CN111170439A - 一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物及其制备方法 - Google Patents
一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物及其制备方法。其特征在于所述柠檬酸/乙二胺四乙酸通过改性整理均匀牢固地附着于棉织物上,再与铁离子改性后形成柠檬酸/乙二胺四乙酸铁改性棉织物。使用本发明所述的改性整理能够使柠檬酸和乙二胺四乙酸同时整理到棉织物上,并且能够通过调节处理浴中柠檬酸和乙二胺四乙酸摩尔比来控制棉织物去除铬离子的性能。此外,以本发明所述柠檬酸/乙二胺四乙酸铁改性棉织物也可使用废旧棉织物制备,不仅更加绿色环保,还进一步降低了成本,有利于工业化的推广。
Description
技术领域
本发明涉及化工和环境保护技术领域,具体为一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物及其制备方法。
背景技术
近年来,随着工业的快速发展,尤其是含铬等重金属的工业废水排放,严重威胁生态环境和人类健康。因此,含铬污水的治理成为环保学界面临的重要研究课题。铬元素广泛存在于自然界中,其常见化合价有+2、+3、+6三种,且在环境中不同条件下有不同的价态,其化学行为和毒性大小亦不同。三价铬和六价铬对人体健康都有害,被怀疑有致癌作用。一般认为六价铬的毒性强,更易为人体吸收,而且可在体内蓄积。六价铬的毒性比三价铬要高100倍,是强致突变物质,可诱发肺癌和鼻咽癌。三价铬有致畸作用。水体中的三价铬容易被吸附在固体物质上而存在于沉积物中;六价铬则多溶于水中,处于稳定状态。因此世界各国皆把铬列为重点污染物之一,并将六价铬浓度也定为水质监测和控制的指标,如我国各种水环境质量和卫生标准及废水排放污染物限量都严格规定:生活饮用水(GB 3838-2002)中应低于0.05mg L-1Cr(VI);地表水(GB 3838-2002)和地下水(GB/T 14848-93)中铬的浓度限值为0.1mg L-1Cr(VI);污水的最高允许排放浓度(GB 8978-1996)为1.5mg L-1Cr及0.5mg L-1Cr(VI);因而对水处理技术提出了更高的要求,尤其是六价铬的去除成为首要目的。
目前,针对含铬废水采用的处理方法主要有还原-沉淀法、活性炭吸附法、电解法、离子交换法、膜分离法、微生物法等,其中应用最为广泛的是化学还原-沉淀法,即通过亚硫酸钠、偏硫酸氢盐、硫酸亚铁或二氧化硫等化学还原剂将六价铬还原为三价铬,为提高还原速率,有时需要加热,导致能耗成本高。而且,反应过程不易控制,还原效率不高。
为了节能环保,提高还原率,广泛开展了光催化还原铬的研究。Hug等研究了铁草酸盐配合物、铁柠檬酸盐配合物对Cr(VI)的光还原[Hug S J,Laubscher H U,James BR.Iron(III)Catalyzed Photochemical Reduction of Chromium(VI)by Oxalate andCitrate in Aqueous Solutions[J].Environmental Science&Technology,1997,31(1):160-170.]。Zhang等报道了Fe(III)羟基配合物对Cr(VI)的光还原[Zhang Z,Wu F,DengN.Photochemical Reduction of Cr(VI)in Aqueous Solutions Containing Fe(III)-hydroxy Complexes[J].Toxicological&Environmental Chemistry Reviews,2002,82(3-4):129-137.]。刘延湘等研究了Fe(III)-多羧酸盐配合物对Cr(VI)的光还原[刘延湘,刘君侠,吴荣,等.Fe(III)-多羧酸盐配合物光催化还原Cr(VI)[J].江汉大学学报(自然科学版),2006,34(4):40-43.]。以上研究中所提供的治理六价铬的方法中均相体系易产生铬泥污,造成二次污染,制约了它们的实际使用。
发明内容
本发明针对现有技术存在的一系列问题,使用用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物,以提供一种操作简单、成本低廉的含铬废水处理方法。
为了实现上述目的,一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物及其制备方法,其采用下述工艺:
步骤1:柠檬酸/乙二胺四乙酸改性溶液的制备:将柠檬酸与乙二胺四乙酸置于温度为40℃的水溶液中,然后加入纳米TiO2作为催化剂,其中柠檬酸/乙二胺四乙酸的总摩尔浓度为0.10至0.29摩尔/升,柠檬酸/乙二胺四乙酸的摩尔比为1∶0-3,纳米TiO2的质量分数为1.0%至5%;
步骤2:柠檬酸/乙二胺四乙酸改性工艺:将棉织物材料放入装有柠檬酸/乙二胺四乙酸改性溶液的高温高压染色机中,使棉织物材料重量(g)和柠檬酸/乙二胺四乙酸改性溶液体积(mL)之比为1∶30-50,从室温开始以1.5℃/分钟的升温速率升至80℃,然后再以1℃/分钟的升温速率升至135℃,并保温30-60分钟,最后得到柠檬酸/乙二胺四乙酸改性棉织物;
步骤3:柠檬酸/乙二胺四乙酸改性棉织物与铁离子的改性反应:将柠檬酸/乙二胺四乙酸改性棉织物浸入0.1摩尔/升氯化铁水溶液中,使柠檬酸/乙二胺四乙酸改性棉织物材料重量(g)和氯化铁改性溶液体积(mL)之比为1∶50,在50℃、pH值为1.0至3.0和搅拌条件下进行改性反应,反应进行1至3小时后得到柠檬酸/乙二胺四乙酸铁改性棉织物。
与已有技术方案相比,本发明可使柠檬酸/乙二胺四乙酸铁均匀牢固的附着在棉织物上,不仅对六价铬有极强的还原能力,且有效吸附还原出的三价铬,避免因产生铬泥污造成的二次污染。本发明的制备方法可有效利用废旧棉织物,不仅更加绿色环保,还进一步降低了成本,有利于工业化的推广。另外,本发明的处理工艺方法还具有处理操作简单、安全性高和使用适应性好等特点。
附图说明
图1为本发明实施例1-5所制备的柠檬酸/乙二胺四乙酸铁改性棉织物对六价铬的还原率;
图2为本发明实施例1-5所制备的柠檬酸/乙二胺四乙酸铁改性棉织物总铬的去除率。
具体实施方式
下面结合实施例及其附图进一步详细叙述本发明:
本发明设计的一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物及其制备方法由柠檬酸/乙二胺四乙酸改性溶液的制备、柠檬酸/乙二胺四乙酸改性工艺、柠檬酸/乙二胺四乙酸改性棉织物与铁离子的改性反应等三个主要步骤构成。该方法也适用于废旧棉织物,扩大了废旧棉的应用范围,进一步降低了成本,也更加绿色环保。
本发明实施例中所述去除铬离子的方法为:首先配制100毫升重铬酸钾浓度为0.1毫摩尔/升的铬离子水溶液,然后添加1.5克的柠檬酸/乙二胺四乙酸铁改性棉织物于其中,将上述混合物置于自行设计的光反应器内进行光催化实验,其中辐射光强度为紫外光(365nm):457微瓦/厘米2,可见光(400-1000nm):4987微瓦/厘米2,使用可见光分光光度计每间隔一定时间取样,用二苯碳酰二肼比色法测定水中的Cr(VI)浓度和用GB 7466-87来测定总Cr浓度。
本发明实施例中所述六价铬还原率(η%)和总铬去除率(R%)是通过下式计算的:
式中c0和ct分别为柠檬酸/乙二胺四乙酸铁改性棉织物光催化处理前后溶液中铬离子的浓度(mmol/L)。
下面介绍本发明的具体实施例,但本发明权利要求不受这些具体实施例的限制。
实施例1
1.柠檬酸/乙二胺四乙酸改性溶液的制备:将柠檬酸与乙二胺四乙酸置于温度为40℃的水溶液中,然后加入纳米TiO2作为催化剂,其中柠檬酸/乙二胺四乙酸的总摩尔浓度为0.28摩尔/升,柠檬酸/乙二胺四乙酸的摩尔比为1∶0,纳米TiO2的质量分数为5%;
2.柠檬酸/乙二胺四乙酸改性工艺:将棉织物材料放入装有柠檬酸/乙二胺四乙酸改性溶液的高温高压染色机中,使棉织物材料重量(g)和柠檬酸/乙二胺四乙酸改性溶液体积(mL)之比为1∶50,从室温开始以1.5℃/分钟的升温速率升至80℃,然后再以1℃/分钟的升温速率升至135℃,并保温60分钟,最后得到柠檬酸/乙二胺四乙酸改性棉织物;
3.柠檬酸/乙二胺四乙酸二钠改性棉织物与铁离子的改性反应:将柠檬酸/乙二胺四乙酸改性棉织物浸入0.1摩尔/升氯化铁水溶液中,使柠檬酸/乙二胺四乙酸改性棉织物材料重量(g)和氯化铁改性溶液体积(mL)之比为1∶50,在50℃、pH值为2.0和搅拌条件下进行改性反应,反应进行2小时后得到柠檬酸/乙二胺四乙酸铁改性棉织物。
实施例2
1.所述柠檬酸/乙二胺四乙酸的摩尔比为3∶1,其余与实施例1中的步骤1工艺相同;
2.与实施例1中的步骤2工艺相同;
3.与实施例1中的步骤3工艺相同。
实施例3
1.所述柠檬酸/乙二胺四乙酸的摩尔比为1∶1,其余与实施例1中的步骤1工艺相同;
2.与实施例1中的步骤2工艺相同;
3.与实施例1中的步骤3工艺相同。
实施例4
1.所述柠檬酸/乙二胺四乙酸的摩尔比为1∶3,其余与实施例1中的步骤1工艺相同;
2.与实施例1中的步骤2工艺相同;
3.与实施例1中的步骤3工艺相同。
实施例5
1.所述柠檬酸/乙二胺四乙酸的摩尔比为0∶1,其余与实施例1中的步骤1工艺相同;
2.与实施例1中的步骤2工艺相同;
3.与实施例1中的步骤3工艺相同。
以上实施例仅用于说明本发明的技术方案,而非对其进行限制;尽管参照前述实施例对本发明进行了详细的说明,但是对于本领域的普通技术人员来说,依然可以对前述实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或替换,并不使相应技术方案的本质脱离本发明所要求保护的技术方案的精神和范围。
从图1中可以看出,对于本发明中涉及的柠檬酸/乙二胺四乙酸铁改性棉织物,随着处理浴中柠檬酸浓度的提高,柠檬酸/乙二胺四乙酸铁改性棉织物对六价铬的还原率提高,并且在柠檬酸/乙二胺四乙酸的摩尔比为3∶1时柠檬酸/乙二胺四乙酸铁改性棉织物对六价铬的还原率比柠檬酸/乙二胺四乙酸的摩尔比为1∶0时更高。图2显示,处理浴中加入柠檬酸,柠檬酸/乙二胺四乙酸铁改性棉织物对总铬的去除率提高,且在柠檬酸/乙二胺四乙酸的摩尔比为1∶3时的还原率柠檬酸/乙二胺四乙酸铁改性棉织物对总铬的去除率最高。
综上所述,使用本发明所述的技术方法能够显著提升对六价铬的还原效率,并且提高了对总铬的去除率,同时非均相系统的应用避免了铬泥污而造成的二次污染。此外,本发明的制备方法可有效利用废旧棉织物,不仅更加绿色环保,还进一步降低了成本,有利于工业化的推广,这对于遏制重金属污染、保护生态环境具有重要意义。
Claims (2)
1.一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物,其特征是使用该方法所制备的除铬材料外观呈织物形状,由柠檬酸/乙二胺四乙酸改性的棉织物与铁离子之间的改性反应构成,在光辐射条件下处理水中铬离子。
2.一种权利要求1所述的一种用于水中铬离子去除的柠檬酸/乙二胺四乙酸铁改性棉织物的制备方法,其采用下述工艺:
步骤1:柠檬酸/乙二胺四乙酸改性溶液的制备:将柠檬酸与乙二胺四乙酸置于温度为40℃的水溶液中,然后加入纳米TiO2作为催化剂,其中柠檬酸/乙二胺四乙酸的总摩尔浓度为0.10摩尔/升至0.29摩尔/升,柠檬酸/乙二胺四乙酸的摩尔比为1:0-3,纳米TiO2的质量分数为1.0%至5%;
步骤2:柠檬酸/乙二胺四乙酸改性工艺:将棉织物材料放入装有柠檬酸/乙二胺四乙酸改性溶液的高温高压染色机中,使棉织物材料重量(克)和柠檬酸/乙二胺四乙酸二钠改性溶液体积(毫升)之比为1∶30-50,从室温开始以1.5℃/分钟的升温速率升至80℃,然后再以1℃/分钟的升温速率升至135℃,并保温30分钟至60分钟,最后得到柠檬酸/乙二胺四乙酸改性棉织物;
步骤3:柠檬酸/乙二胺四乙酸改性棉织物与铁离子的改性反应:将柠檬酸/乙二胺四乙酸改性棉织物浸入浓度为0.1摩尔/升的氯化铁水溶液中,使柠檬酸/乙二胺四乙酸改性棉织物材料重量(克)和氯化铁改性溶液体积(毫升)之比为1∶50,在50℃、pH值为1.0至3.0和搅拌条件下进行改性反应,反应进行1小时至3小时后得到柠檬酸/乙二胺四乙酸铁改性棉织物。
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