CN111346619B - 一种改性赤泥质滤料的制备方法及其对低温污水中氨氮的去除 - Google Patents

一种改性赤泥质滤料的制备方法及其对低温污水中氨氮的去除 Download PDF

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CN111346619B
CN111346619B CN202010309150.6A CN202010309150A CN111346619B CN 111346619 B CN111346619 B CN 111346619B CN 202010309150 A CN202010309150 A CN 202010309150A CN 111346619 B CN111346619 B CN 111346619B
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朱琦
孙宇池
邢子鹏
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Abstract

本发明涉及一种改性赤泥质滤料对低温污水中氨氮的去除方法，解决了污水处理厂低温条件下生物脱氮效果差导致总氮不达标的问题。本发明所制备的处理氨氮的滤料安全无毒，原材料含有木质素和赤泥，其中木质素从秸秆中提取，赤泥来自工业制铝废渣，实现了废物资源化，降低了滤料的成本，体现了绿色可持续发展。本发明专门应用于低温情况下污水处理超标的情况，降低后续生物处理负荷，有助于含氨氮污水达标排放。

Description

一种改性赤泥质滤料的制备方法及其对低温污水中氨氮的 去除
技术领域
本发明涉及一种新型水中去除氨氮的滤料的制备方法及其应用。利用从秸秆中提取的木质素和赤泥为原料制备的去除氨氮的滤料，在低温水环境下快速去除水中氨氮的新型滤料。
背景技术
城市污水处理中，基于传统硝化和反硝化的活性污泥脱氮技术容易受到温度或水质水量急剧变化的影响，使得生物处理能力下降，导致排放不达标。继而导致水体富营养化等问题，所以研制一种低温下有效去除污水中氨氮的滤料，在生物处理前投放，可降低后续生物处理负荷，利于氨氮达标排放。
本发明涉及一种从秸秆中提取木质素制备新型水中氨氮滤料的制备方法及其应用。世界上每年通过光合作用产生约1500亿吨木质素，玉米秸秆、水稻秸秆中含有大量木质素，造纸工业每年产生约5000万吨左右木质素，工业上利用还不到10%，其中大部分直排到自然环境中或被焚烧掉。赤泥是铝工业生产氧化铝而产生的固体废渣，我国每年排放的赤泥量高达数千万吨，如不能得到有效利用从而大量堆积，既浪费资源又占用土地且污染环境。本发明研发的新型滤料，有效的利用了赤泥和秸秆木质素，实现了固体废物资源化。
发明内容
本发明所述氨氮吸附剂制备方法步骤如下：
a、取25.0g经过处理后的玉米秸秆粉末，按照固液比1:15加入375mL浓度为4wt%NaOH溶液，混匀后加热至80℃，搅拌条件下反应3h；彻底反应后，抽滤将不溶物从溶液中分离出来，用10%的HCl将抽滤后溶液pH控制在2，析出不溶物，再次抽滤，将不溶物多次离心至中性后80℃烘干，即得所需木质素；
b、称量1.0g木质素，放入9mL去离子水，加3mL戊二醛溶液，用0. 01 mol/L的氢氧化钠溶液调节pH到12，加热至90℃并搅拌6h；将产物抽滤并烘干，制得交联改性木质素；
c、取1.0g上述制备的交联木质素，按照木质素：苯酚=1:9.5的比例加入苯酚、1.0gAlCl3·6H2O、1mL水加入至烧瓶中匀速搅拌均匀；将上述药品转移至反应釜中，140℃反应2h；待其凉至室温后，用0.5mol/L NaOH溶解，滴加2mol/L HCl溶液使不溶物析出，抽滤后用80℃蒸馏水多次洗涤得到棕褐色酚化改性木质素；
d、将赤泥进行淘洗、研磨之后，再进行原料配比、球磨和造粒之后，焙烧，将焙烧好的颗粒滤料取出；将上述步骤中制备的改性木质素负载至赤泥颗粒滤料上，得到可以吸附氨氮的颗粒滤料。
与目前使用的去除氨氮滤料相比：
1.本发明的新型去除氨氮滤料在水中表面带有大量负电荷，在低温条件下同样能够很好地静电吸附水中的氨氮，增加吸附的用量可以降低污水厂后续工艺处理的负荷，在不改变现有的工艺条件下能够稳定对水体做出净化达标排放；
2.经过处理后氨氮浓度仍然不达标的污水，可将其利用此滤料进行处理，经过处理后氨氮浓度大大降低，低温情况下依旧不受影响，处理过程不复杂，滤料易回收，可重复利用；
3.原材料均廉价易得，不会造成二次污染，适合实际应用。
具体实施方式
一种新型去除水中氨氮的滤料的制备方法及其应用，所述方法如下步骤：
权利要求1-6中任一项所述的滤料制备方法及其应用，所述步骤如下：
a、取25.0g经过处理后的玉米秸秆粉末，按照固液比1:15加入375mL浓度为4wt%NaOH溶液，混匀后加热至80℃，搅拌条件下反应3h；彻底反应后，抽滤将不溶物从溶液中分离出来，用10%的HCl将抽滤后溶液pH控制在2，析出不溶物，再次抽滤，将不溶物多次离心至中性后80℃烘干，即得所需木质素；
b、称量1.0g木质素，放入9mL去离子水，加3mL戊二醛溶液，用0. 01 mol/L的氢氧化钠溶液调节pH到12，加热至90℃并搅拌6h；将产物抽滤并烘干，制得交联改性木质素；
c、取1.0g上述制备的交联木质素，按照木质素：苯酚=1:9.5的比例加入苯酚、1.0gAlCl3·6H2O、1mL水加入至烧瓶中匀速搅拌均匀；将上述药品转移至反应釜中，140℃反应2h；待其凉至室温后，用0.5mol/L NaOH溶解，滴加2mol/L HCl溶液使不溶物析出，抽滤后用80℃蒸馏水多次洗涤得到棕褐色酚化改性木质素；
d、将赤泥进行淘洗、研磨之后，再进行原料配比、球磨和造粒之后，焙烧；将焙烧好的颗粒滤料取出；将上述步骤中制备的改性木质素负载至赤泥颗粒滤料上，得到可以吸附氨氮的颗粒滤料。
实施效果：
使用上述制备方法制备的滤料对污水进行处理，通过《纳式试剂分光光度法》HJ535-2009测定处理的浓度；对于氨氮浓度为68.04mg/L的生活污水，当滤料投加量为100.3g/L，滤料在水中停留时间为2.5h，水体温度为2℃，水体pH为8时，最佳去除率达到73.6%。

Claims (6)

1.一种改性赤泥质滤料的制备方法，所述的制备方法包括如下步骤：
a、取25.0g经过处理后的玉米秸秆粉末，按照固液比1:15加入375mL浓度为4wt%NaOH溶液，混匀后加热至80℃，搅拌条件下反应3h；彻底反应后，抽滤，将不溶物从溶液中分离出来，用10%的HCl将抽滤后溶液pH控制在2，析出不溶物，再次抽滤，将不溶物多次离心至中性后80℃烘干，即得所需木质素；
b、称量1.0g木质素，放入9mL去离子水，加3mL戊二醛溶液，用0. 01 mol/L的氢氧化钠溶液调节pH到12，加热至90℃并搅拌6h；将产物抽滤并烘干，制得交联木质素；
c、取1.0g上述制备的交联木质素，按照木质素：苯酚=1:9.5的比例加入苯酚、1.0gAlCl3·6H2O、1mL水加入至烧瓶中匀速搅拌均匀，转移至反应釜中，140℃反应2h；待其凉至室温后，用0.5mol/L NaOH溶解，滴加2mol/L HCl溶液使不溶物析出，抽滤后用80℃蒸馏水多次洗涤得到棕褐色交联酚化木质素；
d、将赤泥进行淘洗、研磨之后，再进行原料配比、球磨和造粒之后，焙烧；将0.2g聚乙烯醇80℃加热溶于120mL去离子水中，完全溶解后冷却至室温，消泡待用；取0.2g上述制备的交联酚化木质素与1mL上述制备的聚乙烯醇溶液混合成均匀悬浊胶状，喷涂于赤泥颗粒上，并于电热鼓风干燥箱中60℃干燥12h，得到可以吸附氨氮的颗粒滤料。
2.根据权利要求1中所述的制备方法得到的赤泥质滤料在氨氮去除中的应用，其特征在于，所述赤泥质滤料在水温1℃至10℃下吸附水中NH4 +，去除率为55.6%-73.5%。
3.根据权利要求1中所述的制备方法得到的赤泥质滤料在氨氮去除中的应用，其特征在于，所述赤泥质滤料投加66.7g/L至200g/L时，去除率是64.7%-85.3%。
4.根据权利要求1中所述的制备方法得到的赤泥质滤料在氨氮去除中的应用，其特征在于，所述赤泥质滤料吸附时间范围在0.5h至4h，去除率为52.8%-78.2%。
5.根据权利要求1中所述的制备方法得到的赤泥质滤料在氨氮去除中的应用，其特征在于，所述赤泥质滤料在pH为5至10范围内处理水中NH4 +，去除率为57.6%-70.1%。
6.根据权利要求1中所述的制备方法得到的赤泥质滤料在氨氮去除中的应用，其特征在于，所述赤泥质滤料在0.025g/L至0.125g/L NH4 +范围的污水进行处理，去除率为42.9%-87.6%。
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