CN111744059A - 一种可粘膜下注射的稳定性磁性材料制备方法 - Google Patents
一种可粘膜下注射的稳定性磁性材料制备方法 Download PDFInfo
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Abstract
本发明公开的属于医学材料制备技术领域,具体为一种可粘膜下注射的稳定性磁性材料制备方法,包括以下步骤:S1:以石墨粉为原料采取Hummers法获得石墨烯;S2:置于DEG溶液后经超声处理获得石墨稀溶液;该种可粘膜下注射的稳定性磁性材料制备方法,通过提取出具备强磁性能、高稳定性的石墨烯‑四氧化三铁纳米复合体材料,具备高稳定性、不易被生物降解、生物安全性,用于制备粘膜下注射材料可以在复杂的ESD/EMR操作、外科手术术前内镜标记定位乃至长期定位标记、追踪病灶等需要长黏膜***维持时间的临床应用场景中发挥关键的作用,而且这一高稳定性的石墨烯‑四氧化三铁复合体材料在多领域开阔出更广泛的应用。
Description
技术领域
本发明涉及医学材料制备技术领域,具体为一种可粘膜下注射的稳定性磁性材料制备方法。
背景技术
微创顾名思义就是微小的创口、创伤,是现代医学外科手术治疗应用的特点,是一个技术名词,就是在手术治疗过程中只对患者造成微小创伤、术后只留下微小创口的技术,微创相对于传统手术,具有切口小、创伤小、恢复快、痛苦少的特点,是手术发展的方向之一。
在提倡微创化诊疗的新医疗时代,消化内镜下的诊疗技术包括ESD、EMR以及新兴的术中内镜定位标记等技术都在临床上应用的越来越广泛和成熟。ESD、EMR等技术成功的一个关键在于粘膜下注射材料的应用,内镜下黏膜下注射通过将黏膜层与固有肌层分离以助于完整剥离病灶,还可以提高内镜操作的安全性。目前常用的粘膜下注射材料包括有生理盐水、透明质酸、海藻酸钠等,而可黏膜下注射的磁性材料也在逐步的研发和应用当中。
内镜下粘膜下注射材料的稳定性、粘滞性对于分离病灶极为关键,目前研发可粘膜下注射的磁性材料的重点也在于提高其在组织内的稳定性。
但无论是磁流体还是磁性水凝胶都未取得足够满意的黏膜抬举维持效果,稳定性差,易被降解,标记效果难以长期定位,对于面对追踪病灶需要长黏膜***维持时间的周期性不足,不利于提高材料的运用效果和多领域的应用开发。
发明内容
本发明的目的在于提供一种可粘膜下注射的稳定性磁性材料制备方法,以解决上述背景技术中提出的现有的无论是磁流体还是磁性水凝胶都未取得足够满意的黏膜抬举维持效果,稳定性差,易被降解,标记效果难以长期定位,对于面对追踪病灶需要长黏膜***维持时间的周期性不足,不利于提高材料的运用效果和多领域的应用开发的问题。
为实现上述目的,本发明提供如下技术方案:一种可粘膜下注射的稳定性磁性材料制备方法,包括以下步骤:
S1:以石墨粉为原料采取Hummers法获得石墨烯;
S2:置于DEG溶液后经超声处理获得石墨稀溶液;
S3:在石墨烯纳米片上原位生成的纳米四氧化三铁颗粒由Fe3+和Fe2+,摩尔比为1.5:1的FeCl3溶液和FeSO4·7H2O制备;
S4:将上述三种溶液在超声下处理,加入NaOH后,超声处理时间为15min~20min,并产生黑色沉淀;
S5:将该黑色沉淀于40℃~65℃下水浴15min~30min,获得含石墨烯-四氧化三铁纳米复合体的混合物;
S6:将该混合物经去离子水和乙醇反复洗涤3次~5次,获得纯化的石墨烯-四氧化三铁纳米复合体。
优选的,所述石墨粉的粒度小于15μm~30μm的粒子,含量大于80%~95%,碳含量97%~99.85%。
优选的,所述水浴中需装配和反应瓶,反应瓶的容量为150ml~250ml,且所述反应瓶中加入浓硫酸,控制反应温度不超过15℃~20℃,搅拌5min~8min后升温至30℃~40℃。
优选的,所述去离子水和所述乙醇的混合比例为3:0.5~3:1.5。
与现有技术相比,本发明的有益效果是:该种可粘膜下注射的稳定性磁性材料制备方法,通过在制备的石墨烯纳米片上进行化学反应原位生成四氧化三铁纳米颗粒,从而提取出具备强磁性能、高稳定性的石墨烯-四氧化三铁纳米复合体材料,具备高稳定性、不易被生物降解、生物安全性,用于制备粘膜下注射材料可以在复杂的ESD/EMR操作、外科手术术前内镜标记定位乃至长期定位标记、追踪病灶等需要长黏膜***维持时间的临床应用场景中发挥关键的作用,而且这一高稳定性的石墨烯-四氧化三铁复合体材料可以在工业等多领域开阔出更广泛的应用。
附图说明
图1为本发明制备流程示意图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明提供一种技术方案:一种可粘膜下注射的稳定性磁性材料制备方法,包括以下步骤:
S1:以石墨粉为原料采取Hummers法获得石墨烯;
S2:置于DEG溶液后经超声处理获得石墨稀溶液;
S3:在石墨烯纳米片上原位生成的纳米四氧化三铁颗粒由Fe3+和Fe2+,摩尔比为1.5:1的FeCl3溶液和FeSO4·7H2O制备;
S4:将上述三种溶液在超声下处理,加入NaOH后,超声处理时间为15min~20min,并产生黑色沉淀;
S5:将该黑色沉淀于40℃~65℃下水浴15min~30min,获得含石墨烯-四氧化三铁纳米复合体的混合物;
S6:将该混合物经去离子水和乙醇反复洗涤3次~5次,获得纯化的石墨烯-四氧化三铁纳米复合体。
其中,石墨粉的粒度小于15μm~30μm的粒子,含量大于80%~95%,碳含量97%~99.85%;水浴中需装配和反应瓶,反应瓶的容量为150ml~250ml,且反应瓶中加入浓硫酸,控制反应温度不超过15℃~20℃,搅拌5min~8min后升温至30℃~40℃;去离子水和乙醇的混合比例为3:0.5~3:1.5。
实施例1
一种可粘膜下注射的稳定性磁性材料制备方法,包括以下步骤:
S1:以石墨粉为原料采取Hummers法获得石墨烯;
S2:置于DEG溶液后经超声处理获得石墨稀溶液;
S3:在石墨烯纳米片上原位生成的纳米四氧化三铁颗粒由Fe3+和Fe2+,摩尔比为1.5:1的FeCl3溶液和FeSO4·7H2O制备;
S4:将上述三种溶液在超声下处理,加入NaOH后,超声处理时间为15min,并产生黑色沉淀;
S5:将该黑色沉淀于40℃下水浴15min,获得含石墨烯-四氧化三铁纳米复合体的混合物;
S6:将该混合物经去离子水和乙醇反复洗涤3次,获得纯化的石墨烯-四氧化三铁纳米复合体。
其中,石墨粉的粒度小于15μm的粒子,含量大于80%,碳含量97%;水浴中需装配和反应瓶,反应瓶的容量为150ml,且反应瓶中加入浓硫酸,控制反应温度不超过15℃,搅拌5min后升温至30℃;去离子水和乙醇的混合比例为3:0.5。
实施例2
S1:以石墨粉为原料采取Hummers法获得石墨烯;
S2:置于DEG溶液后经超声处理获得石墨稀溶液;
S3:在石墨烯纳米片上原位生成的纳米四氧化三铁颗粒由Fe3+和Fe2+,摩尔比为1.5:1的FeCl3溶液和FeSO4·7H2O制备;
S4:将上述三种溶液在超声下处理,加入NaOH后,超声处理时间为20min,并产生黑色沉淀;
S5:将该黑色沉淀于65℃下水浴30min,获得含石墨烯-四氧化三铁纳米复合体的混合物;
S6:将该混合物经去离子水和乙醇反复洗涤5次,获得纯化的石墨烯-四氧化三铁纳米复合体。
其中,石墨粉的粒度小于30μm的粒子,含量大于95%,碳含量99.85%;水浴中需装配和反应瓶,反应瓶的容量为250ml,且反应瓶中加入浓硫酸,控制反应温度不超过20℃,搅拌8min后升温至40℃;去离子水和乙醇的混合比例为3:1.5。
实施例3
S1:以石墨粉为原料采取Hummers法获得石墨烯;
S2:置于DEG溶液后经超声处理获得石墨稀溶液;
S3:在石墨烯纳米片上原位生成的纳米四氧化三铁颗粒由Fe3+和Fe2+,摩尔比为1.5:1的FeCl3溶液和FeSO4·7H2O制备;
S4:将上述三种溶液在超声下处理,加入NaOH后,超声处理时间为18min,并产生黑色沉淀;
S5:将该黑色沉淀于50℃下水浴20min,获得含石墨烯-四氧化三铁纳米复合体的混合物;
S6:将该混合物经去离子水和乙醇反复洗涤4次,获得纯化的石墨烯-四氧化三铁纳米复合体。
其中,石墨粉的粒度小于20μm的粒子,含量大于90%,碳含量99%;水浴中需装配和反应瓶,反应瓶的容量为200ml,且反应瓶中加入浓硫酸,控制反应温度不超过18℃,搅拌6min后升温至35℃;去离子水和乙醇的混合比例为3:0.8。
实施例4
S1:以石墨粉为原料采取Hummers法获得石墨烯;
S2:置于DEG溶液后经超声处理获得石墨稀溶液;
S3:在石墨烯纳米片上原位生成的纳米四氧化三铁颗粒由Fe3+和Fe2+,摩尔比为1.5:1的FeCl3溶液和FeSO4·7H2O制备;
S4:将上述三种溶液在超声下处理,加入NaOH后,超声处理时间为17min,并产生黑色沉淀;
S5:将该黑色沉淀于55℃下水浴25min,获得含石墨烯-四氧化三铁纳米复合体的混合物;
S6:将该混合物经去离子水和乙醇反复洗涤4次,获得纯化的石墨烯-四氧化三铁纳米复合体。
其中,石墨粉的粒度小于26μm的粒子,含量大于93%,碳含量98%;水浴中需装配和反应瓶,反应瓶的容量为180ml,且反应瓶中加入浓硫酸,控制反应温度不超过15℃,搅拌6min后升温至35℃;去离子水和乙醇的混合比例为3:1。
综合以上所述,该种可粘膜下注射的稳定性磁性材料制备方法,通过在制备的石墨烯纳米片上进行化学反应原位生成四氧化三铁纳米颗粒,从而提取出具备强磁性能、高稳定性的石墨烯-四氧化三铁纳米复合体材料,具备高稳定性、不易被生物降解、生物安全性,用于制备粘膜下注射材料可以在复杂的ESD/EMR操作、外科手术术前内镜标记定位乃至长期定位标记、追踪病灶等需要长黏膜***维持时间的临床应用场景中发挥关键的作用,而且这一高稳定性的石墨烯-四氧化三铁复合体材料可以在工业等多领域开阔出更广泛的应用。
虽然在上文中已经参考实施例对本发明进行了描述,然而在不脱离本发明的范围的情况下,可以对其进行各种改进并且可以用等效物替换其中的部件。尤其是,只要不存在结构冲突,本发明所披露的实施例中的各项特征均可通过任意方式相互结合起来使用,在本说明书中未对这些组合的情况进行穷举性的描述仅仅是出于省略篇幅和节约资源的考虑。因此,本发明并不局限于文中公开的特定实施例,而是包括落入权利要求的范围内的所有技术方案。
Claims (4)
1.一种可粘膜下注射的稳定性磁性材料制备方法,其特征在于:包括以下步骤:
S1:以石墨粉为原料采取Hummers法获得石墨烯;
S2:置于DEG溶液后经超声处理获得石墨稀溶液;
S3:在石墨烯纳米片上原位生成的纳米四氧化三铁颗粒由Fe3+和Fe2+,摩尔比为1.5:1的FeCl3溶液和FeSO4·7H2O制备;
S4:将上述三种溶液在超声下处理,加入NaOH后,超声处理时间为15min~20min,并产生黑色沉淀;
S5:将该黑色沉淀于40℃~65℃下水浴15min~30min,获得含石墨烯-四氧化三铁纳米复合体的混合物;
S6:将该混合物经去离子水和乙醇反复洗涤3次~5次,获得纯化的石墨烯-四氧化三铁纳米复合体。
2.根据权利要求1所述的一种可粘膜下注射的稳定性磁性材料制备方法,其特征在于:所述石墨粉的粒度小于15μm~30μm的粒子,含量大于80%~95%,碳含量97%~99.85%。
3.根据权利要求1所述的一种可粘膜下注射的稳定性磁性材料制备方法,其特征在于:所述水浴中需装配和反应瓶,反应瓶的容量为150ml~250ml,且所述反应瓶中加入浓硫酸,控制反应温度不超过15℃~20℃,搅拌5min~8min后升温至30℃~40℃。
4.根据权利要求1所述的一种可粘膜下注射的稳定性磁性材料制备方法,其特征在于:所述去离子水和所述乙醇的混合比例为3:0.5~3:1.5。
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