CN110773138B - 一种树脂基负载铁氧化物复合除磷吸附剂的制备方法及其应用 - Google Patents
一种树脂基负载铁氧化物复合除磷吸附剂的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种树脂基负载铁氧化物复合除磷吸附剂的制备方法,以强碱性阴离子交换树脂为母体,以高铁酸钾为铁源,利用高铁酸根离子极易吸附于阴离子树脂表面的特性,通过一步法原位水解沉淀制备树脂基负载铁氧化物复合除磷吸附剂,与现有制备方法相比,本发明的制备过程相对更加简单,时间周期更短,生产成本更低。排除废水中其它阴离子的干扰能力强,对磷的吸附能力强、速度快、吸附量大,另外还具有再生能力强,重复使用次数多等优点。
Description
技术领域
本发明属于环境治理领域,具体涉及一种树脂基负载铁氧化物复合除磷吸附剂的制备方法,本发明还涉及复合除磷吸附剂的应用以及一种含磷废水污染处理方法。
背景技术
水体富营养化引起藻类及其他浮游生物迅速繁殖,水体溶解氧量下降,水质恶化,已成为危害人类健康、威胁饮用水安全的重要问题之一。过量磷输入是导致水体富营养化的重要因子,因此,开发有效的除磷剂是减少河流和湖泊水域中的磷输入的重要手段。
目前的除磷技术有化学沉淀法、生物法、膜分离法、吸附法等,但是单一技术往往难以适用于众多不同类型含磷废水的处理。因此,多技术组合使用则成为了优先选择。例如,在农田面源污染废水中磷的处理中,由于废水量大、含磷浓度低,导致化学沉淀法、膜分离法并不适用。生物法中的生态拦截沟渠是农田面源污染磷消减的有效技术之一,然而,生态拦截沟渠往往需要面临季节性问题,而将吸附法与生物法相结合,组建有别于传统的新型生态拦截沟渠,则可以有效解决这一问题。
构建新型生态拦截沟渠的核心则是吸附剂的筛选。传统的吸附剂主要包括活性炭、改性生物炭、赤泥、沸石、硅藻土、铁氧化物等。这些吸附剂尽管对废水中的磷具有一定的吸附能力,然而普遍在稳定性、吸附容量、选择性和实用性等方面存在一些问题。基于磷的去除与回收利用的思路,阴离子树脂被认为是一种理想的除磷材料。部分学者对其进行表面改性以降低阴离子树脂的选择性缺陷。铁(氢)氧化物因其环境友好、化学性质稳定、对磷吸附亲和力强而被认为理想的树脂改性材料。例如,潘炳才团队先后在CN 1772370A和文章(Development of polymer-based nanosized hydrated ferric oxides(HFOs)forenhanced phosphate removal from waste effluents)中报道了阴离子树脂上负载羟基铁氧化物去除砷和磷的研究。
这些方法的核心是将正价的Fe3+以FeCl4 -的形式负载到阴离子树脂上,导致工艺过程复杂,极大的增加了树脂基载铁树脂复合出磷吸附剂的成本。因此,开发生产成本低廉、经济适用、除磷效率稳定的吸附剂材料仍是当前的迫切需求。高铁酸钾是一种集氧化、消毒、絮凝和助凝等多种功能于一体的水处理药剂,其还原产物可形成比铝盐、铁盐水解产物具有更大网状结构,更高正电荷的水解产物,且安全无毒,在低浓度、碱性条件下溶液较为稳定。利用高铁酸根易吸附于阴离子树脂上的特性,一步原位水解制备树脂基载铁复合除磷吸附剂,从而开发更为经济的含铁复合树脂。
发明内容
本发明的目的是提供一种吸附量大、稳定性强、重复利用率高、选择性好、易制备的复合除磷材料,
本发明的技术方案如下:
一种树脂基负载铁氧化物复合除磷吸附剂的制备方法,包括以下步骤:
将强碱性阴离子树脂加入到新鲜制备的碱性高铁酸钾溶液中,常温搅拌1-5小时,使高铁酸根与树脂上的阴离子发生交换反应,弃去上清液后加入清水,加热到50-70℃继续搅拌1-3小时,使交换到树脂上的高铁酸根完全水解成氢氧化铁,之后加入质量分数2-10%的氯化钠溶液,使阴离子树脂上结合的羟基转型为Cl-,最后将负载纳米级水合氧化铁后的复合树脂水洗至中性,干燥后即得。
优选地,所述强碱性阴离子树脂为D-201树脂、201×7树脂、201×4树脂、IRA-900树脂或IRA-402树脂。
优选地,所述碱性高铁酸钾溶液的浓度为0.03~0.2mol/L。
优选地,所述碱性高铁酸钾溶液的pH为9~12。
优选地,所述强碱性阴离子树脂的加入量为20~200g/L。
所述树脂基负载铁氧化物复合除磷吸附剂可用于含磷废水污染处理。
一种含磷废水污染处理方法,包括以下步骤:
1)将按以上所述方法制备的树脂基负载铁氧化物复合除磷吸附剂装柱,将含磷废水上柱后控制温度20-40℃,流速10-30BV/h,进行洗脱;
2)洗脱完成后向树脂内加入质量浓度为2-5%NaCl和2-5%NaOH混合溶液进行树脂再生。
本发明所涉及得反应式:
(1)铁酸根交换到阴离子树脂上:
2R-N+(CH3)3Cl(s)+FeO4 2-(a)→(R-N+(CH3)3)2FeO4(s)+2Cl-(a)
(2)铁酸根在阴离子树脂上水解:
4(R-N+(CH3)3)2FeO4(s)+10H2O(a)→4Fe(OH)3(s)+3O2+8R-N+(CH3)3OH(s)
(3)质量分数5%的氯化钠溶液进行转型:
R-N+(CH3)3OH(s)+NaCl(a)→R-N+(CH3)3Cl(s)+NaOH(a)
与现有技术相比,本发明具有以下优点:
1)本发明以强碱性阴离子交换树脂为母体,以铁酸钾为铁源,利用铁酸根离子极易吸附于阴离子树脂表面的特性,通过一步法原位水解沉淀制备树脂基负载铁氧化物复合除磷吸附剂,与现有制备方法相比,本发明的制备过程相对更加简单,时间周期更短,生产成本更低。
2)本发明的吸附剂用于含磷废水污染处理时,排除废水中其它阴离子的干扰能力强,对磷的吸附能力强、速度快、吸附量大,另外还具有再生能力强,重复使用次数多等优点。
附图说明
图1为实施例7的生态沟立体示意图。图中1-水生植物茭白、2-砾石、3-第一取水点、4-100目尼龙网袋包裹载铁树脂、5-固定铁架、6-第二取水点、7-溢流堰。
具体实施方式
以下通过具体实施例进一步说明本发明。
实施例1
取7.14g高铁酸钾溶于400ml、pH=10的水溶液中,配置成浓度为0.09mol/L的高铁酸钾溶液,立即将20g IRA-402树脂加入到高铁酸钾溶液中,磁力搅拌2h,使高铁酸根与树脂上的阴离子发生交换,而后将上清液倒去并加入清水200mL,50℃下搅拌1小时,使树脂上的高铁酸根完全水解成氢氧化铁,之后用质量分数5%的氯化钠溶液使阴离子树脂上结合的羟基转型为Cl-,最后将负载了纳米级水合氧化铁的复合树脂水洗至中性,于阴凉处风干或烘干,即获得复合除磷吸附剂,其Fe(Ⅲ)的固载量为25.7mg/g。
实施例2
取13.85g高铁酸钾溶于1000ml、pH=12的水溶液中,配置成浓度为0.07mol/L的高铁酸钾溶液,立即将100g IRA-900树脂加入到高铁酸钾溶液中,机械搅拌2h,使高铁酸根与树脂上的阴离子发生交换,而后将上清液倒去并加入清水500mL,70℃下搅拌1小时,使树脂上的高铁酸根完全水解成氢氧化铁,之后用质量分数2%的氯化钠溶液使阴离子树脂上结合的羟基转型为Cl-,最后将负载了纳米级水合氧化铁的复合树脂水洗至中性,于阴凉处风干或烘干,即得复合除磷吸附剂,其Fe(Ⅲ)的固载量为24.5mg/g。
实施例3
取5.94g高铁酸钾溶于200ml、pH=9的水溶液中,配置成浓度为0.15mol/L的高铁酸钾溶液,立即将40g D-201树脂加入到高铁酸钾溶液中,磁力搅拌3h,使高铁酸根与树脂上的阴离子发生交换,而后将上清液倒去并加入清水100mL,60℃下搅拌2小时,使树脂上的高铁酸根完全水解成氢氧化铁,之后用质量分数8%的氯化钠溶液使阴离子树脂上结合的羟基转型为Cl-,最后将负载了纳米级水合氧化铁的复合树脂水洗至中性,于阴凉处风干或烘干,即得复合除磷吸附剂,其Fe(Ⅲ)的固载量为39.2mg/g。
实施例4
在100mL含有不同硫酸根浓度(0~15mM)的磷酸盐溶液(0.1mM P-PO4 3-)中分别加入实施例1~3制得的复合树脂(0.5g/L)进行吸附实验,溶液初始pH为7(吸附过程无调整),恒温震荡吸附24h,检测悬液中的剩余磷含量,计算除磷率,并与原始树脂对比,结果见表1。
表1不同硫酸根浓度测得的除磷率(%)
SO<sub>4</sub><sup>2-</sup>(mM) | 0 | 0.15 | 0.3 | 0.6 | 1 | 3 | 5 | 10 | 15 |
实施例1 | 99 | 99 | 97 | 69 | 42 | 30 | 28 | 26 | 25 |
实施例2 | 93 | 90 | 78 | 54 | 32 | 21 | 19 | 18 | 18 |
实施例3 | 96 | 92 | 84 | 44 | 26 | 24 | 22 | 19 | 17 |
IRA-402 | 90 | 76 | 69 | 19 | 6 | 5 | 1 | 0 | 0 |
IRA-900 | 85 | 68 | 30 | 15 | 2 | 0 | 0 | 0 | 0 |
D-201 | 88 | 73 | 42 | 24 | 10 | 4 | 0 | 0 | 0 |
从以上结果可以看出,随着硫酸根浓度升高,树脂的除磷率相应下降,但是负载纳米水合氧化铁的的树脂除磷率明显高于未处理的树脂。尤其是实施例1直到硫酸根浓度达到0.3mM时,除磷率仍未见明显下降,因此对磷的吸附选择性最高,抗干扰能力最强。
实施例5
将实施例1~3制得的复合树脂加入到初始pH=7,磷酸根浓度为10mg/L的溶液中,复合树脂的投加量为0.5g/L,然后于10、20、30、45、60、80、100、120min不同时间点取样,检测悬液中的剩余磷含量,计算除磷率,并与原始树脂对比,结果见表2。
表2不同时间点测得的除磷率(%)
时间(min) | 10 | 20 | 30 | 45 | 60 | 80 | 100 | 120 |
实施例1 | 10 | 19 | 26 | 39 | 45 | 54 | 62 | 69 |
实施例2 | 9 | 21 | 30 | 39 | 51 | 64 | 69 | 73 |
实施例3 | 11 | 24 | 29 | 41 | 52 | 63 | 67 | 72 |
IRA-402 | 5 | 13 | 22 | 31 | 38 | 47 | 52 | 56 |
IRA-900 | 5 | 14 | 20 | 25 | 33 | 41 | 45 | 52 |
D-201 | 7 | 11 | 18 | 26 | 33 | 42 | 46 | 54 |
从以上结果可以看出,随着时间延长,树脂的除磷率相应增加,但是负载纳米水合氧化铁的树脂除磷率明显高于未处理的树脂,因此本发明对磷的吸附能力更强,速度更快。
实施例6
分别将实施例1、2、3制得的复合树脂5mL加入到内径12mm,长25mm的有机玻璃吸附柱中,将含磷废水(P=2mg/L,及SO4 2-=120mg/L、Cl-=HCO3 -=100mg/L、NO3 -=40mg/L,pH=7)自上而下顺流通过吸附柱,温度=30℃,控制流速15BV/h,三个实施例出水P浓度控制在0.5mg/L以下的处理量分别见表3。吸附穿透后,用50mL质量百分比均为4%的NaCl和NaOH混合溶液在20℃下以10mL/h的流量通过吸附柱进行树脂再生,再生率分别见表3,再生树脂用清水冲洗至中性即可继续使用。
废水处理量 | 树脂再生率(>) | |
实施例1 | 630BV | 98% |
实施例2 | 650BV | 98% |
实施例3 | 550BV | 97% |
IRA-402 | 350BV | 99% |
IRA-900 | 360BV | 99% |
D-201 | 310BV | 99% |
从以上结果可以看出,负载纳米水合氧化铁的树脂对含磷废水的处理量远高于未处理的树脂,而且处理后的树脂具有很强的再生能力。
实施例7
将实施例1制得的复合树脂加入到硬质生态沟渠中,具体结构见附图1。处理约6亩水田所产生的农田径流,在连续监测的54天里,第二取样点与第一取样点相比,农田径流中PO34-平均消减量为34.4%。
Claims (3)
1.一种树脂基负载铁氧化物复合除磷吸附剂的制备方法,其特征在于包括以下步骤:
将强碱性阴离子树脂加入到新鲜制备的碱性高铁酸钾溶液中,常温搅拌1-5小时,使高铁酸根与树脂上的阴离子发生交换反应,弃去上清液后加入清水,加热到50-70℃继续搅拌1-3小时,使交换到树脂上的高铁酸根完全水解成氢氧化铁,之后加入质量分数2-10%的氯化钠溶液,使阴离子树脂上结合的羟基转型为Cl-,最后将负载纳米级水合氧化铁后的复合树脂水洗至中性,干燥后即得,
所述强碱性阴离子树脂为IRA-402树脂,
所述碱性高铁酸钾溶液的浓度为0.03~0.2mol/L,pH为9~12,
所述强碱性阴离子树脂的加入量为20~200g/L。
2.树脂基负载铁氧化物复合除磷吸附剂在含磷废水污染处理中的应用,其特征在于:所述树脂基负载铁氧化物复合除磷吸附剂是按权利要求1所述方法制备的。
3.一种含磷废水污染处理方法,其特征在于包括以下步骤:
1)将按权利要求1所述方法制备的树脂基负载铁氧化物复合除磷吸附剂装柱,将含磷废水上柱后控制温度20-40℃,流速10-30BV/h,进行洗脱;
2)洗脱完成后向树脂内加入质量浓度为2-5%NaCl和2-5%NaOH混合溶液进行树脂再生。
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