CN106219543B - 一种亚毫米级聚苯乙烯基球状活性炭及其制备方法与应用 - Google Patents
一种亚毫米级聚苯乙烯基球状活性炭及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种亚毫米级聚苯乙烯基球状活性炭及其制备方法与应用。该制备方法为：以苯乙烯和二乙烯苯为原料得到聚苯乙烯基微球，将上述聚苯乙烯基微球溶胀于四氯化碳中，加入催化剂，固化成型，制得超交联热固性聚苯乙烯基树脂球，树脂球置于饱和氯化钠溶液中浸泡，并依次用稀盐酸、氢氧化钠溶液、去离子水清洗至中性，干燥；再经高温炭化和水蒸气活化，制得聚苯乙烯基球状活性炭；将上述聚苯乙烯基球状活性炭经空气氧化、高温氮气热处理进行表面改性。本发明的制备方法工艺简单，降低了生产成本，所制得的球状活性炭表面光滑、球形度高、比表面积可达960m2/g～1400m2/g，可用于吸附尿毒素肌酐，在尿毒症治疗领域具有广泛应用前景。
Description
技术领域
本发明涉及一种球状活性炭，具体涉及一种亚毫米级聚苯乙烯基球状活性炭及其制备方法与应用。
背景技术
球状活性炭属高科技、高附加值产品，是一种新型高性能活性炭。与常规活性炭相比，球形活性炭外表为球形，具有耐磨性好，机械强度高，填充密度高，颗粒分布均匀，流动阻力小，孔径分布易控，吸脱附速度快，生理相容性好等特点。近年来在高级环保、催化剂载体及生理医学等方面得到广泛的应用。
采用活性炭治疗肾脏病始于20世纪60年代，1964年，希腊学者首先用未经包裹的活性炭直接接触血液进行灌流，治疗急性药物中毒。由于活性炭具有很强的吸附能力，对血液中的毒素清除效果显著。但是，炭的微粒释放导致的脏器微血管栓塞、不规则无形状引起血小板和白细胞的破坏、溶血、致热原等不良反应带来的副作用严重限制了其在临床上的推广使用。
现有的球状活性炭主要分两大类：沥青基球状活性炭和树脂基球状活性炭，其中树脂基球状活性炭具备无重金属含量、高硬度、高流动性、高机械强度、高比表面积的特性，可以避免用于医疗时因为炭微粒释放导致的各种不良反应。目前，国内外的研究方向以酚醛树脂为原料制备的球状活性炭为主，工业上酚醛树脂通常由苯酚或其同系物和甲醛缩聚制得，原料苯酚价格昂贵，且酚醛树脂的生产工艺复杂，能耗高，导致制备的球状活性炭成本较高。
发明内容
本发明的目的之一是提供一种亚毫米级聚苯乙烯基球状活性炭，成本低廉。
本发明的目的之二是提供上述亚毫米级聚苯乙烯基球状活性炭的制备方法，工艺简单，易操作。
为实现上述目的，本发明的一种亚毫米级聚苯乙烯基球状活性炭，以超交联热固性聚苯乙烯基树脂球为原料制得。所述的球状活性炭的粒径为0.2mm～0.3mm，比表面积为960m2/g～1400m2/g，总孔容为0.3cm3/g～0.8cm3/g，微孔容积为0.2cm3/g～0.6cm3/g。
上述亚毫米级聚苯乙烯基球状活性炭的制备方法，包括以下步骤：
(1)将反应单体苯乙烯和二乙烯苯按质量比1:8～8:1充分混合，得到混合单体，并在混合单体中加入引发剂过氧化二苯甲酰和致孔剂正戊烷，充分搅拌后形成油相A，其中，所述的过氧化二苯甲酰的质量占混合单体质量的0.5％～3％，所述的正戊烷的质量占混合单体质量的0.1％～2％；在去离子水中加入分散剂明胶和氯化钠，缓慢加热并充分搅拌形成水相B，其中，所述的去离子水与混合单体的质量比为20:1～2:1，所述的明胶的质量占去离子水质量的0.2％～2％，所述的氯化钠的质量占去离子水质量的1％～10％；将上述配置好的油相A缓慢加入水相B中，充分排除氧气后加热至70℃～100℃，恒温1h～5h，过滤，真空干燥，经24目和60目过筛后得聚苯乙烯基微球；
(2)将上述聚苯乙烯基微球溶胀于四氯化碳中，加入催化剂，固化成型，制得超交联热固性聚苯乙烯基树脂球，其中，所述的聚苯乙烯基微球：四氯化碳的质量比为1:1～1:100，所述的催化剂：聚苯乙烯基微球的质量比为0.2:1～2:1；
(3)将上述热固性聚苯乙烯基树脂球置于饱和氯化钠溶液中浸泡24h，并依次用5％的稀盐酸和5％氢氧化钠溶液洗涤，最后用去离子水清洗至中性，干燥；
(4)在惰性气体保护下将洗涤后的热固性聚苯乙烯基树脂球升温至500℃～800℃下炭化，恒温1h～10h，制得聚苯乙烯基炭球；
(5)将聚苯乙烯基炭球在750℃～950℃温度下通入水蒸气活化，制得聚苯乙烯基球状活性炭；
(6)对上述聚苯乙烯基球状活性炭进行表面改性，在300℃～500℃空气中氧化0.5h～8h，然后在700℃～800℃氮气条件下热处理0.5h～8h。
步骤(1)中，油水混合相升温速率为1℃/min～20℃/min。
步骤(2)中，所述的固化反应温度为40℃～80℃，固化反应时间为1h～10h。
步骤(2)中，所述的催化剂是无水三氯化铝或无水三氯化铁。
步骤(4)中，所述的炭化升温速率为1℃/min～10℃/min。
步骤(5)中，所述的水蒸气与聚苯乙烯基炭球的质量比为0.5:1～5:1，所述的活化反应时间为1h～2h。
本发明改性后的亚毫米级聚苯乙烯基球状活性炭可用于吸附尿毒素肌酐。
本发明具有如下有益效果：
(1)本发明的聚苯乙烯基球状活性炭以超交联热固性聚苯乙烯基树脂球为原料，聚苯乙烯基树脂球以苯乙烯、二乙烯苯聚合制得，原料便宜，且聚合条件温和，步骤简单，节省能耗，易于工业化生产，降低了球状活性炭的生产成本。
(2)本发明制备的聚苯乙烯基球状活性炭粒径约0.2mm～0.3mm，粒径均一，表面光滑，球形度良好，比表面积可达960m2/g～1400m2/g，总孔容为0.3cm3/g～0.8cm3/g，微孔容积为0.2cm3/g～0.6cm3/g。
(3)本发明制备工艺简单，通过调整制备过程中的工艺参数，可调控最终产品的粒径、比表面积、孔径分布、机械强度等参数。
(4)本发明制备的聚苯乙烯基球状活性炭能用于吸附尿毒素肌酐，且吸附率达95％以上，在尿毒症治疗领域具有广泛应用前景。
附图说明
图1为本发明实施例2制备的聚苯乙烯基球状活性炭的外观图；
图2为图1所示的聚苯乙烯基球状活性炭显微镜图；
图3为不同活化温度下聚苯乙烯基球状活性炭的N2吸附等温曲线图；
图4为不同活化温度下聚苯乙烯基球状活性炭的比表面积变化趋势图；
图5为本发明实施例1至5制备的聚苯乙烯基球状活性炭吸附肌酐的性能图。
具体实施方式
下面结合具体实施例和附图对本发明作进一步详细阐述。
实施例1
一种亚毫米级聚苯乙烯基球状活性炭的制备方法，包括以下步骤：
(1)在三口烧瓶中将反应单体5g苯乙烯和40g二乙烯苯充分混合，得到混合单体，并在混合单体中加入0.25g引发剂过氧化二苯甲酰，搅拌，使过氧化苯甲酰充分溶解，然后再加入0.45g致孔剂正戊烷，充分搅拌后配成油相A；向装有电动搅拌器、温度计和冷凝管的三口烧瓶中加入900g去离子水，在去离子水中加入18g分散剂明胶，并加入90g的氯化钠以防止极性单体在水中的聚合，缓慢加热并充分搅拌形成水相B，升温到55℃后停止搅拌；将上述配置好的油相A缓慢加入水相B中，充分排除氧气后以10℃/min的速率升温到90℃，恒温3h，过滤，真空干燥，经24目和60目过筛后得聚苯乙烯基微球；
(2)取10g上述聚苯乙烯基微球溶胀于1000g四氯化碳中，以2g无水三氯化铁作为催化剂，以5℃/min的速率升温至80℃，反应1.5h固化成型，制得超交联热固性聚苯乙烯基树脂球；
(3)将上述热固性聚苯乙烯基树脂球置于饱和氯化钠溶液中浸泡24h，并依次用5％的稀盐酸和5％氢氧化钠溶液洗涤，最后用去离子水清洗至中性，干燥；
(4)在氮气保护下将洗涤后的热固性聚苯乙烯基树脂球以2℃/min速率升温至500℃进行炭化，炭化2h，制得聚苯乙烯基炭球；
(5)取10g聚苯乙烯基炭球在800℃温度下通入5g水蒸气活化，活化1.5h，制得聚苯乙烯基球状活性炭；
(6)对上述聚苯乙烯基球状活性炭进行表面改性，在300℃空气中氧化8h，然后在700℃氮气条件下热处理8h。
实施例2
一种亚毫米级聚苯乙烯基球状活性炭的制备方法，包括以下步骤：
(1)在三口烧瓶中将反应单体20g苯乙烯和20g二乙烯苯充分混合，得到混合单体，并在混合单体中加入0.2g引发剂过氧化二苯甲酰，搅拌，使过氧化苯甲酰充分溶解，然后再加入0.3g致孔剂正戊烷，充分搅拌后配成油相A；向装有电动搅拌器、温度计和冷凝管的三口烧瓶中加入150g去离子水，在去离子水中加入0.5g分散剂明胶，并加入7.5g的氯化钠以防止极性单体在水中的聚合，缓慢加热并充分搅拌形成水相B，升温到55℃后停止搅拌；将上述配置好的油相A缓慢加入水相B中，充分排除氧气后以5℃/min的速率升温到90℃，恒温2h，过滤，真空干燥，经24目和60目过筛后得聚苯乙烯基微球；
(2)取10g上述聚苯乙烯基微球溶胀于50g四氯化碳中，以10g无水三氯化铁作为催化剂，以2℃/min的速率升温至70℃，反应2h固化成型，制得超交联热固性聚苯乙烯基树脂球；
(3)将上述热固性聚苯乙烯基树脂球置于饱和氯化钠溶液中浸泡24h，并依次用5％的稀盐酸和5％氢氧化钠溶液洗涤，最后用去离子水清洗至中性，干燥；
(4)在氮气保护下将洗涤后的热固性聚苯乙烯基树脂球以1℃/min速率升温至550℃进行炭化，炭化1h，制得聚苯乙烯基炭球；
(5)取10g聚苯乙烯基炭球在750℃温度下通入20g水蒸气活化，活化1h，制得聚苯乙烯基球状活性炭；
(6)对上述聚苯乙烯基球状活性炭进行表面改性，在450℃空气中氧化1h，然后在750℃氮气条件下热处理1h。
实施例3
一种亚毫米级聚苯乙烯基球状活性炭的制备方法，包括以下步骤：
(1)在三口烧瓶中将反应单体30g苯乙烯和10g二乙烯苯充分混合，得到混合单体，并在混合单体中加入0.4g引发剂过氧化二苯甲酰，搅拌，使过氧化苯甲酰充分溶解，然后再加入0.2g致孔剂正戊烷，充分搅拌后配成油相A；向装有电动搅拌器、温度计和冷凝管的三口烧瓶中加入600g去离子水，在去离子水中加入6g分散剂明胶，并加入25g的氯化钠以防止极性单体在水中的聚合，缓慢加热并充分搅拌形成水相B，升温到55℃后停止搅拌；将上述配置好的油相A缓慢加入水相B中，充分排除氧气后以1℃/min的速率升温到70℃，恒温1h，过滤，真空干燥，经24目和60目过筛后得聚苯乙烯基微球；
(2)取10g上述聚苯乙烯基微球溶胀于100g四氯化碳中，以5g无水三氯化铝作为催化剂，以1℃/min的速率升温至40℃，反应10h固化成型，制得超交联热固性聚苯乙烯基树脂球；
(3)将上述热固性聚苯乙烯基树脂球置于饱和氯化钠溶液中浸泡24h，并依次用5％的稀盐酸和5％氢氧化钠溶液洗涤，最后用去离子水清洗至中性，干燥；
(4)在氩气保护下将洗涤后的热固性聚苯乙烯基树脂球以5℃/min速率升温至700℃进行炭化，炭化8h，制得聚苯乙烯基炭球；
(5)取10g聚苯乙烯基炭球在850℃温度下通入10g水蒸气活化，活化2h，制得聚苯乙烯基球状活性炭；
(6)对上述聚苯乙烯基球状活性炭进行表面改性，在400℃空气中氧化6h，然后在700℃氮气条件下热处理6h。
实施例4
一种亚毫米级聚苯乙烯基球状活性炭的制备方法，包括以下步骤：
(1)在三口烧瓶中将反应单体40g苯乙烯和10g二乙烯苯充分混合，得到混合单体，并在混合单体中加入1g引发剂过氧化二苯甲酰，搅拌，使过氧化苯甲酰充分溶解，然后再加入0.5g致孔剂正戊烷，充分搅拌后配成油相A；向装有电动搅拌器、温度计和冷凝管的三口烧瓶中加入500g去离子水，在去离子水中加入7.5g分散剂明胶，并加入48g的氯化钠以防止极性单体在水中的聚合，缓慢加热并充分搅拌形成水相B，升温到55℃后停止搅拌；将上述配置好的油相A缓慢加入水相B中，充分排除氧气后以20℃/min的速率升温到100℃，恒温5h，过滤，真空干燥，经24目和60目过筛后得聚苯乙烯基微球；
(2)取10g上述聚苯乙烯基微球溶胀于200g四氯化碳中，以20g无水三氯化铝作为催化剂，以2℃/min的速率升温至80℃，反应1h固化成型，制得超交联热固性聚苯乙烯基树脂球；
(3)将上述热固性聚苯乙烯基树脂球置于饱和氯化钠溶液中浸泡24h，并依次用5％的稀盐酸和5％氢氧化钠溶液洗涤，最后用去离子水清洗至中性，干燥；
(4)在氩气保护下将洗涤后的热固性聚苯乙烯基树脂球以2℃/min速率升温至650℃进行炭化，炭化5h，制得聚苯乙烯基炭球；
(5)取10g聚苯乙烯基炭球在900℃温度下通入40g水蒸气活化，活化2h，制得聚苯乙烯基球状活性炭；
(6)对上述聚苯乙烯基球状活性炭进行表面改性，在350℃空气中氧化6h，然后在750℃氮气条件下热处理6h。
实施例5
一种亚毫米级聚苯乙烯基球状活性炭的制备方法，包括以下步骤：
(1)在三口烧瓶中将反应单体40g苯乙烯和5g二乙烯苯充分混合，得到混合单体，并在混合单体中加入1.35g引发剂过氧化二苯甲酰，搅拌，使过氧化苯甲酰充分溶解，然后再加入0.9g致孔剂正戊烷，充分搅拌后配成油相A；向装有电动搅拌器、温度计和冷凝管的三口烧瓶中加入90g去离子水，在去离子水中加入0.18g分散剂明胶，并加入0.9g的氯化钠以防止极性单体在水中的聚合，缓慢加热并充分搅拌形成水相B，升温到55℃后停止搅拌；将上述配置好的油相A缓慢加入水相B中，充分排除氧气后以8℃/min的速率升温到80℃，恒温4h，过滤，真空干燥，经24目和60目过筛后得聚苯乙烯基微球；
(2)取10g上述聚苯乙烯基微球溶胀于10g四氯化碳中，以2g无水三氯化铝作为催化剂，以2℃/min的速率升温至60℃，反应5h固化成型，制得超交联热固性聚苯乙烯基树脂球；
(3)将上述热固性聚苯乙烯基树脂球置于饱和氯化钠溶液中浸泡24h，并依次用5％的稀盐酸和5％氢氧化钠溶液洗涤，最后用去离子水清洗至中性，干燥；
(4)在氩气保护下将洗涤后的热固性聚苯乙烯基树脂球以10℃/min速率升温至800℃进行炭化，炭化10h，制得聚苯乙烯基炭球；
(5)取10g聚苯乙烯基炭球在950℃温度下通入50g水蒸气活化，活化2h，制得聚苯乙烯基球状活性炭；
(6)对上述聚苯乙烯基球状活性炭进行表面改性，在500℃空气中氧化0.5h，然后在800℃氮气条件下热处理0.5h。
如图1和图2所示，本发明制得的聚苯乙烯基球状活性炭，直径约0.2～0.3mm，粒径均一，表面光滑，呈圆球形。
聚苯乙烯基球状活性炭的比表面积由图3测得的吸附等温线采用BET法计算得出，相应孔容应用基于多孔固体上吸附氮分子模型的密度函数理论(DFT)分析得到。实施例1至5制得的聚苯乙烯基球状活性炭的孔结构参数如下表所示：
表1不同活化温度下聚苯乙烯基球状活性炭的孔结构参数
由图4可看出，随着活化温度的升高，聚苯乙烯基球状活性炭的比表面积也逐渐增大，可达1387m2/g。
实施例6：聚苯乙烯基球状活性炭对肌酐的吸附实验
用磷酸缓冲液(pH＝7.4)配置100mg/L浓度的肌酐水溶液，定量移取肌酐溶液，置于锥形瓶中，加入一定质量的聚苯乙烯基球状活性炭，其中，聚苯乙烯基球状活性炭与肌酐溶液的比例为1g/5mL，在恒温(37±1)℃下静置2h，沥出溶液，用紫外可见分光光度计在232nm测定肌酐的浓度，计算聚苯乙烯基球状活性炭对肌酐的吸附量。
肌酐吸附性能的测定：
用磷酸缓冲液(pH＝7.4)配制50mg/L的肌酐溶液，分别移取5mL、10mL、15mL、20mL、25mL上述溶液至一系列50mL容量瓶中，定容。分别取上述标准溶液，用紫外可见分光光度计在波长232nm处，以磷酸缓冲液(pH＝7.4)为参比液，测定肌酐标准溶液的吸光度，得到肌酐标准曲线。肌酐标准溶液在上述浓度范围内，吸光值与浓度呈线性关系。即吸附前肌酐溶液的浓度为C0，利用上述标准曲线，可求出在不同测试条件下肌酐被活性炭吸附后的浓度C。计算聚苯乙烯基球状活性炭对肌酐的吸附率W为：
W＝1-C0/C
图5所示为实施例1至5制得的聚苯乙烯基球状活性炭对肌酐的吸附率。从图5可看出，吸附率随着聚苯乙烯基球状活性炭的比表面积的增大而增大。
除了本发明中提及的以聚苯乙烯基树脂球为原料制备聚苯乙烯基球状活性炭，还可以在聚苯乙烯树脂球上引入其他功能基团，如氯甲基、氯乙酰基、磺酸基、纳米二氧化硅等，可制得具有不同功能的改性聚苯乙烯树脂球，从而改善聚苯乙烯基球状活性炭的性能。
Claims (6)
1.一种亚毫米级聚苯乙烯基球状活性炭的制备方法，其特征在于，包括以下步骤：
（1）将反应单体苯乙烯和二乙烯苯按质量比1:8～8:1充分混合，得到混合单体，并在混合单体中加入引发剂过氧化二苯甲酰和致孔剂正戊烷，充分搅拌后形成油相A，其中，所述的过氧化二苯甲酰的质量占混合单体质量的0.5%～3%，所述的正戊烷的质量占混合单体质量的0.1%～2%；在去离子水中加入分散剂明胶和氯化钠，缓慢加热并充分搅拌形成水相B，其中，所述的去离子水与混合单体的质量比为20:1～2:1，所述的明胶的质量占去离子水质量的0.2%～2%，所述的氯化钠的质量占去离子水质量的1%～10%；将上述配置好的油相A缓慢加入水相B中，充分排除氧气后加热至70oC～100oC，恒温1h～5h，过滤，真空干燥，经 24目和60目过筛后得聚苯乙烯基微球；
（2）将上述聚苯乙烯基微球溶胀于四氯化碳中，加入催化剂，固化成型，制得超交联热固性聚苯乙烯基树脂球，其中，所述的聚苯乙烯基微球：四氯化碳的质量比为1:1～1:100，所述的催化剂：聚苯乙烯基微球的质量比为0.2:1～2:1；
（3）将上述热固性聚苯乙烯基树脂球置于饱和氯化钠溶液中浸泡24h，并依次用5%的稀盐酸和5%氢氧化钠溶液洗涤，最后用去离子水清洗至中性，干燥；
（4）在惰性气体保护下将洗涤后的热固性聚苯乙烯基树脂球升温至500oC～800oC下炭化，恒温1h～10h，制得聚苯乙烯基炭球；
（5）将聚苯乙烯基炭球在750oC～950oC温度下通入水蒸气活化，制得聚苯乙烯基球状活性炭；
（6）对上述聚苯乙烯基球状活性炭进行表面改性，在300oC～500oC空气中氧化0.5h～8h，然后在700oC～800oC氮气条件下热处理0.5h～8h。
2.根据权利要求1所述的亚毫米级聚苯乙烯基球状活性炭的制备方法，其特征在于，步骤（1）中，油水混合相升温速率为1oC/min～20oC/min。
3.根据权利要求1所述的亚毫米级聚苯乙烯基球状活性炭的制备方法，其特征在于，步骤（2）中，固化反应温度为40oC～80oC，固化反应时间为1h～10h。
4.根据权利要求1所述的亚毫米级聚苯乙烯基球状活性炭的制备方法，其特征在于，步骤（2）中，所述催化剂是无水三氯化铝或无水三氯化铁。
5.根据权利要求1所述的亚毫米级聚苯乙烯基球状活性炭的制备方法，其特征在于，步骤（4）中，所述的炭化升温速率为1oC/min～10oC/min。
6.根据权利要求1所述的亚毫米级聚苯乙烯基球状活性炭的制备方法，其特征在于，步骤（5）中，所述的水蒸气与聚苯乙烯基炭球的质量比为0.5:1～5:1，所述的活化反应时间为1h～2h。
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