CN106977727B - 端氨基超支化聚酰胺氯化改性花生壳的制备方法及其在水中重金属的分离检测中的应用 - Google Patents
端氨基超支化聚酰胺氯化改性花生壳的制备方法及其在水中重金属的分离检测中的应用 Download PDFInfo
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
本发明提供了一种端氨基超支化聚酰胺氯化改性花生壳及其在水中重金属的分离检测中的应用。所述端氨基超支化聚酰胺氯化改性花生壳对重金属具有很强的吸附分离效果,同时具有优良的循环再生性能。
Description
技术领域
本发明属于化学技术领域,特别涉及一种端氨基超支化聚酰胺氯化改性花生壳的制备方法及其应用。
背景技术
超支化聚合物,具有多端基的″缺陷核壳″空间结构,化学反应活性高,易于改性,与相应的线型聚合物相比,拥有特殊的性能,在多领域展现出广阔的应用前景。超支化聚合物不仅具有与树枝聚合物相似的物理化学性质″,而且与树枝聚合物相比,其对合成条件要求较为温和,不需要多步合成与提纯,合成工艺简单,成本较低,可以实现″一锅煮式″合成,有利于实现工业化。因此,超支化聚合物越来越取代树枝化大分子成为人们研究的重点。目前,已合成出多种类型的超支化聚合物,如超支化聚苯、超支化聚酯、超支化聚醚、超支化聚酰胺等,并广泛应用于农业、医药、化妆品等行业,如作为涂料、黏合剂等。
花生壳主要组成成分有纤维素、木质素及半纤维素。花生壳中粗纤维含量为65.7%~79.3%;粗脂肪含量为1.2%~1.8%;粗蛋白含量为4.8%~7.2%;可溶性糖类化合物含量为10.6%~21.2%;同时矿物质含量也较为全面,如氮1.09%、磷0.06%、钾0.57%、钙0.20%、镁0.07%、硼13mg/kg、铜10mg/kg、锌13mg/kg、铝454mg/kg、锶262mg/kg、钡16mg/kg、铁262mg/kg、锰45mg/kg、钠66mg/kg。根据刘启明等的研究结果表明,花生壳中的纤维素大部分是葡萄糖和木糖,含有较多半乳糖和相对较少的阿拉伯糖,已糖与戊糖的比为3.4∶1;纤维素是很多个含酚羟基的单糖组成的高分子聚合体;单糖酚羟基上的氢原子十分活跃,可以除去重金属离子和染料等。
电镀、有色金属开采或冶炼产生的废水、废气和废渣中会有大量的铅;作为抗爆剂加入汽油中的四乙基铅,使得汽油燃烧过程中产生的废气也会含铅;另外,制革业、化工行业和蓄电池回收产业产生的废弃物中也含有一定量的铅。研究表明,水溶液中Pb2+离子的存在形式有Pb(OH)+,Pb(OH)2,Pb(OH)3-,Pb2(OH)3+,Pb4(OH)44+,Pb6(OH)84+等。在酸性条件下,Pb2+离子主要以游离状态存在。这些含铅物质可以通过食物、饮用水等进入机内,与机体内的酶和蛋白结构上的S-S键和S-H键发生相互作用,使酶失去活性,蛋白质变性,干扰机体正常的新陈代谢和生理作用,使机体组织细胞结构和功能受到损害。铅中毒会对人体健康造成极大危害,它能够对神经系统、消化系统、骨骼造血功能以及男性生殖系统造成持久甚至永久伤害,尤其是对大脑神经系统正处于发育敏感期的儿童的毒害更大。″血铅″事件是铅离子污染危害人体的代表例子。儿童铅中毒往往会表现出注意力无法集中、反应迟钝、性格暴躁,还会表现出腹痛、视觉障碍、食欲下降和颅神经瘫痪等症状。且儿童智力低下的发病率会随铅污染程度的加大而增大,表现为儿童体内血铅每升高0.01mg/mL,智商就降低1分。当血铅含量超过1mg/L时,会出现铅性脑病的症状,如头疼、呕吐、惊厥甚至昏迷,严重的会导致死亡。
治理水中重金属污染的方法可分为化学治理、物理治理和生物治理三大类。常用的方法主要有化学沉淀法、离子交换法、膜过滤法、吸附法和光催化法等。
发明内容
本发明针对以上缺点,提供了一种端氨基超支化聚酰胺氯化改性花生壳,以达到有效从水中分离检测重金属的目的。
为实现上述目的,本发明采取下述技术方案来实现:
本发明提供一种端氨基超支化聚酰胺氯化改性花生壳的制备方法,所述制备方法包括以下步骤:
花生壳的预处理,将花生壳洗净、烘干后制成粉末;
花生壳的碱化:将花生壳粉末浸泡在碱液中,得到碱化花生壳粉末;
花生壳的氯化:将碱化后的花生壳粉末与N,N-二甲基酰胺和氯化亚砜反应,得到氯化花生壳粉末;
端氨基超支化聚酰胺的制备:冰浴下向二乙烯三胺中加入丙烯酸甲酯和甲醇混合液反应,得淡黄色液;然后将该产物在60℃反应1h;然后转到油浴锅里,从100℃开始,每过一小时增加二十摄氏度共油浴3h,得到端氨基超支化聚酰胺;
端氨基超支化聚酰胺氯化花生壳:向氯化花生壳粉末加入DMSO,搅拌均匀,然后加入端氨基超支化聚酰胺进行反应,得到端氨基超支化聚酰胺氯化改性花生壳。
进一步,花生壳的碱化时,将预处理得到的花生壳粉末倒入三颈瓶内,泡在摩尔浓度为5mol/L的氢氯化钠溶剂,隔日后用100目尼龙纱布滤去碱液;之后用去离子水冲洗数遍直至洗出液测量显示中性,放置真空干燥箱中除水烘干。
进一步,花生壳氯化时,花生壳氯化时,将碱化的花生壳粉末三颈瓶中,加入N,N-二甲基酰胺水浴加热至溶剂温度升高到40℃,用滴液漏斗缓缓滴加氯化亚砜;然后待水浴温度缓慢升达90℃,维持2.5h,得到产物;等待三口瓶中的产物完全冷却后,将其缓缓倒入冷水中,在此过程中持续搅拌;然后用真空泵抽滤,丙酮冲洗去酸后,用去离子水冲至中性,放入50℃真空干燥箱中烘干至恒重,得氯化花生壳。
进一步端氨基超支化聚酰胺氯化花生壳时,4.将氯化花生壳粉末,倒于三颈瓶内,二甲基亚砜,水浴加热升温至60℃,缓慢滴加端氨基超支化聚酰胺,维持此温度,持续搅动反应14小时,得深棕色液体产品,自然状态下待其温度降至常温,向其中倒入冷水,抽滤得到端氨基超支化聚酰胺氯化花生壳。
进一步,氯化花生壳粉末与端氨基超支化聚酰胺的反应温度为60℃。
进一步,氯化花生壳粉末与端氨基超支化聚酰胺的反应时间为14h。
进一步,端氨基超支化聚酰胺与氯化花生壳粉末反应时的质量比为4。
本发明还提供一种上述的端氨基超支化聚酰胺氯化改性花生壳的制备方法得到的端氨基超支化聚酰胺氯化改性花生壳在水中重金属的分离检测中的应用。
进一步,端氨基超支化聚酰胺氯化改性花生壳吸附重金属,从而从水中分离出来;吸附反应的pH值为5。
进一步,吸附反应后解吸剂为硝酸。
总之,本发明的有益效果为:本发明的端氨基超支化聚酰胺氯化改性花生壳对重金属的吸附能力强,且具有良好的再生性能,具备循环利用价值。
采用本发明的方法合成的端氨基超支化聚酰胺氯化改性花生壳,具有如下优点:
1、本发明本发明利用化学超支化接枝法制得的端氨基超支化聚酰胺氯化改性花生壳的机械强度和物理稳定性,制备简单易行;
2、本发明方法制得的端氨基超支化聚酰胺氯化改性花生壳能更好的检测和吸附工业废水废渣中重金属离子中的Pb(II)离子,能很好地应用于工业废水废渣中重金属离子中的Pb(II)离子的快速检测和吸附,并且吸附量大,达到460mg/g,远远超过已研发出的基础方法多倍,甚至更高,具有较大的经济价值与优势;
3、本发明以花生壳为母体通过超支化反应制备新型端氨基超支化聚酰胺氯化改性花生壳,较好地体现了绿色化学的特征:原料的原子利用率高(原料中的原子尽可能多地转化到产品中);不向或少向环境中排放有毒有害的副产物,具备优良的再生性能,重复使用性好,节约成本,保护环境;
4、本发明制得的新端氨基超支化聚酰胺氯化改性花生壳吸附剂化学稳定性好,容易洗脱(只需要少量HNO3溶液就可以达到93.5%的洗脱),具有更为优良再生和重复使用性能,减少了二次污染。
综上所述,本发明研究表明:以以花生壳为母体通过超支化反应制备新型端氨基超支化聚酰胺氯化改性花生壳,较好地体现了绿色化学的特征:原料的原子利用率高(原料中的原子尽可能多地转化到产品中);不向或少向环境中排放有毒有害的副产物。而且本发明首次选用对Pb(II)离子具有选择性配位能力的含N、S、O等原子的有机配体,据此合成出了一种性能优异的新型端氨基超支化聚酰胺氯化改性花生壳Pb(II)离子吸附剂,应用于Pb(II)离子的选择性分离富集中。以该法合成的端氨基超支化聚酰胺氯化改性花生壳较其他合成物质具有较高的机械强度、较好的热稳定性,且对Pb(II)离子具有很好的吸附及检测作用,吸附容量大,重复使用性能好,有望在离子的分离富集方面得到广泛应用。
附图说明
图1是预处理后的花生壳粉末的SEM图片。
图2是碱化花生壳粉末的SEM图片。
图3是端氨基超支化聚酰胺氯化改性花生壳的SEM图片。
图4是端氨基超支化聚酰胺氯化改性花生壳吸附重金属后的图片。
图5是反应温度对端氨基超支化聚酰胺氯化改性花生壳的影响。
图6是反应物质量比对端氨基超支化聚酰胺氯化改性花生壳的影响。
图7是反应温时间对端氨基超支化聚酰胺氯化改性花生壳的影响。
图8是pH值对端氨基超支化聚酰胺氯化改性花生壳吸附重金属的影响。
图9是溶液初始浓度对端氨基超支化聚酰胺氯化改性花生壳吸附重金属的影响。
具体实施方式
下面结合附图和具体实施例对本发明进行详细描述。
一、改性前的准备:
1花生壳的预处理
先用自来水多次洗刷清理花生壳,去掉体表上的泥土、灰尘等。然后用去离子水冲洗数遍后,放置50℃鼓风干燥箱中烘干至恒重。然后放入粉碎机粉碎二、三分钟,至花生壳成粉末状,过100目筛,得到的花生壳粉末用密封袋密封好,存于真空干燥器内。图1是预处理后的花生壳粉末的SEM图片。
2花生壳粉的碱化
称取一定量预处理得到的花生壳粉末倒入三颈瓶内,泡在用0.2L摩尔浓度为5mol/L的氢氯化钠溶剂,隔日后用100目尼龙纱布滤去碱液。之后用去离子水冲洗数遍直至洗出液测量显示中性,放置50℃真空干燥箱中除水烘干燥数小时称量呈恒重后备用。图2是碱化花生壳粉末的SEM图片。
3花生壳粉的氯化
准确称取碱化好的花生壳粉末物2g于三口瓶中(装有搅拌器,转速150r/min;恒压滴液漏斗;冷凝管上口加装干燥管),再加入60mL N,N-二甲基酰胺(水浴封),用水浴锅加热至溶剂温度升高到6℃时,用滴液漏斗缓缓滴加氯化亚砜7mL。然后待水浴锅水温缓缓升达90℃,维持2.5h,得深褐色黏性产物。等待三口瓶中的产物完全冷却后,将其缓缓倒入100mL冷水中,在此过程中持续搅拌。然后用真空泵抽滤,丙酮冲洗去酸后,用去离子水冲至中性,放入50℃真空干燥箱中烘干至恒重,得氯化花生壳。
4端氨基超支化聚酰胺的制备
实施例1
准确量取103.17g二乙烯三胺于500mL三颈瓶中,冰浴状态下滴加86.09g丙烯酸甲酯和100mL甲醇混合液。持续搅拌反应16h后得淡黄色液体。将该产物转移至旋转蒸发仪的茄形瓶内,用循环水式真空泵抽真空,回流冷凝,高速旋转,在水浴温度60℃反应1h。然后转到油浴锅里,从100℃开始,每过一小时增加二十摄氏度共油浴3h,得最终产品端氨基超支化聚酰胺HBP-NH2,然后加入同质量去离子水配置成质量分数为50%的HBP-NH2备用。
二、端氨基超支化聚酰胺氯化改性花生壳的制备
端氨基超支化聚酰胺氯化改性花生壳合成路线入下式所示:
实施例2
本实施例中端氨基超支化聚酰胺氧化改性花生壳的实验方法为:
准确称量2g氯化花生壳粉,倒于150mL的装有冷凝管和搅拌器三口瓶中,再加入60mL DMSO,水浴加热升温至60℃,缓慢滴加4mL超支化聚合物HBP-NH2,维持此温度,持续搅动反应14小时,得深棕色液体产品自然状态下待其温度降至常温,向其中倒入100mL冷水,隔夜后抽滤。
对比例1
将实施例2反应温度改为40℃,50℃,80℃,100℃的条件下进行反应,其余完全同实施例的步骤相同,从而探讨反应温度对合成端氨基超支化聚酰胺氯化改性花生壳功能基转化率的影响。
所得的含氮量分别可以从图5中看出,温度在一定程度上影响了配体的接枝,制备端氨基超支化聚酰胺氯化改性花生壳的最佳温度为60℃,高于或低于此温度后含氮量皆有所下降。
对比例2
将实施例2反应物摩尔比改为1,2,3,5的条件下进行反应,其余完全同实施例的步骤相同,从而探讨反应物摩尔比对合成端氨基超支化聚酰胺氯化改性花生壳功能基转化率的影响。
所得的含氮量N分别可以从图6中看出,反应物摩尔比在一定程度上影响了配体的接枝,制备端氨基超支化聚酰胺氯化改性花生壳的最佳反应物摩尔比为4,高于或低于此反应物摩尔比后含氮量皆有所下降。
对比例3
将实施例2反应时间改为8,10,12,16的条件下进行反应,其余完全同实施例的步骤相同,从而探讨反应时间对合成端氨基超支化聚酰胺氯化改性花生壳功能基转化率的影响。
所得的含氮量N分别可以从图7中看出,反应时间在一定程度上影响了配体的接枝,制备端氨基超支化聚酰胺氯化改性花生壳的最佳反应时间为14,高于或低于此反应时间后含氮量皆有所下降。
对比例4
将实施例2中的4mL质量分数50%的超支化聚合物(HBP-NH2)改为2ml二乙烯三胺(分析纯),其余完全同实施例2的步骤,合成的改性花生壳含氮量为3.31%。相比较而言,用50%的超支化聚合物(HBP-NH2)合成的改性花生壳合氮量更高。
图3是端氨基超支化聚酰胺氯化改性花生壳的SEM图片。
图1至图3呈现的是花生壳被物理、化学处理前后的电镜图。图1是未处理的花生壳粉末,表面光滑,图片上出现的水滴状物质应该是样品为完全干燥,残余的水分。图2是20%氢氧化钠处理后的花生壳粉末,与图1相比,花生壳表面变得粗糙,内部分子与分子间的距离明显增大,这说明分子之间的和分子内部的很多氢键发生断裂,分子链上的部分羟基被打开,有利于配体超支化聚合物的接枝。图3与图2相比,花生壳的表面出现有更多的微孔和中孔,孔系增大,孔结构均匀分散各处,片层结构构造清晰可见并规律性排布,这说明改性后的花生壳孔道被大程度打开,比表面积增大,趋向适于重金属的吸附方向发展。
图4是吸附吸附Pb(II)离子后的电镜图。
如图4所示,与吸附前相比,花生壳表面和大量片层的孔道变得模糊,花生壳表面出现许多微小颗粒,这说明有大量Pb(II)离子被花生壳吸附,进入空隙和偏侧间隙。
三、对重金属的吸附实验
1、静态吸附实验
准确称取一定量的改性花生壳,加入25mL的乙酸-乙酸钠(HAc-NaAc)缓冲溶液浸泡24h,再加入一定浓度的重金属离子溶液5mL,以不加花生壳的溶液做空白对照,在150rpm转速下恒温振动箱中振荡,至平衡后ICP法准确测定溶液中剩余的金属离子浓度,吸附量的计算公式如下:
式中:Co(mg/mL)为吸附前金属离子浓度;Ce(mg/mL)为吸附平衡后金属离子浓度;Q(mg/g)为饱和吸附量;V(mL)为溶液体积。
2、静态解吸性能研究
将吸附饱和后的改性花生壳用上述吸附最佳HAC-NaAC缓冲溶液洗涤数次并滤出,晾干后加入不同种类的解吸剂进行探讨,通过测定振荡平衡后溶液中重金属离子浓度计算出解吸率。其中,解吸率E(%)按下式计算:
式中:Cd(mg/mL)为解吸液中金属离子的平衡浓度;Vd(mL)为解吸液体积;Co、Ce和V同上。
3、pH值对花生壳静态吸附量的影响
溶液的pH影响水溶液中重金属离子的存在形式和改性花生壳的性质,因此,有必要选择适宜的pH。准确称取20.0mg充分干燥的改性花生壳置于碘量瓶中,加入25mL不同pH的HAC-NaAC缓冲溶液浸泡24h后,加入5mL的3mg/mL的重金属离子溶液,于25℃的恒温振荡器中振荡,转速150r/min。每间隔一段时间,测定溶液中剩余金属离子的浓度,直至浓度不变即可判断吸附达平衡。根据吸附公式计算出改性花生壳对金属离子的静态饱和吸附量,从而研究pH对改性花生壳吸附量的影响。结果如图8所示,由图8可知,HBPN-cl-P对Pb(II)离子的吸附容量很高,对其他四种重金属离子吸附量相对低,说明HBPN-cl-P对Pb(II)离子有较强的选择吸附能力,分离性能良好。HBPN-cl-P对Pb(II)离子的选择性分离效果好,吸附量随pH的变化而变化。随着pH的升高,HBPN-cl-P对Pb(II)离子的吸附量明显增大,在pH=5.0时达到最大,吸附量为460mg/g,而当pH继续增大时,吸附量反而降低。
4、溶液浓度对花生壳静态吸附量的影响
准确称取20.0mg充分干燥的改性花生壳置于碘量瓶中,加入25mL最佳pH的HAC-NaAC缓冲溶液浸泡24h后,加入5mL的不同浓度的重金属离子溶液,于25℃的恒温振荡器中振荡,转速150r/min。每间隔一段时间,测定溶液中剩余金属离子的浓度,直至浓度不变即可判断吸附达平衡。根据静态吸附公式计算出改性花生壳对金属离子的静态饱和吸附量,从而研究溶液浓度对改性花生壳吸附量的影响。结果如图9所示,由图9可以清楚看到,溶液初始浓度从100ppm增大到500ppm左右的过程中,随着Pb(II)离子浓度的增大,HBPN-cl-P对Pb(II)离子的吸附量迅速增加。当Pb(II)离子浓度超过500ppm为时,继续增大溶液浓度吸附量不变。这是由于Pb(II)离子浓度增大,增加了Pb(II)离子与HBPN-cl-P的接触机会有利于HBPN-cl-P对Pb(II)离子的吸附,因此,增大溶液初始浓度有利于HBPN-cl-P对Pb(II)离子的吸附。但当HBPN-cl-P的吸附点位被占满后,溶液中的Pb(II)离子难于被吸附,吸附量不再增加。所以,选取Pb(II)离子溶液初始浓度为500ppm。
5、端氨基超支化聚酰胺氯化改性花生壳的静态解吸性能
表1为不同解吸剂不同浓度情况下的解吸率
由上表可知,解吸效果受解吸剂的种类及浓度影响很大。HBPN-cl-P先用4mol/LHNO3洗脱,洗脱率达到99.5%,超过95%,说明HBPN-cl-P解吸性能较好。HNO3和HCI是无机酸类解吸剂,由于水中重金属吸附属于阳离子吸附形式,酸液中氢离子可以和重金属阳离子竞争吸附剂吸附位点,从而把重金属离子从吸附剂上解吸下来,且强酸会对花生壳结构造成破坏。柠檬酸属于有机酸,其酸根离子络合能力较强,能够通过络合反应与重金属离子形成可溶性有机酸-金属络合物,从而把重金属从吸附剂上解吸下来。EDTA属于络合剂类解吸剂,其络合能力强于柠檬酸,吸附剂可以各种形式与重金属离子发生络合反应,被解吸下来。因此,HBPN-cl-P的解吸主要是离子交换和结构破坏造成的。
本发明虽然已以较佳实施例公开如上,但其并不是用来限定本发明,任何本领域技术人员在不脱离本发明的精神和范围内,都可以利用上述揭示的方法和技术内容对本发明技术方案做出可能的变动和修改,因此,凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所做出的任何简单修改、等同变化及修饰,均属于本发明技术方案的保护范围。
Claims (5)
1.端氨基超支化聚酰胺氯化改性花生壳在水中重金属Pb(II)离子的分离检测中的应用,其特征在于,所述改性花生壳采用如下方法制备:
花生壳的预处理,将花生壳洗净、烘干后制成粉末;
花生壳的碱化:将花生壳粉末浸泡在碱液中,得到碱化花生壳粉末;
花生壳的氯化:向碱化后的花生壳粉末加入N,N-二甲基酰胺,用滴液漏斗缓缓滴加氯化亚砜,反应得到氯化花生壳粉末;
端氨基超支化聚酰胺的制备:冰浴下向二乙烯三胺中加入丙烯酸甲酯和甲醇混合液反应,得淡黄色液体;然后将该产物在60℃反应1h;然后转到油浴锅里,从100℃开始,每过一小时增加二十摄氏度共油浴3h,得到端氨基超支化聚酰胺;
端氨基超支化聚酰胺氯化花生壳:向氯化花生壳粉末加入二甲基亚砜,水浴加热,然后加入端氨基超支化聚酰胺进行反应,得到端氨基超支化聚酰胺氯化改性花生壳;
端氨基超支化聚酰胺氯化花生壳时,将氯化花生壳粉末,倒于三颈瓶内,加入二甲基亚砜,水浴加热升温至60℃,缓慢滴加端氨基超支化聚酰胺,维持此温度,持续搅动反应14小时,得深棕色液体产品,自然状态下待其温度降至常温,向其中倒入冷水,抽滤得到端氨基超支化聚酰胺氯化花生壳;
端氨基超支化聚酰胺与氯化花生壳粉末反应时的质量比为4。
2.如权利要求1所述的端氨基超支化聚酰胺氯化改性花生壳在水中重金属Pb(II)离子的分离检测中的应用,其特征在于,花生壳的碱化时,将预处理得到的花生壳粉末倒入三颈瓶内,泡在摩尔浓度为5mol/L的氢氯化钠溶剂,隔日后用100目尼龙纱布滤去碱液;之后用去离子水冲洗数遍直至洗出液测量显示中性,放置真空干燥箱中除水烘干。
3.如权利要求1所述的端氨基超支化聚酰胺氯化改性花生壳在水中重金属Pb(II)离子的分离检测中的应用,其特征在于,花生壳氯化时,将碱化的花生壳粉末三颈瓶中,加入 N,N-二甲基酰胺水浴加热至溶剂温度升高到40℃,用滴液漏斗缓缓滴加氯化亚砜;然后待水浴温度缓慢升达90℃,维持2.5h,得到产物;等待三口瓶中的产物完全冷却后,将其缓缓倒入冷水中,在此过程中持续搅拌;然后用真空泵抽滤,丙酮冲洗去酸后,用去离子水冲至中性,放入50℃真空干燥箱中烘干至恒重,得氯化花生壳。
4.根据权利要求1所述的端氨基超支化聚酰胺氯化改性花生壳在水中重金属Pb(II)离子的分离检测中的应用,其特征在于,端氨基超支化聚酰胺氯化改性花生壳吸附重金属Pb(II)离子,从而将重金属Pb(II)离子从水中分离出来;吸附反应的pH值为5。
5.根据权利要求4所述的端氨基超支化聚酰胺氯化改性花生壳在水中重金属Pb(II)离子的分离检测中的应用,其特征在于,吸附反应后解吸剂为硝酸。
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