CN106268624A - 一种吡虫啉废水处理的改性吸附剂 - Google Patents
一种吡虫啉废水处理的改性吸附剂 Download PDFInfo
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Abstract
本发明公开了一种吡虫啉废水处理的改性吸附剂,属于污水处理及环境治理领域。本发明通过对膨润土进行钠化改性,再向钠化膨润土料浆中加入复配活性剂进行2‑3h的插层反应,经过后续固液分离、洗涤、真空抽滤,烘干研磨等步骤制备所述改性吸附剂。本发明的方法制备的改性吸附剂能够有效去除废水中的吡虫啉,反应60min吡虫啉去除率达85%以上,可以应用于吡虫啉废水处理及材料资源化等方面,减少废液排放,减轻环境压力,具有良好的应用前景。
Description
技术领域
本发明涉及一种吡虫啉废水处理的改性吸附剂,属于污水处理及环境治理领域。
背景技术
吡虫啉工业废水含有有机含量高、色度深、排放量大、水质复杂等问题而成为难以治理的工业废水,其中因为吡虫啉具有良好的亲水性和理化特征,使其成为吡虫啉废水中难去除的有机物之一。在目前最常见的化学、生物和物理脱色处理中,其中最为简便和有效的吸附脱除法是物理法。活性炭是迄今为止最优良的吸附剂之一,但是由于活性炭价格及再生费用高等各种限制,因此有关学者的研究热点是如何开发和利用高效廉价的吸附剂。
膨润土(Bentonite)是我国含量丰富的一种以蒙脱石(Montmorillonite)为主要成分的一类层状硅酸盐粘土矿物,该粘土矿物具有独特使其对重金属离子等具有良好的交换性和选择性的晶体结构,因此其在环境保护领域具有广泛的发展前途及应用价值。因为膨润土具有吸水性强的特性,其体积随所吸水分增多而胀大,但在加热后又失去所吸水分。而它的晶层之间存在使层间距离增加,且更易吸附极性水分子而膨胀常吸附Ca2+、Na+等阳离子,根据阳离子种类及相对湿度的不同,层间可以吸附一层或两层水分子。又由于其结构具有能决定膨润土其良好的离子交换能力和吸附性能的特殊性,为其在污水处理及应用中奠定了一定的基础。但多数膨润土是一种具有溶胀性,遇水形成泥浆,通透性能很差,资源利用水平、低粉末状特点的粘土,为初级产品,且由于其表面硅氧结构极强的亲水性及层间阳离子的水解,使其表面通常存在一层薄的水膜。而一般的有机污染物为疏水性物质,故膨润土原土吸附处理有机物的效果较差。除此之外,原土不能去除水中的阴离子污染物,又限制了膨润土在环保领域的应用的原因是因为硅氧结构本身带负电荷。
因此,为了提高其对污水在实际应用中的处理能力,一般要对膨润土原土进行良性改良。因为改性处理不仅能增大其比表面积而且大大提高膨润土的吸附性能,并能有效吸附水溶液中的重金属离子等污染物质。目前用于废水处理的膨润土都是经过了一次或二次改性处理之后的土,其中活化法、添加改进剂法和柱撑是最常用的膨润土改性方法。但是,常规方法改性的膨润土在实际吸附过程中,存在改性剂用量偏大,吸附性能的提高有限等缺点。新型的表面活性剂Gemini是由两个双亲组分在极性基团处或距极性基团很近的烷基链上由联接基团将它们连接在一起而形成的表面活性剂,由于其特有的化学结构,与普通的表面活性剂相比,有许多独特的性能,例如较低的临界胶束浓度,较高的表面活性、润湿性、可溶性、发泡性和钙-皂分散性等性能,被用于膨润土改性过程。虽然Gemini表面活性剂具有上述的优异特性,但是其较高的价格压制了其在工业上的应用,因此,制备一种成本低廉、性能优异的用于膨润土改性的表面活性剂具有重要的工业应用价值。
发明内容
本发明的第一个目的是提供一种复配表面活性剂,是以无水乙醇为溶剂,将十二烷基三甲基溴化铵与Gemini表面活性剂以0.5~0.8的质量比,在10-40℃条件下进行复配;所述十二烷基三甲基溴化铵与Gemini表面活性剂的总质量浓度为1~3%。
在本发明的一种实施方式中,所述Gemini表面活性剂是12-3-12·2Br型Gemini表面活性剂。
本发明的第二个目的是提供所述复配表面活性剂的应用。
在本发明的一种实施方式中,所述应用包括制备改性吸附剂、清洁剂、乳化剂。
本发明的第三个目的是提供一种吡虫啉废水处理的改性吸附剂的制备方法,所述方法是向膨润土中加入与膨润土质量比为0.001-0.002的钠化改性剂,再将钠化膨润土料浆边搅拌边加热直至40-80℃,同时缓慢加入与膨润土质量比为0.001-0.003的权利要求1所述复配表面活性剂溶液进行2-3h的插层反应,反应结束后,进行固液分离、洗涤、真空抽滤,收集湿样于70-100℃条件下进行烘干,并在90-130℃活化1-1.5h,然后研磨制成粉状产品。
在本发明的一种实施方式中,所述钠化改性剂包括NaCl,Na2CO3,NaHCO3,NaOH,NaF。
本发明的第四个目的是提供应用所述方法制备的改性吸附剂。
本发明的第五个目的是提供一种降低吡虫啉含量的方法,所述方法是向含有吡虫啉的溶液中所述改性吸附剂,在45℃-50℃,以130r/min-160r/min的转速恒温振荡50min-70min。
在本发明的一种实施方式中,所述含有吡虫啉的溶液中吡虫啉浓度为100ppm-400ppm。
有益效果:本发明制备的复配表面活性剂,具有很高的表面活性、润湿性、可溶性、发泡性和钙-皂分散性以及很低的临界胶束浓度、很低的C20等性能。本发明制备的改性吸附剂,对吡虫啉废水中吡虫啉的去除率可达85%以上。可以应用于吡虫啉废水处理及材料资源化等方面,可以减少废液排放,减轻环境压力,具有良好的应用前景。
具体实施方式
复配表面活性剂的性能测定方法:将复配表面活性剂溶液恒温至298.15K,由JM99B型动态膜压记录仪测定表面张力,得出表面张力与浓度的对数曲线,通过曲线计算C20值;由DDS-307型数字式电导率仪(采用DJS-1C型铂黑电导电极)测定其电导率,得出电导率-浓度曲线,通过曲线计算CMC值。
吡虫啉浓度检测方法:采用HPLC(Waters2695),C18键合固定相色谱柱(4.6mm×250mm,5μm),流动相A相甲醇,流动相B相水,甲醇:水的体积比为6:4,流速1mL/min,紫外检测器,波长270nm,进样量10μL,柱温:40℃。
实施例1
以无水乙醇为溶剂,将十二烷基三甲基溴化铵与Gemini表面活性剂以0.5~0.8的质量比,在10-40℃条件下进行复配;所述十二烷基三甲基溴化铵与Gemini表面活性剂的总质量浓度为1~3%。经测定,复配表面活性剂具有很高的表面活性、润湿性、可溶性、发泡性和钙-皂分散性以及很低的临界胶束浓度、很低的C20等性能,其临界胶束浓度可达2.36mmol/L,C200.38mmol/L。
实施例2
称取0.5g十二烷基三甲基溴化铵与0.8g 12-3-12·2Br型Gemini表面活性剂,量取100mL无水乙醇溶剂,在25℃配制复配表面活性剂溶液。对100g膨润土先进行活化改性处理,再对钠化膨润土料浆边搅拌边加热直至60℃后,同时缓慢加入10ml复配表面活性剂溶液进行2h的插层反应。当反应结束后,对其进行固液分离、洗涤、真空抽滤,湿样90℃条件下进行烘干,并在105℃活化1h,然后研磨制成粉状产品,密封备用。量取100ml浓度为200ppm的吡虫啉废水,加入1g制备好的改性吸附剂,在40℃温度下,以150r/min的转速恒温振荡60min,测量吸附后吡虫啉废水中吡虫啉浓度为28.9ppm,去除率为85.6%。
实施例3
称取0.5g十二烷基三甲基溴化铵与1.0g 12-3-12·2Br型Gemini表面活性剂,量取100mL无水乙醇溶剂,在温度为20℃配制成复配表面活性剂溶液。对100g膨润土先进行活化改型处理,再通过蒸汽对钠化膨润土料浆进行边搅拌边给***加热直至60℃后,同时缓慢加入10ml复配表面活性剂溶液进行2h的插层反应。当反应结束后,对其进行固液分离、洗涤、真空抽滤,湿样95℃条件下进行烘干,并在110℃活化1h,然后研磨制成粉状产品,密封备用。量取100ml浓度为200ppm的吡虫啉废水,加入1g制备好的改性吸附剂,在45℃温度下,以150r/min的转速恒温振荡60min,测量吸附后吡虫啉废水中吡虫啉浓度为27.6ppm,去除率为86.2%。
实施例4
称取0.5g十二烷基三甲基溴化铵与1.5g 12-3-12·2Br型Gemini表面活性剂,量取100mL无水乙醇溶剂,在温度为20℃配制成复配表面活性剂溶液。对100g膨润土先进行活化改型处理,再通过蒸汽对钠化膨润土料浆进行边搅拌边给***加热直至60℃后,同时缓慢加入10ml复配表面活性剂溶液进行2h的插层反应。当反应结束后,对其进行固液分离、洗涤、真空抽滤,湿样95℃条件下进行烘干,并在110℃活化1h,然后研磨制成粉状产品,密封备用。量取100ml浓度为200ppm的吡虫啉废水,加入1g制备好的改性吸附剂,在45℃温度下,以150r/min的转速恒温振荡60min,测量吸附后吡虫啉废水中吡虫啉浓度为38.5ppm,去除率为80.8%。
实施例5
称取1.5g十二烷基三甲基溴化铵与0.5g 12-3-12·2Br型Gemini表面活性剂,量取100mL无水乙醇溶剂,在温度为20℃配制成复配表面活性剂溶液。对100g膨润土先进行活化改型处理,再通过蒸汽对钠化膨润土料浆进行边搅拌边给***加热直至60℃后,同时缓慢加入10ml复配表面活性剂溶液进行2h的插层反应。当反应结束后,对其进行固液分离、洗涤、真空抽滤,湿样95℃条件下进行烘干,并在110℃活化1h,然后研磨制成粉状产品,密封备用。量取100ml浓度为200ppm的吡虫啉废水,加入1g制备好的改性吸附剂,在45℃温度下,以150r/min的转速恒温振荡60min,测量吸附后吡虫啉废水中吡虫啉浓度为56.3ppm,去除率为71.9%。
实施例6
称取1.3g 12-3-12·2Br型Gemini表面活性剂,量取100mL无水乙醇溶剂,在25℃配制表面活性剂溶液。对100g膨润土先进行活化改性处理,再对钠化膨润土料浆边搅拌边加热直至60℃后,同时缓慢加入10ml表面活性剂溶液进行2h的插层反应。当反应结束后,对其进行固液分离、洗涤、真空抽滤,湿样90℃条件下进行烘干,并在105℃活化1h,然后研磨制成粉状产品,密封备用。量取100ml浓度为200ppm的吡虫啉废水,加入1g制备好的改性吸附剂,在40℃温度下,以150r/min的转速恒温振荡60min,测量吸附后吡虫啉废水中吡虫啉浓度,结果显示,其对吡虫啉废水中吡虫啉的去除率相比是实施例1下降5.1%,但由于Gimini表面活性剂成本高,制备的改性膨润土处理单位体积废水成本提高57.6%,不适合工业化应用。
虽然本发明已以较佳实施例公开如上,但其并非用以限定本发明,任何熟悉此技术的人,在不脱离本发明的精神和范围内,都可做各种的改动与修饰,因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (9)
1.一种复配表面活性剂,其特征在于,以无水乙醇为溶剂,将十二烷基三甲基溴化铵与Gemini表面活性剂以0.5~0.8的质量比在10~40℃条件下进行复配;所述十二烷基三甲基溴化铵与Gemini表面活性剂的总浓度为10~30g/L。
2.根据权利要求1所述的复配表面活性剂,其特征在于,所述Gemini表面活性剂包括12-3-12·2Br型Gemini表面活性剂。
3.权利要求1或2所述复配表面活性剂在制备改性吸附剂、清洁剂、乳化剂中的应用。
4.一种吡虫啉废水处理的改性吸附剂的制备方法,其特征在于,向膨润土中加入与膨润土质量比为0.001-0.002的钠化改性剂,再将钠化膨润土料浆边搅拌边加热直至40-80℃,同时缓慢加入与膨润土质量比为0.001-0.003的权利要求1所述复配表面活性剂进行2-3h的插层反应,反应结束后,进行固液分离、洗涤、真空抽滤,收集湿样于70-100℃条件下进行烘干,并在90-130℃活化1-1.5h,然后研磨制成粉状产品。
5.根据权利要求3所述的方法,其特征在于,所述钠化改性剂包括NaCl、Na2CO3、NaHCO3、NaOH或NaF。
6.权利要求4或5所述方法制备的改性吸附剂。
7.一种降低吡虫啉含量的方法,其特征在于,向含有吡虫啉的溶液中加入权利要求6所述的改性吸附剂,在45℃-50℃,以130r/min-160r/min的转速恒温振荡50min-70min。
8.根据权利要求7所述的方法,其特征在于,所述含有吡虫啉的溶液中吡虫啉浓度为100ppm-400ppm。
9.权利要求6所述改性吸附剂在污水处理中的应用。
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Title |
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YAZHUO SHANG等: "Effect of Ionic Liquids CnmimBr on Properties of Gemini Surfactant 12-3-12 Aqueous Solution", 《IND. ENG. CHEM. RES.》 * |
李万鑫等: "Gemini 表面活性剂改性膨润土对有机红染料的吸附性能研究", 《山东化工》 * |
董燕等: "有机膨润土对吡虫啉的吸附", 《广西大学学报: 自然科学版》 * |
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