钠盐溶液与过硫酸钠的聚溶物，按重量比为过硫酸钠2-5%，聚萘甲醛磺酸钠盐5-10%。
步骤（1）中所述纯水还为去离子水或蒸馏水。
所述的散射银离子化合物进行抗菌，用于对细菌、病毒和真菌的消杀。
本发明的有益效果：
（1）在本发明中，银离子在液态中散射分布，分布均匀，能够得到完全有效的利用；
（2）反应进行得更加充分，产物回收率高，合成高效，没有废弃物，有利于环保，是一种高效、经济和环境友好的绿色生产工艺；
（3）合成的散射银离子化合物无毒无刺激，杀菌迅速，对大肠杆菌、白色念珠菌作用2分钟的杀菌率可达100%，对金黄色葡萄糖球菌作用10分钟的杀菌率为100%。
具体实施方式
下面结合实施例对本发明做更进一步地解释，下列实施例仅用于说明本发明，但并不用来限定本发明的实施范围。
实施例1
称取反应底物蒸馏水20mL，硝酸银5克，散射剂10mL，散射剂中含有过硫酸钠2%wt，聚萘甲醛磺酸钠盐5%wt；于60℃保温30分钟；然后温度降至30℃，加入1mL硝酸，聚乙二醇 1克，搅拌30分钟，转速50r/s，得到散射银离子化合物。
实施例2
称取反应底物去离子水20mL，硝酸银8克，散射剂15mL，散射剂中含有过硫酸钠5%wt，聚萘甲醛磺酸钠盐10%wt；于80℃保温28分钟；温度降至25℃，加入1.5mL硝酸，聚乙二醇1克，30分钟搅拌，转速80r/s，得到散射银离子化合物。
实施例3
称取反应底物纯水20mL，硝酸银10克，散射剂20mL，散射剂中含有过硫酸钠3%wt，聚萘甲醛磺酸钠盐8%wt；于90℃保温25分钟；温度降至30℃，加入1.3mL硝酸，聚乙二醇 1.5克，30分钟搅拌，转速100r/s，得到散射银离子化合物。
实施例4
上述实施例制得的样品经江苏省疾病预防控中心检测，依据《一次性使用卫生用品卫生标准》GB15979-2002的标准对样品检测，其杀菌效果如表1 所示：作用2分钟对大肠杆菌和白色念珠菌均有消杀作用，灭菌率可达100%；对金黄色葡萄糖球菌的杀菌率为作用2分钟达到40.14%，作用10分钟达到100%。
依据卫生部《消毒技术规范》（2002年版）标准进行皮肤刺激、急性眼刺激、阴道粘膜刺激及口毒性试验。对家兔的皮肤刺激、急性眼刺激、阴道粘膜刺激结果为无刺激或极轻刺激性；对雌雄小鼠的口毒性试验结果为无毒。
表1 对试验菌杀菌效果
Claims (3)
1.一种散射银离子化合物的制备方法，其特征在于，包括如下步骤：
(1)按比例称取反应底物，纯水20份，硝酸银5-10份，散射剂10-20份，置入可调温反应釜，升温至60-90℃，保温25-30分钟；所述散射剂为聚萘甲醛磺酸钠盐溶液与过硫酸钠的聚溶物；
(2)物料温度降至25-30℃，加入物料总体积3-4％的硝酸，物料总重量2-3％的聚乙二醇，电动搅拌30分钟，转速50-100r/s，得到散射银离子化合物。
2.根据权利要求1所述的散射银离子化合物的制备方法，其特征在于，步骤(1)中所述聚萘甲醛磺酸钠盐溶液与过硫酸钠的聚溶物，按重量比为过硫酸钠2-5％，聚萘甲醛磺酸钠盐5-10％。
3.根据权利要求1所述的散射银离子化合物的制备方法，其特征在于，步骤(1)中所述纯水还为去离子水或蒸馏水。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101212905A (zh) * | 2005-06-30 | 2008-07-02 | 协和化学工业株式会社 | 包含含有银的铝硫酸盐氢氧化物粒子的抗菌剂及其用途 |
| CN104706668A (zh) * | 2015-04-02 | 2015-06-17 | 苏州泰利三佳纳米科技有限公司 | 含银离子的女性护理液及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101212905A (zh) * | 2005-06-30 | 2008-07-02 | 协和化学工业株式会社 | 包含含有银的铝硫酸盐氢氧化物粒子的抗菌剂及其用途 |
| CN104706668A (zh) * | 2015-04-02 | 2015-06-17 | 苏州泰利三佳纳米科技有限公司 | 含银离子的女性护理液及其制备方法 |
Non-Patent Citations (1)
| Title |
|---|
| 银离子注入热解碳的抗菌性研究;唐慧琴等;《真空科学与技术学报》;20060331;第26卷(第2期);第93页第1段至第94页第2段 * |
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Effective date of registration: 20191118 Address after: Park Road in Jiangning District of Nanjing city and Jiangsu province 210000 No. 18 Patentee after: Nanjing Sanjia silver biological medicine science and Technology Co.,Ltd. Address before: 210032, Jiangsu province Nanjing hi tech Development Zone, Spark Road 10, ding industry, 100 Thai biological building C block 501-1 room Patentee before: Li Yuanping |
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Effective date of registration: 20240422 Address after: Building 3, 3rd Floor, No. 1-1 Fengshan Road, Medical Device Industry Park, Gaochun District, Nanjing City, Jiangsu Province, 211300 Patentee after: Nanjing Bangshiyin Pharmaceutical Co.,Ltd. Country or region after: China Address before: No.18, Zhilan Road, Science Park, Jiangning District, Nanjing City, Jiangsu Province, 210000 Patentee before: Nanjing Sanjia silver biological medicine science and Technology Co.,Ltd. Country or region before: China |