CN115120613B - 一种炉甘石粉的制备方法及应用 - Google Patents
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Abstract
本发明公开了一种炉甘石粉的制备方法以及基于该炉甘石粉用于制备炉甘石洗剂的应用,属于原料药合成工艺领域。其主要步骤是以磁性MOF为前驱体制备多孔碳吸附材料用于除去炉甘石粉中的有毒金属。本制备工艺简单,易操作,具有工业应用价值。
Description
技术领域
本发明涉及到原料药合成工艺领域,更具体的为炉甘石粉的制备方法,尤其是一种低铅、高品质的药用炉甘石粉体的合成方法。
背景技术
炉甘石属于矿物类中药,其主要成分为三角菱锌矿或单斜碳酸锌水合锌矿,具有解毒明目退翳,收涩止痒敛疮之功。对外科、皮肤科、眼科、肛肠科疾病均具有较好的疗效。
含矿物药中药外用制剂临床应用历史悠久,然而,矿物药中重金属及有害元素含量通常较高,造成含矿物药外用制剂临床应用中存在一定的安全性问题。研究表明炉甘石中均含有少量Al、Fe、Ca、Mg、Cd、Pb,普遍含有Mn、Co、Cr、Cu、Mo等微量元素。其中,Pb的含量较高(0.42%-2.9%),给含炉甘石外用制剂的安全性和有效性来潜在的风险。另外,炉甘石成分较复杂,除主成分外,还含有脉石矿物、共生矿物等杂质,如果对这部分杂质不加以限制,就会给炉甘石的质量带来不可控的风险。因此,应提高炉甘石的质量控制,进行炉甘石减杂处理。
金属-有机框架材料(MOFs)是一种新型的晶态多孔材料,具有比表面积大,孔结构可调,易于后修饰等优点,因此近二十多年来,在吸附,分离等领域应用广泛。但由于大多数MOFs的稳定性较差,因此研究者常将MOFs用作前驱体,通过高温裂解,得到含不同活性组分的多孔碳复合材料。MOFs衍生的多孔碳复合材料碳材料,由于其微孔介孔和大孔丰富的孔结构、高表面积、活性组分分布均匀等优点,已经在多技术领域显示了广泛的应用前景。
本发明采用2-甲基咪唑为配体,通过与金属锌和有机铁合成纳米Fe-ZIF-8配合物,以该前体为原料合成多孔碳吸附材料,对炉甘石粉中的铅金属进行吸附,工艺简单,易操作,具有工业应用价值。
发明内容
本发明的技术任务之一是为了弥补现有技术的不足,提供一种制备低铅炉甘石粉的制备方法,制备工艺简单,吸附剂便于除去,具有工业应用前景。
本发明的技术任务之二是提供上述炉甘石粉用于制备炉甘石抑菌洗剂的用途,具有很好的消炎止痛、收敛止痒、促进伤口愈合作用。
本发明的技术方案如下:
1.一种炉甘石粉的制备方法,包括以下步骤:
(1)制备多孔碳磁性吸附材料
将36-38g六水合硝酸锌、30-32g乙酰丙酮铁和19-21g二甲基咪唑分别溶解于200mL的乙醇中;将三种溶液在室温下混合,出现乳状悬浮物,搅拌10-30min,离心并用乙醇洗涤,重复三次,得到红色沉淀,60℃下干燥1h,得到Fe-ZIF-8粉末;
将8-10g Fe-ZIF-8粉末置于管式炉中,在氮气氛围下,以2℃·min-1的速率升高至700-900℃煅烧2-3小时,得到氮和氧化锌共掺杂的石墨相多孔碳磁性吸附材料;
(2)制备炉甘石粉
将100g炉甘石原料放入超声清洗器中,以500W的功率、质量分数为4-5%的乙酸水溶液为介质清洗2-5min,过滤,将得到的固体水洗3次,得到表面光亮的炉甘石;
将清洗过的炉甘石置入110℃的鼓风干燥箱中干燥至恒重,冷却至室温后,经粉碎机粉碎,过120目筛,得到炉甘石粉;
在40-50℃条件下,搅拌条件下,向炉甘石粉中加入140-160mL、质量分数为8%稀盐酸,搅拌至溶解;冷却到室温,过滤去除不溶性固体杂质;将得到的滤液加入100-120mL质量分数为10%氢氧化钠溶液,搅拌20-30min,静置10min后过滤;向滤液中加入0.2-0.5g多孔碳复合材料,搅拌5-10min后,用磁铁去除多孔碳磁性吸附材料,溶液用碳酸钠调节pH8.8-9.2,过滤,水洗固体3次,将得到的固体110℃干燥至恒温,用粉碎机粉碎,过120目筛,制得除铅杂质的碱式碳酸锌,即炉甘石粉。
2.如1所述的制备方法制备的炉甘石粉用于制备炉甘石洗剂的应用,步骤如下:
称取炉甘石粉40g,氧化锌20g,甘油50mL,10g的吐温80,加1000mL水搅拌均匀即得。
本发明有益的技术效果如下:
(1)本发明方案生产的炉甘石粉,色泽均匀,粉体细腻,铅和铜等重金属含量低,纯度高,生物利用度高,工艺简单,易操作,具有工业应用价值;
(2)加入的多孔碳磁性吸附材料不仅含微孔、介孔和大孔,而且有活性氮和氧化锌掺杂,吸附活性高,吸附时间较短;因含磁性四氧化三铁,吸附了重金属离子后,用磁铁就可以快速方便地分离;制得的炉甘石粉纯度可达96.5%。
具体实施方式
下面结合实施例对本发明作进一步描述,但本发明的保护范围不仅局限于实施例,该领域专业人员对本发明技术方案所作的改变,均应属于本发明的保护范围内。
实施例1一种炉甘石粉的制备方法
1)制备多孔碳磁性吸附材料
将36g六水合硝酸锌、30g乙酰丙酮铁和19g二甲基咪唑分别溶解于200mL的乙醇中;将三种溶液在室温下混合,出现乳状悬浮物,搅拌10min,离心并用乙醇洗涤,重复三次,得到红色沉淀,60℃下干燥1h,得到Fe-ZIF-8粉末;
将8g Fe-ZIF-8粉末置于管式炉中,在氮气氛围下,以2℃·min-1的速率升高至700℃煅烧3小时,得到氮和氧化锌共掺杂的石墨相多孔碳磁性吸附材料;
2)制备炉甘石粉
将100g炉甘石原料放入超声清洗器中,以500W的功率、质量分数为4%的乙酸水溶液为介质清洗5min,过滤,将得到的固体水洗3次,得到表面光亮的炉甘石;
将清洗过的炉甘石置入110℃的鼓风干燥箱中干燥至恒重,冷却至室温后,经粉碎机粉碎,过120目筛,得到炉甘石粉;
在40℃条件下,搅拌条件下,向炉甘石粉中加入140mL、质量分数为8%稀盐酸,搅拌至溶解;冷却到室温,过滤去除不溶性固体杂质;将得到的滤液加入100mL质量分数为10%氢氧化钠溶液,搅拌20min,静置10min后过滤;向滤液中加入0.2g多孔碳复合材料,搅拌5min后,用磁铁去除多孔碳磁性吸附材料,溶液用碳酸钠调节pH 8.8,过滤,水洗固体3次,将得到的固体110℃干燥至恒温,用粉碎机粉碎,过120目筛,制得除铅杂质的碱式碳酸锌,即炉甘石粉;所述碱式碳酸锌的含量为96.0%。
实施例2一种炉甘石粉的制备方法
1)制备多孔碳磁性吸附材料
将38g六水合硝酸锌、32g乙酰丙酮铁和21g二甲基咪唑分别溶解于200mL的乙醇中;将三种溶液在室温下混合,出现乳状悬浮物,搅拌30min,离心并用乙醇洗涤,重复三次,得到红色沉淀,60℃下干燥1h,得到Fe-ZIF-8粉末;
将10g Fe-ZIF-8粉末置于管式炉中,在氮气氛围下,以2℃·min-1的速率升高至900℃煅烧2小时,得到氮和氧化锌共掺杂的石墨相多孔碳磁性吸附材料;
2)制备炉甘石粉
将100g炉甘石原料放入超声清洗器中,以500W的功率、质量分数为5%的乙酸水溶液为介质清洗2min,过滤,将得到的固体水洗3次,得到表面光亮的炉甘石;
将清洗过的炉甘石置入110℃的鼓风干燥箱中干燥至恒重,冷却至室温后,经粉碎机粉碎,过120目筛,得到炉甘石粉;
在50℃条件下,搅拌条件下,向炉甘石粉中加入160mL、质量分数为8%稀盐酸,搅拌至溶解;冷却到室温,过滤去除不溶性固体杂质;将得到的滤液加入120mL质量分数为10%氢氧化钠溶液,搅拌30min,静置10min后过滤;向滤液中加入0.5g多孔碳复合材料,搅拌10min后,用磁铁去除多孔碳磁性吸附材料,溶液用碳酸钠调节pH 9.2,过滤,水洗固体3次,将得到的固体110℃干燥至恒温,用粉碎机粉碎,过120目筛,制得除铅杂质的碱式碳酸锌,即炉甘石粉;所述碱式碳酸锌的含量为96.3%。
实施例3一种炉甘石粉的制备方法
1)制备多孔碳磁性吸附材料
将37g六水合硝酸锌、31g乙酰丙酮铁和20g二甲基咪唑分别溶解于200mL的乙醇中;将三种溶液在室温下混合,出现乳状悬浮物,搅拌20min,离心并用乙醇洗涤,重复三次,得到红色沉淀,60℃下干燥1h,得到Fe-ZIF-8粉末;
将9g Fe-ZIF-8粉末置于管式炉中,在氮气氛围下,以2℃·min-1的速率升高至800℃煅烧2.5小时,得到氮和氧化锌共掺杂的石墨相多孔碳磁性吸附材料;
2)制备炉甘石粉
将100g炉甘石原料放入超声清洗器中,以500W的功率、质量分数为4.5%的乙酸水溶液为介质清洗3min,过滤,将得到的固体水洗3次,得到表面光亮的炉甘石;
将清洗过的炉甘石置入110℃的鼓风干燥箱中干燥至恒重,冷却至室温后,经粉碎机粉碎,过120目筛,得到炉甘石粉;
在45℃条件下,搅拌条件下,向炉甘石粉中加入150mL、质量分数为8%稀盐酸,搅拌至溶解;冷却到室温,过滤去除不溶性固体杂质;将得到的滤液加入110mL质量分数为10%氢氧化钠溶液,搅拌25min,静置10min后过滤;向滤液中加入0.35g多孔碳复合材料,搅拌7min后,用磁铁去除多孔碳磁性吸附材料,溶液用碳酸钠调节pH 9.0,过滤,水洗固体3次,将得到的固体110℃干燥至恒温,用粉碎机粉碎,过120目筛,制得除铅杂质的碱式碳酸锌,即炉甘石粉;所述碱式碳酸锌的含量为96.5%。
实施例4炉甘石粉用于制备炉甘石洗剂的应用
称取炉甘石粉40g,氧化锌20g,甘油50mL,10g的吐温80,加1000mL水搅拌均匀即得;所述炉甘石粉选自实施例1、实施例2或实施例3。
Claims (2)
1.一种炉甘石粉的制备方法,其特征在于,包括以下步骤:
(1)制备多孔碳磁性吸附材料
将36-38g六水合硝酸锌、30-32g乙酰丙酮铁和19-21g二甲基咪唑分别溶解于200mL的乙醇中;将三种溶液在室温下混合,出现乳状悬浮物,搅拌10-30min,离心并用乙醇洗涤,重复三次,得到红色沉淀,60℃下干燥1h,得到Fe-ZIF-8粉末;
将8-10g Fe-ZIF-8粉末置于管式炉中,在氮气氛围下,以2℃·min-1的速率升高至700-900℃煅烧2-3小时,得到氮和氧化锌共掺杂的石墨相多孔碳磁性吸附材料;
(2)制备炉甘石粉
将100g炉甘石原料放入超声清洗器中,以500W的功率、质量分数为4-5%的乙酸水溶液为介质清洗2-5min,过滤,将得到的固体水洗3次,得到表面光亮的炉甘石;
将清洗过的炉甘石置入110℃的鼓风干燥箱中干燥至恒重,冷却至室温后,经粉碎机粉碎,过120目筛,得到炉甘石粉;
在40-50℃条件下,搅拌条件下,向炉甘石粉中加入140-160mL、质量分数为8%稀盐酸,搅拌至溶解;冷却到室温,过滤去除不溶性固体杂质;将得到的滤液加入100-120mL质量分数为10%氢氧化钠溶液,搅拌20-30min,静置10min后过滤;向滤液中加入0.2-0.5g多孔碳复合材料,搅拌5-10min后,用磁铁去除多孔碳磁性吸附材料,溶液用碳酸钠调节pH 8.8-9.2,过滤,水洗固体3次,将得到的固体110℃干燥至恒温,用粉碎机粉碎,过120目筛,制得除铅杂质的碱式碳酸锌,即炉甘石粉。
2.根据权利要求1所述的制备方法制备的炉甘石粉用于制备炉甘石洗剂的应用。
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