CN116212825B - 一种改性废弃咖啡渣生物炭吸附材料及其制备方法 - Google Patents
一种改性废弃咖啡渣生物炭吸附材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种改性废弃咖啡渣生物炭吸附材料及其制备方法，该生物炭吸附材料由海泡泥、壳聚糖和十六烷基磺丙基甜菜碱复合改性咖啡渣而成，并应用于海洋溢油治理。本发明通过废弃的咖啡渣先与海泡泥高温反应成咖啡渣生物炭土，海泡泥可使吸附材料具有较大的比表面积和高孔隙率，增加吸附活性点，提高吸油率。再与十六烷基磺丙基甜菜碱和壳聚糖反应，其中，壳聚糖可以减少咖啡渣炭土的团聚，在海水中形成天然凝胶浮于水面，提高生物炭的保油率和便于回收；十六烷基磺丙基甜菜碱具有良好的疏水性，可与负载咖啡渣表面形成光滑分子层构成双层亚胶束结构，提高吸附材料疏水性。
Description
技术领域
本发明属于海洋溢油污染处理技术领域，具体涉及一种改性废弃咖啡渣生物炭吸附材料及其制备方法
背景技术
石油在开采或运输过程中，由于意外事故或操作失误，造成原油或油品从作业现场或储器里外泄，流向地面、水面、海滩或海面，同时由于油质成分的不同，形成薄厚不等的一片油膜，这一现象称为溢油。海上发生溢油污染事故发生时，为了防止油污染区域继续扩大以造成更大的损失，需要对油污进行及时有效地处理。在面对油污染时，常用的处理方法可分为：物理处理法、化学处理法和生物处理法。其中，物理吸附法是利用活性炭、玉米秸秆、聚氨酯吸油树脂等吸油材料对水中所包含的油分子进行吸附，进而实现去除油污的目的。
活性炭是由木质、煤质和石油焦等含碳的原料经热解、活化加工制备而成，具有发达的孔隙结构、较大的比表面积和丰富的表面化学基团，特异性吸附能力较强的炭材料的统称，被广泛地用于重金属污水处理、废气处理、染料污水处理等方面。专利CN114570342A公开了一种硅烷化活性炭吸附材料的制备方法和专利CN110732315A公开的活性炭吸附材料、其制备方法及其在催化分解有机污染物领域中的应用均是利用活性炭的大孔径表面，增加其亲水性，可有效地选择吸附有机物的特性对污水进行处理。然而，这些活性炭由于密度大于海水的密度，并不适合用于海洋溢油处理。因此寻找无毒且环保、可浮于海水表面、快速吸油的吸附材料非常重要。专利CN 110237814 A公开的利用热分解法制备的焦炭活性炭，具有高吸油率且可短时间浮于海水表面表面，但是其保油率差无法长时间使用。本发明基于废物再利用，将海泡泥、壳聚糖和十六烷基磺丙基甜菜碱与废弃咖啡渣反应，生成一种具有较好吸附能力、良好的保油率和可浮于海水表面的废弃咖啡渣生物炭吸附材料，吸油后的油渣可作为是潜在生物燃料使用，实现废弃咖啡渣生物炭在海洋溢油污染治理中的应用。
发明内容
本发明的第一个发明目的在于：提供一种由废弃咖啡渣制备的新型吸附材料，用于吸附海洋油污染物。该吸附材料具有成本低廉、合成工艺简单，克服了目前吸油材料所存在成本高、吸油时间长和保油率低等不足，吸油后所得油炭的点火温度为210.78℃，可作为是潜在生物燃料使用，从而实现废物再利用，具有大规模商业化应用的潜能。
本发明的第二个发明目的在于：本发明选用的海泡泥可增加咖啡渣生物炭材料的比表面积和孔隙率，使材料整体更加疏松多孔；通过十六烷基磺丙基甜菜碱与咖啡渣通过阳离子交换作用附着在咖啡渣表层，利用疏水作用力发生有序化聚集，形成表面疏水缔合物构成的双层亚胶束结构，提高咖啡渣吸附材料的疏水性，克服了活性炭的高亲水性和吸油能力低等问题。
本发明的第三个发明目的在于：本发明引入天然高分子产物壳聚糖作为改性剂，使其与咖啡渣中的纤维素以氢键和物理缠结相互作用，在海水中可形成天然凝胶浮于海水表面，且长时间疏水保油，克服了活性炭材料吸油后沉降、不易回收和低保油率等不足。
为达到上述目的，本发明通过以下技术方案实现：
1)将新鲜的废弃咖啡渣通过Tyler 35目筛进行筛分，筛分后咖啡渣用超纯水清洗、过滤后置于100℃的真空烘干箱中干燥至恒重，得到干燥粉末；
2)将海泡泥置于烧杯中，向烧杯中不断加入1.0mol/L NaOH溶液，直到溶液刚好没过海泡泥的表面后，100r/min机械搅拌8h，过滤、用超纯水清洗至中性，100℃干燥至恒重，得到NaOH浸海泡泥；
3)向步骤1)所述的干燥粉末中依次缓慢加入步骤2)所述的NaOH浸海泡泥、100mL1mol/L的FeCl3溶液和100mL的1mol/L天然有机酸，40℃水浴下，100r/min机械搅拌12h后真空抽滤，用超纯水清洗至中性，100℃干燥至恒重，得到咖啡渣炭土混合体；
4)将步骤3)所述的咖啡渣炭土混合体置于10mL/min的流速加压N2保护的马弗炉中，300℃焙烧40min后，炉冷至室温20min后取出，得到黑色炭土粉末；
5)将步骤4)所述的黑色炭土粉末溶解于NaOH(6wt.％)-尿素(12wt.％)-超纯水(82wt.％)混合溶液中，在-12℃水浴中快速机械搅拌8min后，加入壳聚糖粉末，在-12℃水浴中快速机械搅拌30min后，得到均匀的黑色溶液；
6)将步骤5)所述的黑色溶液过滤后，置于-25℃真空冷冻干燥机中冷冻干燥24h，得到黑色冷冻粉末；
7)将步骤6)所述的黑色冷冻粉末在室温自然解冻后，置于100mL十六烷基磺丙基甜菜碱超纯水溶液中，置于超声振荡器中振荡15min，使黑色粉末均匀分散在溶液中。后把混合液置于60℃水浴锅中，继续机械搅拌4h后，用0.45μm PTFE滤膜抽滤，利用无水乙醇和超纯水多次冲洗黑色滤出固体直至滤液无泡沫后，将黑色滤出固体于100℃真空干燥24h，即得到改性废弃咖啡渣生物炭吸附材料。
其中，本发明所涉及的原料组分(重量百分比wt％.)：37.76％-45.45％废弃咖啡渣、22.72％-36.76％海泡泥、10.74％-13.63％壳聚糖、14.71％-18.18％十六烷基磺丙基甜菜碱；所述步骤3)中天然有机酸为奎宁酸、柠檬酸、酒石酸、苹果酸等一种或两种。天然有机酸能够与咖啡渣炭土中的金属离子形成有机盐，扩大碳晶体之间的距离，在炭土表面及内部形成多活性位点。
本发明的有益效果是：
1、本发明提供一种由废弃咖啡渣制备的新型吸附材料，用于吸附海洋油污染物。该吸附材料具有成本低廉、合成工艺简单，克服了目前吸油材料所存在成本高、吸油时间长和保油率低等不足，吸油后所得油炭的点火温度为210.78℃，可作为是潜在替代燃料使用，从而实现废物再利用，具有大规模商业化应用的潜能。
2、本发明提供一种改性废弃咖啡渣生物炭吸附材料及其制备方法和应用，海泡泥作为矿土改性剂，可增加咖啡渣生物炭材料的比表面积和孔隙率，使材料整体更加疏松多孔；通过十六烷基磺丙基甜菜碱与咖啡渣通过阳离子交换作用附着在咖啡渣表层，利用疏水作用力发生有序化聚集，形成表面疏水缔合物构成的双层亚胶束结构，提高咖啡渣吸附材料的疏水性。
3、本发明提供一种改性废弃咖啡渣生物炭吸附材料及其制备方法和应用，引入天然高分子产物壳聚糖作为改性剂，使其与咖啡渣中的纤维素以氢键和物理缠结相互作用，在海水中可形成天然凝胶，可长时间疏水保油，减少咖啡渣飘散于海水表面，便于回收。
附图说明
图1为用于处理海洋溢油污染的改性废弃咖啡渣生物炭的制备步骤图。
图2为用于处理海洋溢油污染的改性废弃咖啡渣生物炭的红外光谱图。
图3为用于处理海洋溢油污染的改性废弃咖啡渣生物炭的X射线衍射分析图。
图4为用于处理海洋溢油污染的改性废弃咖啡渣生物炭的扫描电镜图。
图5为用于处理海洋溢油污染的改性废弃咖啡渣生物炭的氮气吸附-脱附图。
图6为用于处理海洋溢油污染的改性废弃咖啡渣的吸附动力学拟合图。
图7为用于处理海洋溢油污染的改性废弃咖啡渣的接触角图。
图8为用于处理海洋溢油污染的吸附材料的比表面积对比图。
图9为不同吸附材料的吸附能力图
图10为不同吸附材料的保油能力图。
图11为柴油吸附后不同咖啡渣材料的热重曲线图。
具体实施方式
下面将结合实施例对本发明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；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。
一、用与海洋溢油污染处理的改性废弃咖啡渣生物炭的制备的实施例1：
将新鲜的废弃咖啡渣通过Tyler 35目筛进行筛分，筛分后咖啡渣用超纯水清洗、过滤后置于100℃的真空烘干箱中干燥至恒重，取出待用；将海泡泥置于烧杯中，向烧杯中不断加入1.0mol/L NaOH溶液，直到溶液刚好没过海泡泥的表面后，100r/min机械搅拌8h，过滤、用超纯水清洗至中性，100℃干燥至恒重，即得到碱浸海泡泥。
向38.15wt.％干燥废弃咖啡渣粉末中缓慢加入33.75wt.％NaOH浸海泡泥、100mL1mol/L的FeCl3溶液和100mL的1mol/L奎宁酸，40℃水浴下，100r/min机械搅拌12h后真空抽滤，用超纯水清洗至中性后100℃干燥至恒重；随后，将干燥的混合物置于10mL/min的流速加压N2保护的马弗炉中，300℃焙烧40min后，炉冷至室温20min后取出；将干燥后的粉末溶解于100mL NaOH(6wt.％)-尿素(12wt.％)-超纯水(82wt.％)混合溶液中，在-12℃水浴中快速机械搅拌8min后，加入12.68wt.％壳聚糖粉末，在-12℃水浴中继续搅拌30min后，过滤置于-25℃真空冷冻干燥机中冷冻干燥24h后，将冷冻粉末在室温自然解冻后，置于100mL十六烷基磺丙基甜菜碱(15.42wt.％)超纯水溶液中，置于超声振荡器中振荡15min，使黑色粉末均匀分散在溶液中，后把混合液置于60℃水浴锅中，继续机械搅拌4h后，用0.45μm PTFE滤膜抽滤，利用无水乙醇和超纯水多次冲洗黑色滤出固体直至滤液无泡沫后，将黑色滤出固体于100℃真空干燥24h，即得到改性废弃咖啡渣生物炭吸附材料。
实施例2：
将新鲜的废弃咖啡渣通过Tyler 35目筛进行筛分，筛分后咖啡渣用超纯水清洗、过滤后置于100℃的真空烘干箱中干燥至恒重，取出待用；将海泡泥置于烧杯中，向烧杯中不断加入1.0mol/L NaOH溶液，直到溶液刚好没过海泡泥的表面后，100r/min机械搅拌8h，过滤、用超纯水清洗至中性，100℃干燥至恒重，即得到碱浸海泡泥。
向45.00wt.％干燥废弃咖啡渣粉末中缓慢加入26.86wt.％NaOH浸海泡泥、100mL1mol/L的FeCl3溶液和100mL的1mol/L柠檬酸，40℃水浴下，100r/min机械搅拌12h后真空抽滤，用超纯水清洗至中性后100℃干燥至恒重；随后，将干燥的混合物置于10mL/min的流速加压N2保护的马弗炉中，300℃焙烧40min后，炉冷至室温20min后取出；将干燥后的粉末溶解于100mL NaOH(6wt.％)-尿素(12wt.％)-超纯水(82wt.％)混合溶液中，在-12℃水浴中快速机械搅拌8min后，加入10.90wt.％壳聚糖粉末，在-12℃水浴中继续搅拌30min后，过滤置于-25℃真空冷冻干燥机中冷冻干燥24h后，将冷冻粉末在室温自然解冻后，置于100mL十六烷基磺丙基甜菜碱(17.24wt.％)超纯水溶液中，置于超声振荡器中振荡15min，使黑色粉末均匀分散在溶液中，后把混合液置于60℃水浴锅中，继续机械搅拌4h后，用0.45μm PTFE滤膜抽滤，利用无水乙醇和超纯水多次冲洗黑色滤出固体直至滤液无泡沫后，将黑色滤出固体于100℃真空干燥24h，即得到改性废弃咖啡渣生物炭吸附材料。
实施例3：
将新鲜的废弃咖啡渣通过Tyler 35目筛进行筛分，筛分后咖啡渣用超纯水清洗、过滤后置于100℃的真空烘干箱中干燥至恒重，取出待用；将海泡泥置于烧杯中，向烧杯中不断加入1.0mol/L NaOH溶液，直到溶液刚好没过海泡泥的表面后，100r/min机械搅拌8h，过滤、用超纯水清洗至中性，100℃干燥至恒重，即得到碱浸海泡泥。
向40.19wt.％干燥废弃咖啡渣粉末中缓慢加入31.87wt.％NaOH浸海泡泥、100mL1mol/L的FeCl3溶液和100mL的1mol/L奎宁酸，40℃水浴下，100r/min机械搅拌12h后真空抽滤，用超纯水清洗至中性后100℃干燥至恒重；随后，将干燥的混合物置于10mL/min的流速加压N2保护的马弗炉中，300℃焙烧40min后，炉冷至室温20min后取出；将干燥后的粉末溶解于100mL NaOH(6wt.％)-尿素(12wt.％)-超纯水(82wt.％)混合溶液中，在-12℃水浴中快速机械搅拌8min后，加入13.20wt.％壳聚糖粉末，在-12℃水浴中继续搅拌30min后，过滤置于-25℃真空冷冻干燥机中冷冻干燥24h后，将冷冻粉末在室温自然解冻后，置于100mL十六烷基磺丙基甜菜碱(14.74wt.％)超纯水溶液中，置于超声振荡器中振荡15min，使黑色粉末均匀分散在溶液中，后把混合液置于60℃水浴锅中，继续机械搅拌4h后，用0.45μm PTFE滤膜抽滤，利用无水乙醇和超纯水多次冲洗黑色滤出固体直至滤液无泡沫后，将黑色滤出固体于100℃真空干燥24h，即得到改性废弃咖啡渣生物炭吸附材料。
二、用于海洋溢油污染处理的改性废弃咖啡渣生物炭的吸附性能测试及表征。
图2为用于海洋溢油污染处理的改性废弃咖啡渣生物炭的红外光谱图，其中，a为废弃咖啡渣，b为复合改性废弃咖啡渣生物炭；由图2可以看到，改性后咖啡渣生物炭分子中的羟基和羧基含量降低，且在1637cm-1处的峰发生了些许的移动，这是由于咖啡渣中的纤维素与壳聚糖分子之间存在氢键相互作用所致；同时，在2800-2400cm-1处出现了C-H中-CH2-和-CH3的振动峰，表明改性咖啡渣表面的烷基结构数量增加，表明十六烷基磺丙基甜菜碱附着在咖啡渣表面；1056cm-1和760cm-1处的Si-O和Si-O-Si伸缩振动峰明显增强，证明咖啡渣与海泡泥较好地结合。由曲线b可证明海泡泥、壳聚糖和十六烷基磺丙基甜菜碱分别与咖啡渣反应，附着于废弃咖啡渣表面，增加其疏水性能。图3为用于处理海洋溢油污染的改性废弃咖啡渣生物炭的X射线衍射分析图。其中，a为废弃咖啡渣，b为复合改性废弃咖啡渣生物炭；与废弃咖啡渣对比，复合改性未改变废弃咖啡渣的结构，在2θ＝28.23°处的峰值出现了左移，说明改性后材料的晶胞参数变大，晶面间距变大，使其层间距增大，对海洋溢油污染具有更强的吸附力。图4为阴极材料的扫描电镜图，其中，a为废弃咖啡渣，b为复合改性废弃咖啡渣生物炭。由图可知，相比与未改性咖啡渣，改性后材料为表面粗糙的颗粒堆叠结构，未出现团聚现象，各个颗粒彼此之间堆叠组建起大量孔隙结构，使材料具有高孔隙率和大比表面积，为油分子提供大量的吸附位点，进而提升材料的吸附能力。图5为用于处理海洋溢油污染的改性废弃咖啡渣生物炭的氮气吸附-脱附图。由图可知复合改性咖啡渣材料的吸附-脱附曲线符合Ⅱ型等温线模型，且均拥有H3型迟滞环，说明复合材料中存在着缝隙状孔洞结构，当相对压力达到0.4-1.0时，出现毛细管凝结的单层吸附现象，这意味着其表面存在大量介孔和大孔结构。图6为用于处理海洋溢油污染的改性废弃咖啡渣的吸附动力学拟合图。由图6可知，复合材料伪二级动力学拟合系数R2＝0.9866趋近于1，这表示伪二级动力学吸附方程能够更加准确地反应出其对油污的吸附过程。因此，复合改性废弃咖啡渣生物炭通过与油污形成化学键，以化学吸附为主要吸附方式处理海洋溢油。
图7为用于处理海洋溢油污染的改性废弃咖啡渣的接触角图，如图可知，复合改性后材料的接触角均大于100°，表现出良好的疏水性，有利于其浮于海水表面。图8为用于处理海洋溢油污染的吸附材料的比表面积对比图。通过比表面积分析表对比可知，复合材料的比表面积及孔容与废弃咖啡渣相比均有明显提高，且高于普通的活性炭吸附材料，这表明复合改性剂可以增加咖啡渣的比表面积和孔径，这与XRD和SEM得出的结论保持一致。图9为不同吸附材料的吸附能力图，其中，复合改性咖啡渣实例1-3最大吸附量分别为33.75g/g、33.82g/g和32.92g/g，高于未改性的废弃咖啡渣吸附材料，证明复合改性咖啡渣吸附材料具有更好的吸附能力。图10为不同吸附材料的保油能力图。从图中可以看出，实例1-3的复合改性咖啡渣吸附材料在吸附后随着时间变化，内部含油量逐渐下降并趋于平衡。在180min内保油率均达到达到90％以上，这表明复合改性咖啡渣吸附材料亲油性提高，对油分子的结合力增强，具有较好的保油能力。图11为柴油吸附前后复合改性咖啡渣材料的热重曲线图，其中a为吸油后的废弃咖啡渣材料，b为吸油后复合改性咖啡渣材料，c为柴油。从图11可知，在DTG曲线中，改性前后的咖啡渣曲线均出现三个峰，分别是咖啡渣中的全纤维素的燃烧、咖啡渣中的木质素的燃烧和咖啡渣高温焦炭氧化，说明改性前后其热稳定性没有改变，且油炭在空气中燃烧，柴油与咖啡渣没有其他副反应发生；同时，基于交集法计算法，吸附柴油后改性后的废弃咖啡渣油渣材料的点燃温度为210.78℃，接近柴油的点火温度，这表明吸油后的咖啡渣形成的油炭渣可作为一种潜在可行的替代生物燃料使用。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (5)
1.一种改性废弃咖啡渣生物炭吸附材料的制备方法，其特征在于，包括以下步骤：
1）将新鲜的废弃咖啡渣通过Tyler 35目筛进行筛分，筛分后咖啡渣用超纯水清洗、过滤后置于100℃的真空烘干箱中干燥至恒重，得到干燥粉末；
2）将海泡泥置于烧杯中，向烧杯中不断加入1.0mol/L NaOH溶液，直到溶液刚好没过海泡泥的表面后，100r/min机械搅拌8h，过滤、用超纯水清洗至中性，100℃干燥至恒重，得到NaOH浸海泡泥；
3）向步骤1）所述的干燥粉末中依次缓慢加入步骤2）所述的NaOH浸海泡泥、100 mL1mol/L的FeCl3溶液和100mL的1mol/L天然有机酸，40℃水浴下，100r/min机械搅拌12h后真空抽滤，用超纯水清洗至中性，100℃干燥至恒重，得到咖啡渣炭土混合体；
4）将步骤3）所述的咖啡渣炭土混合体置于10 mL/min的流速加压N2保护的马弗炉中，300℃焙烧40min后，炉冷至室温20min后取出，得到黑色炭土粉末；
5）将步骤4）所述的黑色炭土粉末溶解于6wt.%NaOH 、12wt.%尿素、82wt.%超纯水混合溶液中，在-12℃水浴中快速机械搅拌8min后，加入壳聚糖粉末，在-12℃水浴中快速机械搅拌30min后，得到均匀的黑色溶液；
6）将步骤5）所述的黑色溶液过滤后，置于-25℃真空冷冻干燥机中冷冻干燥24h，得到黑色冷冻粉末；
7）将步骤6）所述的黑色冷冻粉末在室温自然解冻后，置于100mL十六烷基磺丙基甜菜碱超纯水溶液中，置于超声振荡器中振荡15min，使黑色粉末均匀分散在溶液中；后把混合液置于60℃水浴锅中，继续机械搅拌4h后，用0.45 μm PTFE滤膜抽滤，利用无水乙醇和超纯水多次冲洗黑色滤出固体直至滤液无泡沫后，将黑色滤出固体于100℃真空干燥24h，即得到改性废弃咖啡渣生物炭吸附材料。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤3）中天然有机酸为奎宁酸、柠檬酸、酒石酸或苹果酸中一种或两种；天然有机酸能够与咖啡渣炭土中的金属离子形成有机盐，扩大碳晶体之间的距离，使炭土表面及内部形成多活性位点。
3. 根据权利要求1所述的制备方法，其特征在于，所述步骤3）中的干燥粉末38.15wt.%-45 wt.%。
4. 根据权利要求1所述的制备方法，其特征在于，所述步骤3）中的NaOH浸海泡泥为26.86wt.%- 33.75wt.%。
5.一种利用权利要求1-4中任一项所述制备方法制备的改性废弃咖啡渣生物炭吸附材料，其特征在于，包括以下原料组分重量百分比wt%.为：37.76%-45.45% 废弃咖啡渣、22.72%-36.76%海泡泥、10.74%-13.63%壳聚糖、14.71%-18.18%十六烷基磺丙基甜菜碱。
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