CN105417786B - 含2‑氯乙基丙基醚废水的处理方法 - Google Patents
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
本发明属于废水处理技术领域，具体涉及一种含2‑氯乙基丙基醚废水的处理方法。本发明主要针对氯化亚砜法制备2‑氯乙基丙基醚过程中水解产生的强酸性废水，结合零价铁法、Fenton试剂与UV/H2O2三种系统的优势，先加入铁粉反应至彻底溶解，调整pH值，在LED紫外灯作用下滴加H2O2溶液，经搅拌、中和、絮凝、沉淀、分离，最终达到降解水中有机物，去除废水异味和色度的目的。与现有工艺相比，本发明效率更高，处理效果显著，处理后的2‑氯乙基丙基醚废水CODCr去除率达99％以上，颜色由深黄色变为无色透明，无异味残留，完全达到排放标准，经济和社会效益显著。
Description
技术领域
本发明属于废水处理技术领域，具体涉及一种含2-氯乙基丙基醚废水的处理方法。
背景技术
2-氯乙基丙基醚(简称氯醚)是制备除草剂丙草胺的重要原料之一，该除草剂作为低毒、广谱、高效的专业选择性除草剂，在水稻种植领域应用广泛。工业上基本采用氯化亚砜法合成，此工艺在反应结束后，需加入水分解过量氯化亚砜，产生废水酸性强，需消耗大量液碱中和处理，经分液得到氯醚和废水，每吨产品废水产生量高达400～600kg。由于氯醚在水中有一定溶解度，且密度与水相近难以做到彻底分液，废水中含有大量氯醚、催化剂、无机盐等杂质，从而导致废水气味大、CODCr高(4～5×104mg/L)、颜色深，严重限制了其规模化生产和应用。另外，氯醚分子式为C5H11ClO，分子量122.59，分子中含有醚键和氯元素，决定了其挥发性强，气味大，毒性高，对环境污染大，且稳定性高，可生化性差，自然界降解缓慢，环境危害周期长。
零价铁法是利用金属电化学腐蚀原理，形成原电池对废水进行处理的良好工艺，又称为微电解法、内电解法、铁还原法等。零价铁粉对污染物具有吸附降解还原作用，可应用于吸附降解水体中的残留农药、催化分解卤代烃类有害物质、以及吸附还原水体中的微量重金属等领域。
芬顿试剂(Fenton试剂，简称FR)氧化催化法被认为是一种极具潜力的温和的脱氯降解方法，自20世纪60年代开始应用于废水处理。在传统FR的基础上，又开发出许多类FR，如光-FR、电-FR等，均属于高级氧化技术(AOPs)。其利用·OH的非选择性特性，可降解多种类有机物。FR氧化反应是利用Fe2+在酸性条件下催化H2O2分解产生的·OH来进攻有机物分子内键，羟基自由基·OH具有极高的反应活性和氧化能力，且无选择性，能与大多数有机物作用使其降解以至矿化。
UV/Fenton试剂法是经典Fenton试剂与UV/H2O2两种系统的复合，其基本原理类似于经典Fenton试剂，所不同的是反应体系在紫外光照射下三价铁与水中氢氧根离子的复合离子可以直接产生·OH并产生二价铁离子，二价铁离子可与H2O2进一步反应生成·OH，从而加快水中有机污染物降解速度；H2O2在紫外光照射作用下也可直接分解生成·OH；部分有机污染物在紫外光作用下也能够被直接降解。
目前，工业上对有机氯化物的处理主要有物理法、生物法、化学氧化法和化学还原法，存在成本高、实施困难、适应性小或降解率低等缺点。而且最重要的是降解时间长，难以用于庞大的工业、生活污水处理。因此，研究和开发高效、低廉、温和的脱氯降解方法是十分必要的。
发明内容
本发明的目的是提供一种条件温和、工艺简单、降解速率快、效果明显、成本低廉、适合工业化实施的含2-氯乙基丙基醚废水的处理方法。
本发明所述的含2-氯乙基丙基醚废水的处理方法，包括以下步骤：
(1)向含2-氯乙基丙基醚的废水中加入铁粉，搅拌反应至铁粉全部溶解；
氯化亚砜法合成2-氯乙基丙基醚中，反应结束后，需加入水分解过量氯化亚砜，产生氯化氢大部分都溶于水中，使废水呈强酸性，直接加入铁粉反应，可将废水中部分2-氯乙基丙基醚的氯离子置换出，形成易降解的乙基丙基醚，同时消耗其中一部分氢离子，减少后序工艺用碱量；
(2)调整废水pH值至3～4；
(3)向其中滴加H2O2，同时开启LED紫外灯照射，控制系统温度，滴加完毕后，在LED紫外灯照射下，继续搅拌2～6小时；根据废水CODCr的值确定H2O2的加入量和浓度即可，反应机理概括如下：
Fe0+2H+→Fe2++H2
H2+RClO→RHO+H++Cl-
Fe2++H2O2→Fe3++OH-+·OH
Fe2++·OH→Fe3++OH-
(4)将步骤(3)处理后的废水pH值调至8～9，形成红褐色沉淀；
(5)加入絮凝剂，经絮凝、沉淀、固液分离去除沉淀物。
其中，优选的技术方案如下：
步骤(1)所述铁粉的铁含量为70～90％，目数为30～200目。
步骤(1)所述铁粉的加入量为加入H2O2质量的10～20％。
步骤(3)所述H2O2的加入量为废水CODCr质量的1～3倍。
步骤(3)所述H2O2的浓度为10～30％。
步骤(3)中所述LED紫外灯的波长为380～450nm。
步骤(3)中所述控制系统温度为30～50℃。
步骤(5)中所述絮凝剂为阴离子型聚丙烯酰胺或聚合氯化铝。
步骤(5)中所述絮凝剂加入量为待处理废水质量的0.01～0.1‰。
调整pH值所用溶液为氢氧化钠溶液。
本发明的有益效果如下：
本发明主要针对氯化亚砜法制备2-氯乙基丙基醚过程中水解产生的强酸性废水，结合零价铁法、Fenton试剂与UV/H2O2三种系统的优势，先加入铁粉反应至彻底溶解，调整pH值，在LED紫外灯作用下滴加H2O2溶液，经搅拌、中和、絮凝、沉淀、分离，最终达到降解水中有机物，去除废水异味和色度的目的。与现有工艺相比，本发明效率更高，处理效果显著，处理后的2-氯乙基丙基醚废水CODCr去除率达99％以上，颜色由深黄色变为无色透明，无异味残留，完全达到排放标准。
具体实施方式
以下结合实施例对本发明做进一步描述。
实施例1
取强酸性氯醚废水，检测CODCr为4.6×104mg/L，取100ml(123.2g)该废水加入反应容器中，加入铁粉0.92g，搅拌反应至完全溶解，用氢氧化钠溶液将废水的pH值调至3～4，配制浓度为10％的双氧水溶液92g，缓慢滴加并剧烈搅拌，同时开启LED紫外灯，控制系统温度35±5℃，滴加完毕，继续搅拌2小时，反应结束，用氢氧化钠溶液调整pH值至8，称量废水质量为225.5g，加入阴离子型聚丙烯酰胺2.3mg，再经沉淀、固液分离去除沉淀物得无色透明清液，无异味，检测其CODCr为342mg/L，350nm吸光度为0.078(自来水的吸光度为0.013，空白样为去离子水)。
实施例2
取100ml(123.0g)实施例1用强酸性氯醚废水加入反应容器中，加入铁粉1.04g，搅拌反应至全部溶解，配制浓度为15％的双氧水溶液69g，缓慢滴加并剧烈搅拌，同时开启LED紫外灯，控制系统温度40±5℃，滴加完毕，继续搅拌3小时，反应结束，用氢氧化钠溶液调整pH值至9，称量废水质量为201.4g，加入阴离子型聚丙烯酰胺11.0mg，再经沉淀、固液分离去除沉淀物得无色透明清液，无异味，检测其CODCr为376mg/L，350nm吸光度为0.071(空白样为去离子水)。
实施例3
取100ml(123.1g)实施例1用强酸性氯醚废水加入反应容器中，加入铁粉1.38g，搅拌反应至全部溶解，配制浓度为12％的双氧水溶液76.7g，缓慢滴加并剧烈搅拌，同时开启LED紫外灯，控制系统温度45±5℃，滴加完毕，继续搅拌3小时，反应结束，用氢氧化钠溶液调整pH值至9，称量废水质量为228.3g，加入阴离子型聚丙烯酰胺13.7mg，再经沉淀、固液分离去除沉淀物得无色透明清液，无异味，检测其CODCr为328mg/L，350nm吸光度为0.082(空白样为去离子水)。
实施例4
取100ml(123.1g)实施例用强酸性氯醚废水加入反应容器中，加入铁粉2.73g，搅拌至全部溶解，用浓度为30％的双氧水溶液45.8g，缓慢滴加并剧烈搅拌，同时开启LED紫外灯，控制系统温度40±5℃，滴加完毕，继续搅拌6小时，反应结束，用氢氧化钠溶液调整pH值至9，称量废水质量为210.5g，加入阴离子型聚丙烯酰胺21mg，再经沉淀、固液分离去除沉淀物得无色透明清液，无异味，检测其CODCr为286mg/L，350nm吸光度为0.065(空白样为去离子水)。
Claims (6)
1.一种含2-氯乙基丙基醚废水的处理方法，其特征在于包括以下步骤：
（1）向含2-氯乙基丙基醚的废水中加入铁粉，搅拌反应至铁粉全部溶解；
（2）调整废水pH值至3～4；
（3）向其中滴加H2O2，同时开启LED紫外灯照射，控制系统温度，滴加完毕后，在LED紫外灯照射下，继续搅拌2～6小时；
（4）将步骤（3）处理后的废水pH值调至8～9，形成红褐色沉淀；
（5）加入絮凝剂，经絮凝、沉淀、固液分离去除沉淀物；
步骤（1）所述铁粉的铁含量为70～90％，目数为30～200目；所述铁粉的加入量为加入H2O2质量的10～20％；
步骤（3）所述H2O2的加入量为废水CODCr质量的1～3倍；
步骤（3）所述LED紫外灯的波长为380～450nm。
2.根据权利要求1所述的处理方法，其特征在于步骤（3）所述H2O2的浓度为10～30％。
3.根据权利要求1所述的处理方法，其特征在于步骤（3）所述控制系统温度为30～50℃。
4.根据权利要求1所述的处理方法，其特征在于步骤（5）所述絮凝剂为阴离子型聚丙烯酰胺或聚合氯化铝。
5.根据权利要求1所述的处理方法，其特征在于步骤（5）所述絮凝剂加入量为待处理废水质量的0.01～0.1‰。
6.根据权利要求1所述的处理方法，其特征在于调整pH值所用溶液为氢氧化钠溶液。
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