CN115535984A - 一种立方体磷酸锆载体及其载锌或载银的抗菌粉的制备方法 - Google Patents
一种立方体磷酸锆载体及其载锌或载银的抗菌粉的制备方法 Download PDFInfo
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Abstract
一种立方体磷酸锆载体的制备方法,包括以下步骤:S1、称取200kg氧氯化锆,并将其加入45kg去离子水中溶解,称取13.3kg磷酸二氢钠,并将其加入45kg去离子水溶解;S2、将上述两组溶液进行混合,得到磷酸锆载体溶胶;综上所述,载体的制备采用常压水热合成法,本发明选取磷酸盐型载体,其中磷酸盐载体具有较多的、可被阳离子所占有的活性位点,其多孔的结构具有很强的离子交换能力,对银离子具有很强的选择吸附性,且有很大的比表面积,是良好的银离子交换载体。
Description
技术领域
本发明属于化学合成技术领域,具体涉及一种立方体磷酸锆载体及其载锌或载银的抗菌粉的制备方法。
背景技术
人类所处的环境周围存在着大量有益或是有害的微生物,它们与人类赖以生存的环境息息相关,微生物可以被人们用来发酵食品饮料,同时人们也时刻受到微生物的威胁。调查显示,有害微生物感染是全球第二大使人类致病的杀手。世界卫生组织数据表明,每年由于细菌感染致死的人数已经超过1700万。人们在平常生活中都会接触到一些传染病病菌,如疟疾、肺炎、霍乱、结核等,而生活中最常用的毛巾就能传播皮肤病、红眼病、感冒、肺结核等常见的疾病。致病微生物己成为人们健康的主要威胁之一。
抗菌剂的合成制备由来已久,二十世纪初便出现了由人工合成的有机类抗菌剂,之后又出现了酒精、乙酸作抗菌剂,后来人们又把银、铜等无机物用作杀菌剂。现阶段,对抗菌剂的要求如下:(a)抗菌性能优良、广谱抗菌;(b)持久抗菌,耐洗涤、使用周期长;(c)稳定性好,耐酸碱、耐日照、耐热等不宜变质失效;(d)添加抗菌剂后的材料易于加工,既与基材有较好的亲和力、又不使其发生颜色变化、对基材产品的美感或使用价值没有任何损害;(e)安全无毒,对环境友好;(f)不易使细菌产生耐药性。
发明内容
本发明旨在提供一种立方体磷酸锆载体及其载锌或载银的抗菌粉的制备方法。
为解决上述技术问题,本发明采用以下技术方案:一种立方体磷酸锆载体的制备方法,包括以下步骤:
S1、称取200kg氧氯化锆,并将其加入45kg去离子水中溶解,称取13.3kg磷酸二氢钠,并将其加入45kg去离子水溶解;
S2、将上述两组溶液进行混合,得到磷酸锆载体溶胶;
S3、将所述磷酸锆载体溶胶、模板剂溶于去离子水并在反应釜中充分混合反应,即得磷酸锆载体;
S4、通过板框式滤布压滤机不断循环压制磷酸锆载体,将载体压实;
S5、将压实后的磷酸锆载体用去离子水反复冲洗干净,即制成磷酸锆载体滤饼。
步骤S3中,所述模板剂为草酸钠,所述反应压力为常压,反应温度控制在90-110℃,反应时间控制在24h-48h,草酸钠加入量为3.8kg,去离子水加入量为80kg。
一种立方体磷酸锆载锌的制备方法,包括以下步骤:
在酸性介质中,将步骤A3制得的100kg磷酸锆载体溶解于200kg的去离子水,称取50kg一水硝酸锌,加入100kg去离子水溶解,制成一水硝酸锌水溶液,然后将磷酸锆载体溶解液分散在40-50%浓度的一水硝酸锌水溶液中,在90-100℃温度下恒温混合搅拌3-5小时,过滤可制得含锌离子浓度为4-5%的立方体磷酸锆载锌。
一种立方体磷酸锆载银的制备方法,包括以下步骤:
将上述制得的立方体磷酸锆载锌用去离子水配制成6-10%的水分散液,在酸性介质中加入已定量溶解的硝酸银溶液,其中硝酸银溶液由3kg硝酸银溶解于10kg去离子水中配制而成,在60-90℃温度下恒温2-4h,洗涤过滤后制得立方体磷酸锆载银无机抗菌粉的半成品;
然后将上述立方体磷酸锆载银无机抗菌粉的半成品在烘干机中烘干,烘干温度控制在130-150℃,控制粉体含水率在5-8%,取出后利用机器进行锤粉破碎,再将其送入煅烧窑炉中进行高温定型,控制温度在700-900℃,控制时间5-8小时,待冷却至40-60℃后进行气流粉碎,打开团聚体,即制得立方体磷酸锆载银抗菌粉成品。
与现有技术相比,本发明的有益效果是:本发明选取磷酸盐型载体,其中磷酸盐载体具有较多的、可被阳离子所占有的活性位点,其多孔的结构具有很强的离子交换能力,对银离子具有很强的选择吸附性,且有很大的比表面积,是良好的银离子交换载体。通过离子交换,制得银型抗菌剂的载银量较大,且银离子在其晶体结构中能够稳定存在,并且以很小的速度释放,因此以该材料为载体制备的抗菌剂具有持久的抗菌活。
用水热法制得的磷酸锆载体,通过与银离子发生离子交换制得含银量为3wt%的抗菌剂。该抗菌剂放入水中浸泡5天时间,用ICP测定水溶液中银离子的含量,结果显示,此抗菌剂银离子的溶出量不到1微克,因而以磷酸锆为载体的抗菌剂具有较好的银离子缓释效果。对该材料进行大肠杆菌和金黄细菌抗菌测试,结果显示,含有0.005wt%载银磷酸锆溶液能在6h内完全杀灭大肠杆菌和金黄色葡萄球菌,且在48h之后,也没有细菌存活;该研究证明了此抗菌材料不仅抗菌效果优良,而且具有银离子缓释性能,因此该抗菌材料具有抗菌持久性。
附图说明
附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。在附图中:
图1为立方体磷酸锆载体的粒径正态分布图;
图2为立方体磷酸锆载银抗菌粉的粒径正态分布图;
图3为立方体磷酸锆载银抗菌粉的扫描电镜图,在图3中,标尺为100nm;
图4为立方体磷酸锆载银抗菌粉的扫描电镜图,在图4中,标尺为0.2μm。
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。
以下结合实施例对本发明作进一步的详细描述。
1、磷酸盐载体的制备
磷酸盐纳米颗粒作为复合材料的载体,在实际应用中,需要找到一种快速和简单的合成方法,同时制备过程应该具有产率髙和环境影响小的特点。制备磷酸锆(ZrP)是通过ZrOCl2与H3PO4的混合溶液反应,得到具有不同的结晶度和不同的粒径ZrP。
一种立方体磷酸锆载体的制备方法,包括以下步骤:
S1、称取200kg氧氯化锆,并将其加入45kg去离子水中溶解,称取13.3kg磷酸二氢钠,并将其加入45kg去离子水溶解;
S2、将上述两组溶液进行混合,得到磷酸锆载体溶胶;
S3、将所述磷酸锆载体溶胶、模板剂溶于去离子水并在反应釜中充分混合反应,即得磷酸锆载体;
S4、通过板框式滤布压滤机不断循环压制磷酸锆载体,将载体压实;
S5、将压实后的磷酸锆载体用去离子水反复冲洗干净,即制成磷酸锆载体滤饼。
步骤S3中,所述模板剂为草酸钠,所述反应压力为常压,反应温度控制在90-110℃,反应时间控制在24h-48h,草酸钠加入量为3.8kg,去离子水加入量为80kg。
2、载银磷酸盐的制备
磷酸盐(如磷酸锆)因其结构十分稳定,结构内部存在很多空隙、孔洞等比较大的空间,起电价平衡作用的钾、钠、钙等一些金属离子存在于这些空间中。将银的硝酸盐溶液或者其他化合物溶液与载体充分混合,制成悬液,体系中的钠、钾、钙便能被银离子通过离子交换的方式替换出来。其中较为简便的方法是浸啧交换法。
浸溃交换法是用水或有机溶剂作分散液,将磷酸盐粉末分散成悬浮液,再按一定比例将待交换的银盐溶液加入到无机化合物载体的悬浮液中,在一定温度下,均匀搅拌一定时间,通过不断的搅拌来使离子交换反应快速进行。离子交换完成后经过滤、洗涤,烘干即可制得载银抗菌剂样品。该方法要求载体是不可溶的,并能在溶剂中稳定存在,同时又要在水或有机溶剂中能很好地分散,这就要求载体有足够小的粒度。通过离子交换法制备的载银抗菌剂具有较理想的载银量,同时又可以在载体间载入大分子有机化合物。
一种立方体磷酸锆载锌的制备方法,包括以下步骤:
在酸性介质中,将步骤A3制得的100kg磷酸锆载体溶解于200kg的去离子水,称取50kg一水硝酸锌,加入100kg去离子水溶解,制成一水硝酸锌水溶液,然后将磷酸锆载体溶解液分散在40-50%浓度的一水硝酸锌水溶液中,在90-100℃温度下恒温混合搅拌3-5小时,过滤可制得含锌离子浓度为4-5%的立方体磷酸锆载锌。
一种立方体磷酸锆载银的制备方法,包括以下步骤:
将上述制得的立方体磷酸锆载锌用去离子水配制成6-10%的水分散液,在酸性介质中加入已定量溶解的硝酸银溶液,其中硝酸银溶液由3kg硝酸银溶解于10kg去离子水中配制而成,在60-90℃温度下恒温2-4h,洗涤过滤后制得立方体磷酸锆载银无机抗菌粉的半成品;
然后将上述立方体磷酸锆载银无机抗菌粉的半成品在烘干机中烘干,烘干温度控制在130-150℃,控制粉体含水率在5-8%,取出后利用机器进行锤粉破碎,再将其送入煅烧窑炉中进行高温定型,控制温度在700-900℃,控制时间5-8小时,待冷却至40-60℃后进行气流粉碎,打开团聚体,即制得立方体磷酸锆载银抗菌粉成品。
图1给出本发明实施例制得的立方体磷酸锆载体的粒径正态分布图;
图2给出本发明实施例制得的立方体磷酸锆载银抗菌粉的粒径正态分布图;
图3给出给出本发明实施例制得的立方体磷酸锆载银抗菌粉的扫描电镜图;
图4给出给出本发明实施例制得的立方体磷酸锆载银抗菌粉的扫描电镜图。
3、立方体磷酸锆载银抗菌粉的性能测试
定量测试--GBAT21510-2008粉末抗菌性能试验方法振荡法
取磷酸锆载银粉体0.5g放入三角烧瓶中,再加入95mL含 0.1% 吐温-80的磷酸盐缓冲液,混匀后,再加入5.0ml预制菌悬液(菌液浓度约1.0X105CFU/ml),在作用温度37℃条件下,以150r/min速度,检测样品需要稀释后使用的材料振荡接触1h-4h,再菌落培养。我们研发出来的磷酸锆抗菌粉体对大肠杆菌、金黄色葡萄球菌、白色念珠菌的抗菌率都大于90%。
需要说明的是,在本文中,诸如术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解,在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (4)
1.一种立方体磷酸锆载体的制备方法,其特征在于,包括以下步骤:
S1、称取200kg氧氯化锆,并将其加入45kg去离子水中溶解,称取13.3kg磷酸二氢钠,并将其加入45kg去离子水溶解;
S2、将上述两组溶液进行混合,得到磷酸锆载体溶胶;
S3、将所述磷酸锆载体溶胶、模板剂溶于去离子水并在反应釜中充分混合反应,即得磷酸锆载体;
S4、通过板框式滤布压滤机不断循环压制磷酸锆载体,将载体压实;
S5、将压实后的磷酸锆载体用去离子水反复冲洗干净,即制成磷酸锆载体滤饼。
2.根据权利要求1所述的一种立方体磷酸锆载体的制备方法,其特征在于:步骤S3中,所述模板剂为草酸钠,所述反应压力为常压,反应温度控制在90-110℃,反应时间控制在24h-48h,草酸钠加入量为3.8kg,去离子水加入量为80kg。
3.一种立方体磷酸锆载锌的制备方法,其特征在于,包括以下步骤:
在酸性介质中,酸性介质的pH小于7,将步骤A3制得的100kg磷酸锆载体溶解于200kg的去离子水,称取50kg一水硝酸锌,加入100kg去离子水溶解,制成一水硝酸锌水溶液,然后将磷酸锆载体溶解液分散在40-50%浓度的一水硝酸锌水溶液中,在90-100℃温度下恒温混合搅拌3-5小时,过滤可制得含锌离子浓度为4-5%的立方体磷酸锆载锌。
4.一种立方体磷酸锆载银的制备方法,其特征在于,包括以下步骤:
将上述制得的立方体磷酸锆载锌用去离子水配制成6-10%的水分散液,在酸性介质中加入已定量溶解的硝酸银溶液,其中硝酸银溶液由3kg硝酸银溶解于10kg去离子水中配制而成,在60-90℃温度下恒温2-4h,洗涤过滤后制得立方体磷酸锆载银无机抗菌粉的半成品;
然后将上述立方体磷酸锆载银无机抗菌粉的半成品在烘干机中烘干,烘干温度控制在130-150℃,控制粉体含水率在5-8%,取出后利用粉碎机进行锤粉破碎,再将其送入煅烧窑炉中进行高温定型,控制温度在700-900℃,控制时间5-8小时,待冷却至40-60℃后进行气流粉碎,打开团聚体,即制得立方体磷酸锆载银抗菌粉成品。
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CN102763678A (zh) * | 2012-08-01 | 2012-11-07 | 晋大纳米科技(厦门)有限公司 | 立方体磷酸锆载银抗菌粉的制备方法 |
WO2017092232A1 (zh) * | 2015-12-01 | 2017-06-08 | 东华大学 | 一种高载银含量磷酸锆粉体的制备方法 |
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CN102763678A (zh) * | 2012-08-01 | 2012-11-07 | 晋大纳米科技(厦门)有限公司 | 立方体磷酸锆载银抗菌粉的制备方法 |
WO2017092232A1 (zh) * | 2015-12-01 | 2017-06-08 | 东华大学 | 一种高载银含量磷酸锆粉体的制备方法 |
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