CN111659347B - 一种用于尿素吸附的微孔活性炭及其制备方法和应用 - Google Patents
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Abstract
本发明涉及一种用于尿素吸附的微孔活性炭及其制备方法和应用,通过碱金属化合物活化碳料或活性炭制备,所述微孔活性炭的比表面积>1500m2/g,微孔比表面积>500m2/g,微孔孔容>0.4cm3/g,微孔孔径为0.4~1.5nm。本发明提供的微孔活性炭对尿素具有高的吸附容量,活化后的活性炭可用于溶液中尿素的吸附及透析液再生系统,极大的简化移动式或穿戴式透析机的开发。
Description
技术领域
本发明涉及尿素吸附材料的制备领域,具体涉及一种用于尿素吸附的微孔活性炭及其制备方法和应用。
背景技术
肾功能衰退或丧失时,导致体内各种毒素在血液或组织中累积,对身体造成严重损害,危及生命。血液透析和腹膜是治疗肾功能衰竭、丧失或替代的有效疗法。最近的研究表明,与常规的间歇式透析治疗相比较,更高频次的治疗或持续治疗与良好的治疗效果具有正相关性。开发便携式或穿戴式的透析机,一方面可以实现持续治疗的目的,提高治疗效果,另一方面有利于改善病患的生活质量,节约成本。将透析液再生循环使用,能极大地减少外加水源,减小透析机的重量和尺寸,是开发移动式或可穿戴式透析机的一种有效方式。
有效地移除尿素,实现透析液再生循环是该领域面临的最大难点。基于脲酶分解尿素开发出的REDY系统是目前研究最广泛的技术,能有效的清除尿素,实现透析液再生。然而,中性的尿素被脲酶分解后,形成的碳酸铵导致透析液的酸碱失衡,同时为清除产生的铵离子,需要采用离子交换树脂,导致透析液中的离子浓度也出现失衡,需要复杂的调控系统,在实际应用中存在较大的风险。
直接吸附尿素,是一种简单有效的方式,迄今为止,还未开发出具有实用价值的尿素吸附材料。活性炭是一种广谱的吸附材料,可以清除透析液中除了尿素外的各种毒素。目前已知的活性炭对尿素的吸附容量低,不能满足实际使用的需求。
发明内容
针对现有技术中存在的缺陷和不足,本发明提供了一种用于尿素吸附的微孔活性炭及其制备方法和应用。
本发明的目的之一在于提供一种用于尿素吸附的微孔活性炭,通过碱金属化合物活化碳料或活性炭制备,所述微孔活性炭的比表面积>1500m2/g,微孔比表面积>500m2/g,微孔孔容>0.4cm3/g,微孔孔径为0.4~1.5nm。
根据本发明的一些优选实施方式,所述微孔活性炭的比表面积1500~3000m2/g,微孔比表面积500~2000m2/g,微孔孔容为0.4~0.8cm3/g,微孔孔径为0.4~1.5nm。
根据本发明的一些优选实施方式,所述碱金属化合物选自钾、钠或锂的单质、无机物及C1-C16的有机物中的一种或多种;优选的,所述碱金属化合物选自钾、钠或锂的碳酸盐、碳酸氢盐、氢氧化物、氧化物、氢化物、氯化物、磷酸盐、磷酸氢盐、磷酸二氢盐、C1-C16的烷氧基化合物、C1-C16的酚羟基化合物和C1-C16的羧酸盐中的一种或多种,更优选为氢氧化钾、氧化钾、碳酸钾或碳酸氢钾。
根据本发明的一些优选实施方式,所述碳料为焦化碳料,优选为60-300目的椰壳碳化料。
本发明的另一目的在于提供一种所述微孔活性炭的制备方法,包括由所述碱金属化合物和所述碳料在惰性气氛条件下,于750~1000℃,进行活化1~4h的步骤。
根据本发明的一些优选实施方式,所述碱金属化合物与所述碳料的质量比为1:1~6:1,优选为1.5:1~3:1。
根据本发明的一些优选实施方式,反应温度为800~900℃。
根据本发明的一些优选实施方式,所述微孔活性炭制备还包括水洗、酸洗及干燥的后处理步骤。
本发明的另一目的在于提供所述的微孔活性炭或所述的制备方法制备得到的微孔活性炭的应用,所述微孔活性炭用于溶液中尿素的吸附,优选用于4~40℃温度范围内溶液中尿素的吸附;所述微孔活性炭的尿素吸附容量优选为不低于15mg/g。
本发明的再一目的在于提供所述的微孔活性炭或所述的方法制备得到的微孔活性炭或所述的应用,在血液透析或腹膜透析中的应用。
本发明的有益效果至少在于:本发明通过采用碱金属活化的方式,对一些常规活性炭或碳化料进行活化,极大改善其对尿素的吸附性能,解决目前活性炭吸附尿素容量低的问题,活化后的活性炭可用于溶液中尿素的吸附及透析液再生系统,极大的简化移动式或穿戴式透析机的开发。
附图说明
图1为本发明中微孔活性炭代表性的制备条件及尿素吸附容量(尿素:2g/L,38℃);
图2为不同碱/碳料比例与尿素吸附容量关系(850℃-2.5h,尿素2g/L);
图3为不同碱比例制备的活性炭(850℃-2.5h)在不同温度下对尿素的吸附(尿素2g/L);
图4为KOH/C=2@850-2.5在4度和38度对不同尿素浓度的吸附;
图5为尿素动态吸附(活性炭100g,流速:100mL/min,15℃);
图6为尿素动态吸附容量(活性炭100g,流速:100mL/min,15℃)。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。本发明技术方案不局限于以下所列举具体实施方式,还包括各具体实施方式间的任意组合,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。
本发明中,实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件,或者按照产品说明书进行。所用仪器等未注明生产厂商者,均为可通过正规渠道商购买得到的常规产品。本发明以下实施例中所用的原料均可在国内市场方便买到。
实施例1
本实施例提供活性炭及制备:将KOH与80-120目椰壳碳化料按照质量比1.5混合均匀后,置于管式炉中,在氮气氛围下,加热至850℃,按照设定的时间2.5h保温。冷却后,用去离子水洗去可溶物,将所得到的固体置于1M稀盐酸中,加热至50℃,调节至弱酸性pH=6左右,过滤,再水洗至中性后,于110℃干燥,得活性炭,孔径参数采用BET分析表征,制备的活性炭(KOH/C=1.5@850-2.5h)孔径参数见表1。
对比例1
采用与实施例1相同的方法,不同之处在于直接将碳料置于管式炉,在氮气氛围下加热,制备的活性炭(C@850-2.5h)孔径参数见表1。
实施例2
采用与实施例1相同的方法,不同之处在于KOH与碳料的质量比为2,制备的活性炭(KOH/C=2@850-2.5h)孔径参数见表1。
实施例3
采用与实施例1相同的方法,不同之处在于将KOH替换为CH3COOK,制备的活性炭(CH3COOK/C=3@850-2.5h)孔径参数见表1。不同条件制备活性碳对尿素对吸附性能见表2和图2。
表1对比例及实施例1~3的孔径参数
实验例1(尿素的静态吸附测试)
测试方法:取100mg微孔活性炭,加入6mL尿素水溶液,于设定的温度下,置于摇床中振荡60min,过滤,收集滤液。采用HPLC,测试尿素浓度变化,计算尿素吸附量。测试条件:C18柱,检测波长:200nm,流动相:甲醇/水=5%,流速:0.5mL/min。
1)微孔活性炭的制备条件(具体测试的微孔活性炭的制备条件如图1,其他条件均与实施例1相同)及尿素吸附容量测试结果见图1。由图可见,碱金属活化的活性炭对尿素的吸附容量与活化温度及碱用量相关。活化温度在800~900℃之间有利于提高尿素的吸附,当温度超过950℃后,活性炭对尿素的吸附容量明显下降。
2)不同碱/碳料比例与尿素吸附容量关系测试,测试的微孔活性炭的制备条件如图2(其他条件均与实施例1相同),尿素吸附容量测试(850℃-2.5h,尿素2g/L)结果见图2。由图可见,通过改变碱的用量,可以明显改善活性炭对尿素的吸附性能。当活化温度为850℃,活化时间为2.5h时,碱用量与碳料的比处于1.5~3之间,有利于得到高尿素吸附容量的活性炭,进一步增加碱的用量,产生的活性炭对尿素的吸附容量逐渐降低。碱活化的活性炭对尿素的吸附容量均明显高于未活化的活性炭。
3)活性炭(900℃-2h)在不同温度下对尿素的吸附测试,测试的微孔活性炭的制备条件如图3(其他条件均与实施例1相同),尿素吸附容量测试结果见图3。由图可见,活性炭在4-38℃范围内均具有明显的尿素吸附。低温更有利于尿素的吸附,活性炭吸附尿素在低温透析中具有更优异的性能。
4)KOH/C=2@850-2.5在4℃和38℃对不同尿素浓度的吸附测试,测试的微孔活性炭的制备条件如图4(其他条件均与实施例1相同),尿素吸附容量测试结果见图4。由图可见,活性碳对尿素的吸附与浓度正相关。透析患者的体内尿素浓度通常在2g/L左右,碱活化的活性炭在此浓度单位内均展现出高的吸附容量。
5)不同碱活化碳吸附尿素的测试,测试的微孔活性炭的制备条件如表2(其他条件均与实施例1相同),尿素吸附容量测试结果见表2。
表2几种不同碱活化碳吸附尿素结果
实验例2(尿素的动态吸附测试)
为了模拟透析过程中尿素的吸附,采用不同浓度的尿素生理盐水溶液,测试100g活性炭对尿素的动态吸附。
取100g实施例2的活性炭,装入直径6cm柱中,于15℃的温度下,用尿素的生理盐水淋洗,流速为100mL/min,收集淋洗液。采用HPLC,测试尿素浓度变化。
由图5尿素动态吸附(活性炭100g,流速:100mL/min,15℃)的测试结果,可见,低温下,活性炭展示出明显的尿素吸附,当淋洗液中尿素浓度在0.5-2.5g/L之间时,前10min的淋出液中均无尿素。吸附饱和均出现在20min左右。
图6为尿素动态吸附容量(活性炭100g,流速:100mL/min,15℃)的测试结果,基于动态淋洗测试发现,活性炭对尿素的吸附与浓度呈线性关系,尿素浓度越高,吸附容量越大。1.5~2kg的活性炭可以吸附20g左右尿素。
虽然,上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述,但在本发明基础上,可以对之作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。
Claims (5)
1.一种用于血液透析或腹膜透析的微孔活性炭的制备方法,其特征在于,由碱金属化合物和60-300目的椰壳碳化料在惰性气氛条件下,进行活化2.5h制备;所述碱金属化合物为氢氧化钾、碳酸钾、氢氧化锂或水杨酸钠;所述碱金属化合物为碳酸钾时,所述碳酸钾与所述60-300目的椰壳碳化料的质量比为1,活化温度为850℃,所述碱金属化合物为氢氧化锂时,所述氢氧化锂与所述60-300目的椰壳碳化料的质量比为1,活化温度为850℃,所述碱金属化合物为水杨酸钠时,所述水杨酸钠与所述60-300目的椰壳碳化料的质量比为2,活化温度为800℃;
所述微孔活性炭的比表面积为1500~3000m2/g,微孔比表面积 500~2000m2/g,微孔孔容为0.4~0.8cm3/g,微孔孔径为0.4~1.5nm。
2.根据权利要求1所述的制备方法,其特征在于,所述微孔活性炭制备还包括水洗、酸洗及干燥的后处理步骤。
3.根据权利要求1或2所述的制备方法,其特征在于,所述微孔活性炭用于溶液中尿素的吸附。
4.根据权利要求3所述的制备方法,其特征在于,所述微孔活性炭用于4~40℃温度范围内溶液中尿素的吸附。
5.根据权利要求4所述的制备方法,其特征在于,所述微孔活性炭的尿素吸附容量为不低于15mg/g。
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