CN107952414A - 一种含油废水吸附剂及其制备方法 - Google Patents

一种含油废水吸附剂及其制备方法 Download PDF

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CN107952414A
CN107952414A CN201711033152.1A CN201711033152A CN107952414A CN 107952414 A CN107952414 A CN 107952414A CN 201711033152 A CN201711033152 A CN 201711033152A CN 107952414 A CN107952414 A CN 107952414A
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杨华亮
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Abstract

本发明公开了一种含油废水吸附剂及其制备方法,由粉煤灰、油菜秸秆、氢氧化钙、镁砂、正硅酸乙酯、四氧化三铁粉末等原料制成,本发明通过秸秆与粉煤灰的混合,利用其疏松多孔的优秀载体性能结合改性镁砂制成颗粒,令成品吸附剂颗粒具有质轻、化学稳定性高等特点,同时不会对环境造成污染,操作简单,成本低,可以循环利用,对含油废水吸附处理后废水中剩余COD等浓度满足国家排放要求,适合规模化含油废水的处理。

Description

一种含油废水吸附剂及其制备方法
技术领域
本发明涉及水体治理技术领域,尤其涉及一种含油废水吸附剂及其制备方法。
背景技术
含油废水是一种常见的工业废水。石油开采、炼制、石油化工、机械加工等行业每年均产生大量的含油废水,具有污染物种类多、浓度高、难生物降解和高残留性,对环境的危害大等特点,特别是产生的恶臭严重污染环境并危害人类健康。目前,由于原油业产生的废水量大、成分复杂、特别是其含高浓度的酚、硫化物、硫醇、环烷酸等物质,恶臭、污染极其严重,使用常规的水处理技术处理后的含油废水会残余更难降解的物质,这类物质对人类的危害最大。
目前,常用的含油废水处理方法有电化学法、膜分离法、气浮法、化学凝聚法等,但其在能耗、药剂添加、运行费用、污泥脱水等方面均存在其各自缺陷。吸附法处理含油废水是利用吸附剂的多孔性和高比表面积,对废水中的油及有机物进行吸附,从而达到油水分离的目的。吸附法在含油废水处理领域得到了越来越广泛的研究。但常用的活性炭吸附法存在药剂费用高、再生困难等不足,因此,国内外对性能良好的廉价吸附材料的使用日益重视。通常,这类吸附材料需要不仅具备廉价易得、具有优良的处理效能,而且操作简单,运行费用低。
我国镁矿资源丰富,菱镁矿总储量约3.1×106亿吨,其中约85%集中在辽宁东南部地区。镁砂是由菱镁石矿、水镁石矿或海水中提取的氢氧化镁经高温煅烧、烧结的产物的统称,其主要成分为MgO。研究表明,镁砂是非等轴晶系方镁石,其晶格存在点状缺陷和位错,具有较高的表面能,易于进行物理化学反应,活性良好。MgO在印染废水脱色处理、酸性废水处理、有机物脱除、废水脱磷、脱氨和烟气脱硫等领域得到了广泛的研究和应用。
尽管镁砂材料廉价易得,但使用其直接作为吸附材料使用则有着吸附位点有限,且吸附后随着时间的延长易发生解吸从而影响使用效果。二氧化锰易与烃基等含氧官能团相结合,吸附位点多,对水中的有机物、重金属阳离子等具有较强的离子交换作用和络合吸附作用。然而二氧化锰颗粒细小,难以从水中分离,限制了其使用范围。因此将镁砂与二氧化锰进行混合负载并通过改性工艺,从而获得复合材料以大幅提高使用性能,成为一种可行的工艺选择。
发明内容
本发明目的就是为了弥补已有技术的缺陷,提供一种含油废水吸附剂及其制备方法。
本发明是通过以下技术方案实现的:
一种含油废水吸附剂,通过以下方法制备:
(1)将油菜秸秆洗净后烘干,送入粉碎机中粉碎并过120-150目筛,得到秸秆粉末备用;
(2)将粉煤灰、氢氧化钙以及秸秆粉末按质量比(4-6):(1-1.5):(13-15)混合后浸没于无水乙醇中,再用球磨机球磨混料90-120分钟,完成后过滤取出送入烘干机中干燥,将干燥物料置于高温炉中烧结,冷却后取出粉碎过150-180目筛备用;
(3)将镁砂送入高温炉中,在500-550℃下焙烧60-90分钟,冷却后取出,粉碎过30-40目筛,再放入清水中煮沸30-40分钟,冷却至室温后过滤去除水中上浮灰分及杂质,再置于干燥箱中干燥10-12小时,将干燥后的粉末按固液比1:25-30g/mL加入到质量分数为2.7-3.0%的高锰酸钾溶液中,浸渍7-8小时后过滤取出并送入高温炉中,升温至450-480℃,焙烧2-3小时,得到预改性镁砂粉末备用;
(4)将预改性镁砂粉末与正硅酸乙酯按固液比1:2-3混合后搅拌5-6小时,再用超声分散后加入混合体系总质量3-3.5%的γ-氯丙基三乙氧基硅烷,继续搅拌5-6小时后用清水洗涤干净,冷冻干燥,将所得粉末与四氧化三铁粉末按质量比4-5:1混合后再按1-1.5g/L加入到20%氯化铁溶液中,超声分散后在150-180转/分下震荡20-40分钟,过滤后清水冲洗干净,冷冻干燥得改性镁砂粉末备用;
(5)将步骤2所得物料与步骤4所得改性镁砂粉末按质量比4-6:1混合送入造粒机中造粒,即得本发明含油废水吸附剂。
所述步骤2中高温炉烧结条件为先升温至230-250℃,烧结25-30分钟,再升温至380-400℃,烧结10-15分钟。
所述步骤3中用高锰酸钾溶液浸渍后用清水冲洗至冲洗水不再浑浊且与超纯水pH值相同后,置于60-65℃干燥箱中干燥8-12小时,再送入高温炉中进行焙烧处理。
所述步骤4中两次超声分散的条件依次为25-28kHz下超声100-120分钟以及35-36kHz下超声40-60分钟。
本发明的优点是:
本发明通过秸秆与粉煤灰的混合,利用其疏松多孔的优秀载体性能结合改性镁砂制成颗粒,令成品吸附剂颗粒具有质轻、化学稳定性高等特点,同时不会对环境造成污染,其中镁砂经焙烧处理脱除了大量的吸附水和结构水,增加有效比表面积,同时通过高锰酸钾的浸渍负载二氧化锰,结合二者优势,提升复合材料的吸附种类和吸附强度,在此条件下为强化对污染物的吸附效果和絮凝沉淀作用,又向复合材料中加入四氧化三铁磁粉,并通过二氧化硅的包覆使材料整体稳固结合,不仅可以增大材料颗粒碰撞效率与频率,强化对颗粒物、有机物的去除,同时利用外加磁场即可进行材料使用后的回收,在使用上便捷高效,本发明操作简单,成本低,可以循环利用,对含油废水吸附处理后废水中剩余COD等浓度满足GB8978-1996《污水综合排放标准》一级标准,适合规模化含油废水处理。
具体实施方式
一种含油废水吸附剂,通过以下方法制备:
(1)将油菜秸秆洗净后烘干,送入粉碎机中粉碎并过120目筛,得到秸秆粉末备用;
(2)将粉煤灰、氢氧化钙以及秸秆粉末按质量比5:1:14混合后浸没于无水乙醇中,再用球磨机球磨混料90分钟,完成后过滤取出送入烘干机中干燥,将干燥物料置于高温炉中先升温至230℃,烧结25分钟,再升温至380℃,烧结10分钟,冷却后取出粉碎过150目筛备用;
(3)将镁砂送入高温炉中,在500℃下焙烧60分钟,冷却后取出,粉碎过30目筛,再放入清水中煮沸30分钟,冷却至室温后过滤去除水中上浮灰分及杂质,再置于干燥箱中干燥10小时,将干燥后的粉末按固液比1:25g/mL加入到质量分数为2.7%的高锰酸钾溶液中,浸渍7小时后过滤取出用清水冲洗至冲洗水不再浑浊且与超纯水pH值相同后,置于60℃干燥箱中干燥8小时并送入高温炉中,升温至450℃,焙烧2小时,得到预改性镁砂粉末备用;
(4)将预改性镁砂粉末与正硅酸乙酯按固液比1:2混合后搅拌5小时,再在28kHz下超声分散115分钟后加入混合体系总质量3%的γ-氯丙基三乙氧基硅烷,继续搅拌5小时后用清水洗涤干净,冷冻干燥,将所得粉末与四氧化三铁粉末按质量比4:1混合后再按1g/L加入到20%氯化铁溶液中,在36kHz下超声分散55分钟后在150转/分下震荡20分钟,过滤后清水冲洗干净,冷冻干燥得改性镁砂粉末备用;
(5)将步骤2所得物料与步骤4所得改性镁砂粉末按质量比4:1混合送入造粒机中造粒,即得本发明含油废水吸附剂。

Claims (5)

1.一种含油废水吸附剂,其特征在于通过以下方法制备:
(1)将油菜秸秆洗净后烘干,送入粉碎机中粉碎并过120-150目筛,得到秸秆粉末备用;
(2)将粉煤灰、氢氧化钙以及秸秆粉末按质量比(4-6):(1-1.5):(13-15)混合后浸没于无水乙醇中,再用球磨机球磨混料90-120分钟,完成后过滤取出送入烘干机中干燥,将干燥物料置于高温炉中烧结,冷却后取出粉碎过150-180目筛备用;
(3)将镁砂送入高温炉中,在500-550℃下焙烧60-90分钟,冷却后取出,粉碎过30-40目筛,再放入清水中煮沸30-40分钟,冷却至室温后过滤去除水中上浮灰分及杂质,再置于干燥箱中干燥10-12小时,将干燥后的粉末按固液比1:25-30g/mL加入到质量分数为2.7-3.0%的高锰酸钾溶液中,浸渍7-8小时后过滤取出并送入高温炉中,升温至450-480℃,焙烧2-3小时,得到预改性镁砂粉末备用;
(4)将预改性镁砂粉末与正硅酸乙酯按固液比1:2-3混合后搅拌5-6小时,再用超声分散后加入混合体系总质量3-3.5%的γ-氯丙基三乙氧基硅烷,继续搅拌5-6小时后用清水洗涤干净,冷冻干燥,将所得粉末与四氧化三铁粉末按质量比4-5:1混合后再按1-1.5g/L加入到20%氯化铁溶液中,超声分散后在150-180转/分下震荡20-40分钟,过滤后清水冲洗干净,冷冻干燥得改性镁砂粉末备用;
(5)将步骤2所得物料与步骤4所得改性镁砂粉末按质量比4-6:1混合送入造粒机中造粒,即得本发明含油废水吸附剂。
2.根据权利要求1所述的含油废水吸附剂的制备方法,其特征在于,所述步骤2中高温炉烧结条件为先升温至230-250℃,烧结25-30分钟,再升温至380-400℃,烧结10-15分钟。
3.根据权利要求1所述的含油废水吸附剂的制备方法,其特征在于,所述步骤3中用高锰酸钾溶液浸渍后用清水冲洗至冲洗水不再浑浊且与超纯水pH值相同后,置于60-65℃干燥箱中干燥8-12小时,再送入高温炉中进行焙烧处理。
4.根据权利要求1所述的含油废水吸附剂的制备方法,其特征在于,所述步骤4中两次超声分散的条件依次为25-28kHz下超声100-120分钟以及35-36kHz下超声40-60分钟。
5.权利要求1-4任一项所述的含油废水吸附剂的使用方法,其特征在于,将吸附剂颗粒按15-25g/L的量均匀投入待处理含油废水中,3-4小时后通过过滤及外加磁场回收吸附剂即可。
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