CN113718263A - 一种焦化废水深度处理用药剂的制备方法 - Google Patents
一种焦化废水深度处理用药剂的制备方法 Download PDFInfo
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Abstract
本发明涉及工业废水处理技术领域,尤其涉及一种焦化废水深度处理用药剂的制备方法。具体包括如下步骤:1、用去离子水将马来酸酐溶解生成马来酸;2、加氢氧化钠溶液调节pH值为7~8;3、水浴加热控制反应温度为50℃~60℃,加入钒催化剂5mg/L~10mg/L,搅拌,再分3‑5次加入过氧化氢,间隔为15min~30min,1h~2h后,加入六偏磷酸钠,升高反应温度为90~100℃,反应0.5h~1h,生成环氧琥珀酸盐复配物;4、将生成物溶于丙酮溶液中,沉淀干燥1h~2h,配成30%~40%的溶液,加氢氧化钙,在70℃~80℃反应0.5h~1h后得到聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂。本发明更高效的去除水中污染物质,提高使用效率,减少药剂投加量,避免多余药剂对水系统二次污染且能起到阻垢作用。
Description
技术领域
本发明涉及工业废水处理技术领域,尤其涉及一种焦化废水深度处理用药剂的制备方法。
背景技术
焦化废水是有毒有害、难降解的高浓度有机废水,其中有机物以苯酚类化合物居多,约占总有机物的一半,有机物中还包括多环芳香族化合物和含氮、氧、碳的杂环化合物等,无机污染物主要以氨氮、氰化物、硫化物、硫氰化物为主。
目前,国内大多数焦化厂废水处理系统采用一级处理和二级处理工艺,但近几年来也开始采用三级处理工艺。一级处理指高浓度废水中污染物的回收利用,包括氨水脱酚、氨水蒸馏、终冷水脱氰等;二级处理主要指酚氰废水无害化处理,以活性污泥法为主,还包括生物强化技术,如生物铁法、投加生长素法、强化曝气法等;三级深度处理是指在生化处理后的排水仍不能达到排放标准时所采用的再次深度净化,其主要工艺有活性炭吸附法、炭—生物膜法、混凝沉淀法和氧化塘法。而国外在二级生化处理之前采取了更为复杂的预处理和其他方法控制进入生化系统的水质,防止有毒污染物浓度过高,并在生化处理流程之后采取三级净化系统。
在废水处理过程中,需要向水中添加大量化学药剂对其进行沉降、过滤、混凝、絮凝、缓蚀、阻垢等水质调理,这些处理剂包括,改善固液分离的化学制品、pH调节剂、表面活性剂、延缓或防止换热设备结垢的阻垢剂、金属或其他材料的缓蚀剂、延缓膜污染的稳定剂、生物分散剂杀菌剂、化学清洁清洗剂、污水生化处理中的添加剂、氧化还原剂等等,化学药剂的选择决定了废水处理的效果。针对不同工况、不同水质、不同水处理目的,选择合适的化学药剂是水处理加药过程中面临的最重要的问题。因此,化学药剂的使用是当前研究的重点。
发明内容
为了克服现有技术的不足,本发明提供一种焦化废水深度处理用药剂的制备方法。能够减小药剂投加量,药剂作用充分发挥,使用效率高,且运行稳定,提高了处理效果,避免无效投加和药剂污染,出水水质稳定。
为了达到上述目的,本发明采用以下技术方案实现:
一种焦化废水深度处理药剂的制备方法,水处理药剂为聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂,具体包括如下步骤:
1、以马来酸酐10g/L~20g/L为原料,用去离子水将其溶解生成马来酸。马来酸酐质量浓度为10g/L~20g/L。
2、加入碱液调节pH,在搅拌条件下缓慢加入质量浓度为30%~40%的氢氧化钠溶液,调节反应pH值至7~8。
3、水浴加热,控制反应温度为50℃~60℃,向反应液中加入钒催化剂5mg/L~10mg/L,钒催化剂主要成分为五氧化二钒,以硅藻土为载体。
搅拌均匀,再分3-5次加入质量百分比浓度30%-50%的过氧化氢催化剂,过氧化氢催化剂与马来酸酐的质量比为1:3~1:4,边搅拌边缓缓加入,时间间隔为15min~30min,使环氧化反应充分完全。
反应1h~2h后,加入六偏磷酸钠,六偏磷酸钠与马来酸酐的质量比为1:2~1:3,升高反应温度为90~100℃,继续反应0.5h~1h,生成环氧琥珀酸盐复配物。
4、将合成的环氧琥珀酸盐复配物溶于质量百分比浓度为10%~20%的丙酮溶液中,沉淀干燥1h~2h,配成质量百分比浓度为30%~40%的溶液,加入氢氧化钙10mg/L~20mg/L引发聚合反应,在温度70℃~80℃条件下反应0.5h~1h后得到聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂。
与现有方法相比,本发明的有益效果是:
本发明聚环氧琥珀酸兼具阻垢缓蚀双重功效,生物降解性能好并适用于高碱、高金属含量水系,与六偏磷酸钠协同使用,缓蚀效果明显增强,能够更高效的去除水中的污染物质,提高使用效率,减少药剂投加量,避免多余药剂对水系统的二次污染且能起到阻垢的作用。经上述药剂深度处理后的焦化废水,阻垢率大于75%,腐蚀率小于0.1,COD去除率大于90%,SS去除率大于85%,氨氮去除率大于90%,电导率低于500,药剂作用充分发挥,极大的改善了处理效果,避免无效投加和药剂污染,出水水质稳定。
具体实施方式
本发明公开了一种焦化废水深度处理用药剂的制备方法。本领域技术人员可以借鉴本文内容,适当改进工艺参数实现。特别需要指出的是,所有类似的替换和改动对本领域技术人员来说是显而易见的,它们都被视为包括在本发明。本发明的方法及应用已经通过较佳实施例进行了描述,相关人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和应用进行改动或适当变更与组合,来实现和应用本发明技术。
以下介绍本发明的最佳实施方式:
实施例1:
一种焦化废水深度处理用药剂的制备方法如下:
1、用去离子水将10g/L马来酸酐溶解,生成马来酸;
2、在搅拌条件下缓慢加入质量浓度为30%的氢氧化钠溶液,调节反应pH为7;
3、反应温度为50℃,向反应液中加入钒催化剂5mg/L,搅拌均匀,再分3次加入质量百分比浓度30%过氧化氢催化剂,过氧化氢催化剂与马来酸酐的质量比为1:3,边搅拌边缓缓加入,每次加入时间间隔为15min,使环氧化反应充分完全,反应1h后加入六偏磷酸钠,六偏磷酸钠与马来酸酐的质量比为1:2,升高反应温度为90℃,继续反应0.5h,生成环氧琥珀酸盐复配物;
4、将合成的环氧琥珀酸盐复配物溶于质量百分比浓度10%的丙酮溶液中,沉淀干燥1.0h,配成质量百分比浓度为30%的溶液,加入氢氧化钙10mg/L引发聚合反应,在温度70℃条件下反应0.5h后得到聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂。
实施例2:
一种焦化废水深度处理用药剂的制备方法如下:
1、用去离子水将15g/L马来酸酐溶解,生成马来酸;
2、在搅拌条件下缓慢加入质量浓度为35%的氢氧化钠溶液,调节反应pH为7;
3、反应温度为55℃,向反应液中加入钒催化剂7mg/L,搅拌均匀,再分4次加入质量百分比浓度40%过氧化氢催化剂,过氧化氢催化剂与马来酸酐的质量比为1:3,边搅拌边缓缓加入,每次加入时间间隔为20min,使环氧化反应充分完全,反应1.5h后加入六偏磷酸钠,六偏磷酸钠与马来酸酐的质量比为1:2,升高反应温度为95℃,继续反应0.8h,生成环氧琥珀酸盐复配物;
4、将合成的环氧琥珀酸盐复配物溶于质量百分比浓度10%的丙酮溶液中,沉淀干燥1.5h,配成质量百分比浓度为35%的溶液,加入氢氧化钙15mg/L引发聚合反应,在温度75℃条件下反应0.7h后得到聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂。
实施例3:
一种焦化废水深度处理用药剂的制备方法如下:
1、用去离子水将20g/L马来酸酐溶解,生成马来酸;
2、在搅拌条件下缓慢加入质量浓度为40%的氢氧化钠溶液,调节反应pH为8;
3、反应温度为60℃,向反应液中加入钒催化剂10mg/L,搅拌均匀,再分5次加入质量百分比浓度50%过氧化氢催化剂,过氧化氢催化剂与马来酸酐的质量比为1:4,边搅拌边缓缓加入,每次加入时间间隔为30min,使环氧化反应充分完全,反应2h后加入六偏磷酸钠,六偏磷酸钠与马来酸酐的质量比为1:3,升高反应温度为100℃,继续反应1.0h,生成环氧琥珀酸盐复配物;
4、将合成的环氧琥珀酸盐复配物溶于质量百分比浓度20%的丙酮溶液中,沉淀干燥2h,配成质量百分比浓度为40%的溶液,加入氢氧化钙20mg/L引发聚合反应,在温度80℃条件下反应1.0h后得到聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂。
按照以上各实施例的技术要求,焦化废水经上述药剂处理后,各实施例对污染物的去除效果如表1所示。
表1 各实施例对污染物的去除效果
由表1中结果可知,经上述药剂深度处理后的焦化废水,阻垢率大于75%,腐蚀率小于0.1,COD去除率大于90%,SS去除率大于85%,氨氮去除率大于90%,电导率低于500,药剂作用充分发挥,极大的改善了处理效果,避免无效投加和药剂污染,出水水质稳定。
以上所述,仅为本发明较佳的具体实施方式,但本发明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揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (5)
1.一种焦化废水深度处理药剂的制备方法,其特征在于,所述处理药剂为聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂,具体包括如下步骤:
1)以马来酸酐为原料,用去离子水将其溶解生成马来酸;
2)加入碱液调节pH,在搅拌条件下加入质量浓度为30%~40%的氢氧化钠溶液,调节反应pH值至7~8;
3)水浴加热,控制反应温度为50℃~60℃,向反应液中加入钒催化剂5mg/L~10mg/L,搅拌均匀,再分3~5次加入质量百分比浓度30%-50%的过氧化氢催化剂,边搅拌边缓缓加入,时间间隔为15min~30min,反应1h~2h后,加入六偏磷酸钠,升高反应温度至90~100℃,继续反应0.5h~1h,生成环氧琥珀酸盐复配物;
4)将合成的环氧琥珀酸盐复配物溶于质量百分比浓度为10%~20%的丙酮溶液中,沉淀干燥1h~2h,配成质量百分比浓度为30%~40%的溶液;加入氢氧化钙10mg/L~20mg/L,在温度70℃~80℃条件下反应0.5h~1h后得到聚环氧琥珀酸/六偏磷酸钠复配缓蚀剂。
2.根据权利要求1所述的一种焦化废水深度处理药剂的制备方法,其特征在于,所述步骤1)马来酸酐质量浓度为10g/L~20g/L。
3.根据权利要求1所述的一种焦化废水深度处理药剂的制备方法,其特征在于,所述步骤3)钒催化剂主要成分为五氧化二钒,以硅藻土为载体。
4.根据权利要求1所述的一种焦化废水深度处理药剂的制备方法,其特征在于,所述步骤3)过氧化氢催化剂与马来酸酐的质量比为1:3~1:4。
5.根据权利要求1所述的一种焦化废水深度处理药剂的制备方法,其特征在于,所述步骤3)六偏磷酸钠与马来酸酐的质量比为1:2~1:3。
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