CN107792912B - 一种含油废水吸附材料的制备方法 - Google Patents
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Abstract
本发明公开了一种含油废水吸附材料的制备方法,由聚邻苯二甲酸丙二醇酯、双酚A环氧树脂、乙烯基苄基三甲基氯化铵、椰壳、苯酚、聚乙烯醇等原料制成,本发明以椰壳制备多孔碳纤维,经多次改性工艺处理,得到高机械强度、高吸附性的多孔碳纤维,再与油脂具有优良亲和性的乙烯基苄基三甲基氯化铵结合,得到具有良好的物理化学稳定性和优异的机械强度的油脂吸附洗脱材料,由于稳定性强适合于多种复杂环境条件下应用,具有很好的环境、经济效益,且易于规模化生产。
Description
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材料的制备方法。
背景技术
含油废水是一种常见的工业废水主要来源于石油工业的采油、炼油、贮油、运输以及石油化工生产等过程,具有污染物种类多、浓度高、难生物降解和高残留性,油品进入水体后,会在表层形成水膜,阻止氧气溶入水体,从而导致水体缺氧、生物死亡、造成严重的环境污染,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。所以,含油废水的处理成为当下石油化工产业和环境保护等多个领域亟待解决的问题。
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,这类吸附材料不仅需要具备廉价易得、具有优良的处理效能,而且操作简单,运行费用低。
多孔碳纤维是一种新型的多孔纤维状吸附材料,因其独特的孔隙结构和形态而具有较一般多孔炭更大的比表面积、更高的孔容、更快的吸附速率和更强的再生能力。自从上世纪七十年代问世以来,就被广泛应用于空气净化、废气废水处理、军事防护、金属回收、电子器材等方面,其在含油吸附方面,也表现出了优异的性能。目前,市场上的多孔碳纤维主要有聚丙烯腈基多孔碳纤维、沥青基多孔碳纤维、粘胶基多孔碳纤维和酚醛基多孔碳纤维等,不同碳纤维在碳化速度、产碳率、孔隙率以及碳化后的韧性均不一样。因此,需要结合传统碳纤维制备方法,通过优化改进工艺,提供孔径小、孔隙率高、纤维均一性好以及结合力强的多孔碳纤维。
与此同时,由于碳纤维的制备工艺包括碳化或石墨化,使得碳纤维表面的碳原子堆叠取向更一致,原子层间距更小,所以纤维表面表现为非极性和化学惰性,另外碳纤维表面有疏水、光滑、吸附性能低等缺点,导致碳纤维与其复合的材料间界面粘结性差。因此,需要对碳纤维表面进行改性,提高其与复合材料的界面粘结强度。
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材料的制备方法。
本发明是通过以下技术方案实现的:
一种含油废水吸附材料的制备方法,包括以下步骤:
(1)将聚邻苯二甲酸丙二醇酯、双酚A环氧树脂按质量比1:(3-4)混合后加热至110-130℃,搅拌至分散完全,降温至70-80℃后再向其中加入对枯基聚醚基磺酸盐,搅拌40-50分钟,得预混液备用;
(2)将纺丝液置于静电纺丝仪中,使用铝箔纸包裹接收器,使初纺纤维收集在铝箔纸上,纺丝过程工艺参数为正压15-16kV,负压1.5-2kV,推进速率0.04-0.05mm/min,接收速率30-32r/min,针头与接收器之间距离为15-18cm,环境温度30-40℃,纺丝完成后在室温下静置一天,得到初纺纤维,再将其置于烘箱中,升温至160-170℃固化60-70分钟,取出后再送入管式炉中,在氮气气氛下以5-10℃/min的升温速率从室温升至750-850℃,保温1-2小时,自然冷却后得到碳纤维备用;
(3)以步骤2所得碳纤维作为阳极,石墨为阴极,在质量分数为8-10%的磷酸铵电解质中,控制电流密度为0.3-0.35A/m2,阳极氧化处理1.5-2分钟,收集碳纤维用清水冲洗净,得到改性碳纤维备用;
(4)将步骤1所得预混液用水稀释1.5-2倍后将步骤3所得改性碳纤维浸渍于其中,2-4分钟后取出并干燥备用;
(5)将步骤4所得干燥产物与乙烯基苄基三甲基氯化铵、高锰酸钾以及水按质量比(8-10):(10-12):(0.5-1):(25-28)混合后加热至70-80℃,反应4-5小时后冷却至室温,用水洗至滤液为中性,经固液分离后在60-80℃下干燥,即得本发明吸附材料。
所述步骤1中对枯基聚醚基磺酸盐加入量为混合液体系质量的3-6%。
所述步骤2中纺丝液的制备方法为将椰壳粉碎过100-120目筛,烘干后与苯酚、浓硫酸按质量比(5-7):(20-25):(0.6-0.9)混合并搅拌均匀,置于140-160℃油浴锅中反应100-120分钟,之后降至室温,加入氢氧化钠中和pH至中性,将产物与80%二恶烷水溶液按体积比1:(9-11)混合搅拌60-80分钟,离心并过滤,除去残渣后将滤液经旋转蒸发仪在60-70℃下浓缩,除去二恶烷,得纯液化物,再与聚乙烯醇按质量比(45-46):(4-5)混合后用氢氧化钠调节pH至10-11,之后加入甲醛溶液,升温至80-85℃,反应2-3小时后冷却至室温,得到纺丝液。
所述步骤4中干燥过程使用热风在130-150℃下吹2-5分钟。
所述步骤5中干燥产物、乙烯基苄基三甲基氯化铵、高锰酸钾、水的质量比为9:11:0.8:26。
所述的纺丝液的制备方法,加入的甲醛和苯酚物质的量之比为n(甲醛):n(苯酚)=(1.4-1.5):1。
本发明的优点是:
本发明采用苯酚液化的方法,将椰壳液化为多活性小分子,避免传统木质素因结构复杂且含大量杂质,直接用于纺丝效果不理想的缺陷,再以酚醛为单元连接为高聚物,具有更快的碳化速度、更高的产碳率和孔隙率,并且酚醛树脂由于形成交联结构,所以碳化后仍可保持一定韧性,再结合静电纺丝优化的工艺参数处理,较传统的熔融纺丝,使纤维直径更细,达到纳米级,从而具有更大的比表面积,得到的碳纤维再经聚邻苯二甲酸丙二醇酯、双酚A环氧树脂处理提高碳纤维材料整体强度,最后经与油脂具有优良亲和性的乙烯基苄基三甲基氯化铵结合,得到具有良好的物理化学稳定性和优异的机械强度的油脂吸附洗脱材料,由于稳定性强适合于多种复杂环境条件下应用,同时碳纤维本身极轻的质量令材料可以在水中悬浮,从而更多的接触油脂,提高油脂的吸附效率,具有很好的环境、经济效益,且易于规模化生产。
具体实施方式
一种含油废水吸附材料的制备方法,包括以下步骤:
(1)将聚邻苯二甲酸丙二醇酯、双酚A环氧树脂按质量比1:3.5混合后加热至110℃,搅拌至分散完全,降温至70℃后再向其中加入混合液体系质量的3%的对枯基聚醚基磺酸盐,搅拌40分钟,得预混液备用;
(2)将纺丝液置于静电纺丝仪中,使用铝箔纸包裹接收器,使初纺纤维收集在铝箔纸上,纺丝过程工艺参数为正压15kV,负压1.5kV,推进速率0.04mm/min,接收速率30r/min,针头与接收器之间距离为15cm,环境温度30℃,纺丝完成后在室温下静置一天,得到初纺纤维,再将其置于烘箱中,升温至160℃固化60分钟,取出后再送入管式炉中,在氮气气氛下以5℃/min的升温速率从室温升至750℃,保温1小时,自然冷却后得到碳纤维备用;
(3)以步骤2所得碳纤维作为阳极,石墨为阴极,在质量分数为8%的磷酸铵电解质中,控制电流密度为0.3A/m2,阳极氧化处理1.5分钟,收集碳纤维用清水冲洗净,得到改性碳纤维备用;
(4)将步骤1所得预混液用水稀释1.5倍后将步骤3所得改性碳纤维浸渍于其中,2分钟后取出,使用热风在130℃下吹2分钟干燥备用;
(5)将步骤4所得干燥产物与乙烯基苄基三甲基氯化铵、高锰酸钾以及水按质量比9:11:0.8:26混合后加热至70℃,反应4小时后冷却至室温,用水洗至滤液为中性,经固液分离后在60℃下干燥,即得本发明吸附材料。
所述纺丝液的制备方法为将椰壳粉碎过100目筛,烘干后与苯酚、浓硫酸按质量比6:22:0.8混合并搅拌均匀,置于140℃油浴锅中反应100分钟,之后降至室温,加入氢氧化钠中和pH至中性,将产物与80%二恶烷水溶液按体积比1:10混合搅拌60分钟,离心并过滤,除去残渣后将滤液经旋转蒸发仪在60℃下浓缩,除去二恶烷,得纯液化物,再与聚乙烯醇按质量比45:4混合后用氢氧化钠调节pH至10,之后加入甲醛溶液,加入的甲醛和苯酚物质的量之比为n(甲醛):n(苯酚)=1.5:1,升温至80℃,反应2小时后冷却至室温,得到纺丝液。
Claims (1)
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;
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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