CN108395027A - 1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水处理工艺 - Google Patents
1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水处理工艺 Download PDFInfo
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Abstract
本发明涉及化工生产废水处理工艺，具体涉及1‑萘酚‑5‑磺酸合成2‑亚硝基‑1‑萘酚‑5‑磺酸中间体的生产废水处理工艺。本发明首先向1‑萘酚‑5‑磺酸合成2‑亚硝基‑1‑萘酚‑5‑磺酸中间体的生产废水中加入芬顿试剂氧化反应，然后加入Ca(OH)2分层过滤分离上层液体后得滤液，向该滤液中加入次氯酸钠，处理完成。由于本发明每个处理工艺单元之间有效地衔接和协同作用，使废水CODCr的去除效率高达96％，处理水的CODCr值<800mg/L。同时本发明处理工艺中所涉及化学试剂均为常见化工产品，易购买，价格便宜。
Description
技术领域
本发明涉及化工生产废水处理工艺，具体涉及1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水处理工艺。
背景技术
由1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水，具有pH低、高浓度、高色度、难降解、高毒性、可生化性能差等缺点。目前国内还未有针对2-亚硝基-1-萘酚-5-磺酸中间体生产废水处理工艺的相关报道。马冬梅等报道了Fe2+催化双氧水氧化处理H酸(1-氨基-8-萘酚-3,6-二磺酸)结晶废母液萃取余液的效能。在H2O2投加量为140mmoL/Ln(H2O2):n(Fe2+)为15:1，初始pH值为2.0时，CODCr降低率可达79％，TOC降低率可达50％。由于原水为结晶废母液的萃取余液，CODCr平均值为仅为1620mg/L，通过芬顿试剂氧化处理后，出水的CODCr值较低。但是此类废水在萃取处理前含有大量流失的染料分子以及生产中间体，CODCr值通常为几万到几十万毫克每升之间，仅通过芬顿试剂一种方法的处理效率很有限。萃取是处理高浓度、难降解有机物的一种有效的方法，但是该处理方法中萃取剂需要再生处理，增加处理成本。综上，本领域亟需一种高效、成本低的2-亚硝基-1-萘酚-5-磺酸中间体的生产废水处理工艺。
发明内容
为弥补现有技术的空白，本发明提供一种1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水处理工艺。该工艺CODCr去除率高，处理方法简单、成本低。
为实现上述目的，本发明采用如下技术方案：
(1)芬顿试剂氧化：向1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水加入5g/L的FeSO4·7H2O和0.5L/L的H2O2、反应时间1.5hr；
(2)中和-混凝处理：向芬顿试剂氧化后废水中，缓慢加入Ca(OH)2石灰乳，搅拌，将废水的pH值调至7-8，然后静置2hr，分层，上层为淡黄色浑浊液体，下层为黄灰色沉淀，过滤分离上层淡黄色浑浊液体，得滤液；
(3)次氯酸钠氧化：向60mL/L滤液中添加浓度10％的次氯酸钠，反应时间2hr，废水处理完成。
本发明构思巧妙，处理工艺简单易操作，先在2-亚硝基-1-萘酚-5-磺酸中间体的生产废水中加入芬顿试剂，芬顿试剂在一定的pH条件下(pH＝2-5)，通过Fe2+催化分解H2O2产生·OH，使芬顿试剂表现出极强的氧化性，利用芬顿试剂的强氧化性，降解生产废水中的残留的1-萘酚-5-磺酸、2-亚硝基-1-萘酚-5-磺酸等有机物质。由于芬顿氧化工艺的pH通常为2-5，而1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水pH为1-2，满足芬顿氧化工艺的要求，因此，本发明废水处理工艺中在芬顿氧化处理过程不需要调节pH值，极大地节约了药剂费用。由芬顿氧化处理后废水pH为3左右，发明人采用石灰乳中和芬顿氧化处理后废水pH的同时利用石灰乳的混凝沉淀作用，进一步处理废水中的有机污染物降低CODCr值，并为后续的次氯酸钠氧化工艺提供必要的pH值，在此基础上，加入次氯酸钠氧化进一步降低CODCr值。
由于本发明每个处理工艺单元之间有效地衔接和协同作用，使废水CODCr的去除效率高达96％，处理水的CODCr值<800mg/L。在与其他废水混合进行后续处理时，大大降低了后续处理的有机负荷率。同时本发明处理工艺中所涉及化学试剂均为常见化工产品，易购买，价格便宜。
具体实施方式
下面通过具体实施例详述本发明，但不限制本发明的保护范围。如无特殊说明，本发明所采用的实验方法均为常规方法，所用实验器材、材料、试剂等均可从化学公司购买。
实施例1
(1)芬顿试剂氧化
1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水的pH为1-2，在此pH值下，添加5g/L FeSO4·7H2O于废水中、搅拌溶解，滴加H2O2，H2O2的添加量为0.5L/L，反应时间90min。CODCr的去除效率为84％，废水颜色由深褐色变为棕黄色。
(2)中和-混凝处理
向芬顿试剂氧化后废水中，缓慢加入Ca(OH)2石灰乳，搅拌，将废水的pH值调至7-8。静置2hr，分层。上层为淡黄色浑浊液体，下层为黄灰色沉淀，过滤分离上层淡黄色浑浊液体，得滤液。CODCr的去除效率为30％。芬顿试剂氧化-中和混凝处理的CODCr总去除率为88％。
(3)次氯酸钠氧化
不调节滤液pH值，直接向滤液中添加10％的次氯酸钠，添加量为60mL/L，反应时间2hr。CODCr的去除率为68％，废水的颜色变为浅黄色。
经过上述处理工艺处理后，原水的CODCr由16800mg/L降解为600mg/L，CODCr去除率为96％。
对比例
向1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水中添加量芬顿试剂，反应时间90min，芬顿试剂组成为：每投加140mmoL/L H2O2，n(H2O2):n(Fe2+)为15:1。CODCr的去除效率＜80％。
以上所述，仅为本发明创造较佳的具体实施方式，但本发明创造的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明创造披露的技术范围内，根据本发明创造的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明创造的保护范围之内。
Claims (2)
1.一种1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水处理工艺，其特征在于，向1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水中先加入芬顿试剂氧化反应，然后加入Ca(OH)2分层过滤分离上层液体后，得滤液，向该滤液中加入次氯酸钠，处理完成。
2.根据权利要求1所述1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水处理工艺，其特征在于，具体包括以下步骤：
(1)芬顿试剂氧化：向1-萘酚-5-磺酸合成2-亚硝基-1-萘酚-5-磺酸中间体的生产废水加入5g/L的FeSO4·7H2O和0.5L/L的H2O2、反应时间1.5hr；
(2)中和-混凝处理：向芬顿试剂氧化后废水中，缓慢加入Ca(OH)2，搅拌，将废水的pH值调至7-8，然后静置2hr，分层，上层为淡黄色浑浊液体，下层为黄灰色沉淀，过滤分离上层淡黄色浑浊液体，得滤液；
(3)次氯酸钠氧化：向60mL/L滤液中添加浓度10％的次氯酸钠，反应时间2hr，废水处理完成。
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| CN112093882A (zh) * | 2020-08-25 | 2020-12-18 | 中钢集团鞍山热能研究院有限公司 | 一种联萘酚生产废水预处理方法 |
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| CN112093882A (zh) * | 2020-08-25 | 2020-12-18 | 中钢集团鞍山热能研究院有限公司 | 一种联萘酚生产废水预处理方法 |
| CN112093882B (zh) * | 2020-08-25 | 2022-07-01 | 中钢集团鞍山热能研究院有限公司 | 一种联萘酚生产废水预处理方法 |
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