CN105994346A - 一种稀土负载抗菌剂的制备方法 - Google Patents
一种稀土负载抗菌剂的制备方法 Download PDFInfo
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- 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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Abstract
本发明涉及一种稀土负载抗菌剂的制备方法,将一定量的Q高流速琼脂糖微球分散到乙醇中,加入双(五甲基钴环戊二烯),1‑烯丙基‑3‑甲基氯化咪唑,进行聚合反应,即得到经表面聚合的含稀土的Q高流速琼脂糖微球微悬浮液产品。
Description
技术领域
本发明涉及一种抗菌剂的制备方法,尤其是一种稀土负载抗菌剂的制备方法。
背景技术
稀土元素及其化合物有很好的抗炎、杀菌、抗癌、抗凝血、镇痛作用。杂环化合物是一类具有广泛的生物活性的化合物,许多杂环化合物具有杀菌、消炎、抗病毒等生物活性,因而备受关注。杂环化合物与金属离子形成配合物之后,由于协同效应,金属配合物的抗菌作用将会增强。相关研究表明,与许多有机合成药物相比,稀土配合物的毒性更低,同时通过口服或外用稀土配合物未发现体内积累,因此具有更广泛的应用
CN103053602A本发明公开的是一种新型功能稀土抗菌剂,采用回流冷凝法、低温固相法、微波合成等技术创新合成了一系列稀土功能配合物;然后通过UV、FT-IR、ICP、EA、TG-DTA、XPS、XRD、TEM等方法对产物进行表征;表征完成后,依次采用平板抑菌圈法、MIC法考察所制备配合物的抗菌活性,最后采用循环伏安法、紫外光谱法、凝胶电泳法探究配合物与DNA作用的机理。从分子水平得出抗菌的本质,从而筛选出能作为复合抗菌剂的稀土功能配合物。
CN101176468B公开了一种含锌-稀土的无机复合抗菌剂及其制备方法和应用,该抗菌剂是以天然的或化学合成的离子交换材料为载体,通过离子交换法负载锌离子和稀土离子双活性中心,锌离子的含量为6.0~8.0wt%,稀土离子的含量为2.0~4.0wt%。该抗菌剂是通过液相或固相离子交换法将锌离子和稀土离子交换至载体中,然后经过后处理制得无机复合抗菌剂。该抗菌剂由于含有可产生协同效应的锌离子和稀土离子双抗菌活性中心,故其抗菌谱广、抗菌效率较高,并且具有耐热性和耐光性优良、颜色稳定、成本低的特点,是载银无机抗菌剂的理想替代品,可添加在塑料、橡胶、纤维、涂料、胶粘剂、纸张或陶瓷等材料中制备抗菌功能材料。
现有公知技术制备的稀土抗菌剂,均为离子交换或复配,稀土元素分部不均匀,容易流失,抗菌防霉性能不稳定。
发明内容
针对现有技术的不足,本发明提供了一种稀土负载抗菌剂的制备方法。
本发明提供一种稀土负载抗菌剂的制备方法,其制备方法通过以下步骤实现:
将一定量的Q高流速琼脂糖微球分散到乙醇中,按下述比例加入双(五甲基钴环戊二烯),1-烯丙基-3-甲基氯化咪唑,过氧化苯甲酰和聚乙烯醇、十二烷基苯磺酸钠等,升温,在60-80℃反应6-15小时,即得到经表面聚合的含稀土的Q高流速琼脂糖微球微悬浮液产品。
组分 重量份
Q高流速琼脂糖微球 5-15
双(三羰基环戊二烯钼) 1-3
1-烯丙基-3-甲基氯化咪唑 0.1-0.5
过氧化苯甲酰 0.01-0.05
聚乙烯醇 0.1-0.5
十二烷基苯磺酸钠 0.1-0.5
乙醇 200
所述的Q高流速琼脂糖微球为市售产品,如西安蓝晓科技新材料股份有限公司研制的产品。所述的1-烯丙基-3-甲基氯化咪唑为市售产品,如上海宝曼生物科技有限公司生产的产品。所述的双(三羰基环戊二烯钼)为市售产品。
本发明的有益效果:
Q高流速琼脂糖微球为载体,稀土元素包覆在抗菌剂表面,不容易流失,抗菌效果稳定,提高了制品的抗菌防霉性能;1-烯丙基-3-甲基氯化咪唑离子液体所带咪唑官能团也提高了抑菌效果。
具体实施方式
以下实施例仅仅是进一步说明本发明,并不是限制本发明保护的范围。
实施例1
在500L反应釜中,按下列配比加入Q高流速琼脂糖微球分散到乙醇中,按下述比例加入双(三羰基环戊二烯钼),1-烯丙基-3-甲基氯化咪唑,过氧化苯甲酰和聚乙烯醇、十二烷基苯磺酸钠等,升温,在80℃反应6小时,即得到经表面聚合的含稀土的Q高流速琼脂糖微球微悬浮液产品,编号为M-1。
组分 Kg
Q高流速琼脂糖微球 10
双(三羰基环戊二烯钼) 2
1-烯丙基-3-甲基氯化咪唑 0.3
过氧化苯甲酰 0.02
聚乙烯醇 0.2
十二烷基苯磺酸钠 0.2
乙醇 200
实施例2
在500L反应釜中,按下列配比加入Q高流速琼脂糖微球分散到乙醇中,按下述比例加入双(三羰基环戊二烯钼),1-烯丙基-3-甲基氯化咪唑,过氧化苯甲酰和聚乙烯醇、十二烷基苯磺酸钠等,升温,在70℃反应10小时,即得到经表面聚合的含稀土的Q高流速琼脂糖微球微悬浮液产品,编号为M-2。
组分 Kg
Q高流速琼脂糖微球 5
双(三羰基环戊二烯钼) 1
1-烯丙基-3-甲基氯化咪唑 0.1
过氧化苯甲酰 0.01
聚乙烯醇 0.1
十二烷基苯磺酸钠 0.1
乙醇 200
实施例3
在500L反应釜中,按下列配比加入Q高流速琼脂糖微球分散到乙醇中,按下述比例加入双(三羰基环戊二烯钼),1-烯丙基-3-甲基氯化咪唑,过氧化苯甲酰和聚乙烯醇、十二烷基苯磺酸钠等,升温,在60℃反应15小时,即得到经表面聚合的含稀土的Q高流速琼脂糖微球微悬浮液产品,编号为M-3
组分 Kg
Q高流速琼脂糖微球 15
双(三羰基环戊二烯钼) 3
1-烯丙基-3-甲基氯化咪唑 0.5
过氧化苯甲酰 0.05
聚乙烯醇 0.5
十二烷基苯磺酸钠 0.5
乙醇 200
比较例1
双(三羰基环戊二烯钼)不加入,其它同实施例1。所得产品编号为M-4。
比较例2
1-烯丙基-3-甲基氯化咪唑不加入,其它同实施例1。所得产品编号为M-5。
比较例3
1-烯丙基-3-甲基氯化咪唑,双(三羰基环戊二烯钼)不加入,其它同实施例1。所得产品编号为M-6。
实施例1-3以及对比例1-4得到的稀土抗菌剂用于皮革涂饰,按照QBT 4199-2011皮革 防霉性能测试方法检测抗菌防霉性能。见表1:
表1:不同工艺做出的试验样品抗菌防霉性能的比较
编号 | 抑菌带宽度/mm | 试样下面细菌繁殖情况 |
M-1 | >1 | 无 |
M-2 | >1 | 无 |
M-3 | >1 | 无 |
M-4 | 0 | 轻微 |
M-5 | 0-1 | 无 |
M-6 | 0 | 中等 |
以上仅为本发明的具体实施例,但本发明的技术特征并不局限于此。任何以本发明为基础,为解决基本相同的技术问题,实现基本相同的技术效果,所作出的简单变化、等同替换或者修饰等,皆涵盖于本发明的保护范围之中。
Claims (2)
1.一种稀土负载抗菌剂的制备方法,其特征在于稀土负载抗菌剂由以下组份组成:
组分 重量份
Q高流速琼脂糖微球 5-15
双(三羰基环戊二烯钼) 1-3
1-烯丙基-3-甲基氯化咪唑 0.1-0.5
过氧化苯甲酰 0.01-0.05
聚乙烯醇 0.1-0.5
十二烷基苯磺酸钠 0.1-0.5
乙醇 200。
2.一种稀土负载抗菌剂的制备方法,其特征在于包括以下步骤:
将Q高流速琼脂糖微球分散到乙醇中,加入双(五甲基钴环戊二烯),1-烯丙基-3-甲基氯化咪唑,过氧化苯甲酰和聚乙烯醇、十二烷基苯磺酸钠,升温,在60-80℃反应6-15小时,即得到经表面聚合的含稀土的Q高流速琼脂糖微球微悬浮液产品。
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CN107258828A (zh) * | 2017-06-21 | 2017-10-20 | 芜湖蓝天工程塑胶有限公司 | 复合抗菌纤维素保鲜盒及其制备方法 |
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CN116251223B (zh) * | 2023-05-09 | 2023-08-01 | 天津包钢稀土研究院有限责任公司 | 一种用于伤口表面杀菌的稀土金属基敷料及其制备方法 |
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CN107258828A (zh) * | 2017-06-21 | 2017-10-20 | 芜湖蓝天工程塑胶有限公司 | 复合抗菌纤维素保鲜盒及其制备方法 |
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