CN107986386A - 一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法 - Google Patents
一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法 Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
Abstract
本发明公开了一种采用UV/Na2SO3光还原降解2,4,6‑三溴酚的方法,在含有2,4,6‑三溴酚的水中,加入亚硫酸钠,曝气除去溶解氧,控制溶液pH,进行紫外光照反应,实现降解2,4,6‑三溴酚。本发明采用UV/Na2SO3光还原降解2,4,6‑三溴酚,在三溴苯酚初始质量浓度100mg·L‑1,三溴酚的降解率随紫外光解时间的增加而增加,2min~10min降解速率明显增加,至20min几乎完全降解。当SO3 2‑浓度为10mmol·L‑1时,三溴苯酚的降解率明显提高,三溴酚在SO3 2‑浓度为10mmol/L的UV/Na2SO3体系中,每个时间梯度pH=6时降解率呈稳定上升状态,在pH=6的条件下降解效果最佳。
Description
技术领域
本发明属于有机污染物处理技术领域,具体涉及一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法。
背景技术
卤代酚类有机污染物是一类在地表水、土壤等自然环境中普遍存在的有毒有机污染物,来源主要包括农药、防腐剂、工业溶剂和助燃剂等。而溴代酚类物质中,三溴苯酚作为一种重要的阻燃剂中间体而被广泛应用。2,4,6-三溴酚是一种非常好的助燃剂,可用于塑料工艺的改性。因此,2,4,6-三溴酚在世界内大量生产,2001年年产量达到9500t。研究发现在江河湖泊的水体和底泥、空气和土壤、生物体内甚至人乳中都有发现,对人类健康和环境造成持久性危害。
溴代酚类有机废水成分复杂,有机物含量高,处理难度极大。首先,溴代酚类有机污染物在水中的含量一般比较低,以至于一般的常规的水处理工艺无法有效的除去,需要一些更加高效的水处理工艺来降解这些有污染物。其次,溴代酚类有机物由于自身结构的原因使其在水中的溶解度很低,容易通过食物链富集,而且难以通过微生物降解方法把它从环境中去除出来。
卤代有机物的特点就是大部分都有 C-X 键,而卤素原子较大的电负性和较强的诱导效应使得在处理这类有机物的过程中还原性的方法反而会起到意想不到的效果。紫外强化还原技术就是指利用紫外活化还原剂产生还原性的活性物种(主要要为水合电子以及氢原子),来还原水中有机物的方法,目前常用的还原剂有铁氰酸盐,碘化钾,亚硫酸盐等。针对卤代有机物而言,水合电子(eaq -)是一种最有效的选择性活性物种,所谓选择性活性物种,其特点就是可以有针对性的和目标污染物迅速的进行反应,从而使得其对污染物的降解可以持续的保持在一个很高的效率上,这样相比于羟基自由基的体系,其能耗以及成本都会大大的降低。在针对微污染物去除的情况下,选择性自由基的效率优势会更加明显。水合电子的氧化还原电位是-2.9V,在所有已知的还原剂中,是活性最高的一种。由于其较强的还原性,它可以和很多卤代有机物以扩散控制的速率反应。同时随着 C-X 的断裂而脱卤释放出卤素离子。但是目前针对还原性脱卤的研究还十分少。ellanki 和 Bachelor 教授在文献中对目前的几种紫外强化还原技术做了系统的比较,实验表明紫外-亚硫酸盐体系的还原效果最好。同时李旭春在文献中阐述了 MCAA 在紫外-亚硫酸盐体系下出色的降解效果。实验表明,在紫-亚硫酸盐体系下,一氯乙酸的降解效率随着初始浓度的增加而降低,亚硫酸盐是通过光照产生的水合电子从而更有效的将一氯乙酸降解。研究表明除了紫外亚硫酸盐体系可以产生水合电子外,有些有机物自身也能产生水合电(如吲哚,苯酚等),而目前关于这些的研究还极少。
发明内容
发明目的:针对现有技术中存在的不足,本发明的目的是提供一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,具有反应简单,降解效果好等优点。
技术方案:为了实现上述发明目的,本发明采用的技术方案为:
一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,在含有2,4,6-三溴酚的水中,加入亚硫酸钠,曝气除去溶解氧,控制溶液pH,进行紫外光照反应,实现降解2,4,6-三溴酚。
所述的亚硫酸钠的浓度为5~10mmol/L。
所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,用高纯氮气曝气,除去溶解氧。
所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,pH值为6~12,优选为6。
所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,光照2~20min,优选光照10min。
有益效果:与现有技术相比,本发明采用UV/Na2SO3光还原降解2,4,6-三溴酚,在三溴苯酚初始质量浓度100mg·L-1,三溴酚的降解率随紫外光解时间的增加而增加,2min~10min降解速率明显增加,至20min几乎完全降解。当SO3 2- 浓度为10mmol·L-1时,三溴苯酚的降解率明显提高,三溴酚在SO3 2-浓度为10mmol/L的UV/Na2SO3体系中,每个时间梯度pH=6时降解率呈稳定上升状态,在pH=6的条件下降解效果最佳。
附图说明
图1是不同光照时间紫外体系下对三溴苯酚的降解效果图;
图2是不同SO3 2-浓度对三溴酚降解效果的影响结果图;
图3是光照2min不同pH对降解率的影响结果图;
图4是光照3.5min pH对降解率的影响图;
图5是光照5min pH对降解率的影响结果图;
图6是光照7.5min pH对降解率的影响结果图;
图7是光照10min pH对降解率的影响图。
具体实施方式
下面结合具体实施例对本发明做进一步的说明。
以下实施例中,三溴苯酚测定采用高效液相色谱法,选取甲醇和蒸馏水作为流动相。色谱条件:甲醇 70%,水30%,流速1.0mL/min,进样量80μL,柱温25℃,检测波长290nm;溴离子测定采用PBr-1-01溴离子电极。
实施例1
一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,步骤如下:
1)称取100mg 2,4,6-三溴苯酚,放入烧杯中加蒸馏水以及适量氢氧化钠搅拌后放入KH-100E型超声波清洗器直到三溴苯酚完全溶解。
2)将溶解完全的三溴苯酚移液定容至1L容量瓶中,反应溶液用高纯氮气曝气8min以出溶解氧,避光保存。
3)分别取20mL三溴苯酚母液于石英试管中,放入2XF-LCA光催化反应器中光照0min、2min、5min、10min、20min、40min。
4)将光照后的溶液分别取样用高效液相色谱测定三溴苯酚的浓度并记录数据。
不同光照时间紫外体系下,对三溴苯酚的降解效果如图1所示,与无光照相比,2,4,6-三溴苯酚在紫外体系下降解效果有显著提高,光照2min降解效果不明显,2min~10min降解速率明显增加,光照20min几乎降解完全。
实施例2
一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,步骤如下:
(1)配置1mmol/L亚硫酸钠+100mg/L三溴苯酚溶液,用AE124型电子天平称取0.0126g亚硫酸钠,用三溴苯酚将其溶解并定容到100mL容量瓶中,实验前反应溶液用高纯氮气曝气2min以出溶解氧,避光保存。
(2)重复以上步骤,配置5mmol/L亚硫酸钠+100mg/L三溴苯酚溶液、10mmol/L亚硫酸钠+100mg/L三溴苯酚溶液、20mmol/L亚硫酸钠+100mg/L三溴苯酚溶液、40mmol/L亚硫酸钠+100mg/L三溴苯酚溶液。
(3)分别取20mL配置好的溶液于石英试管中,放入2XF-LCA光催化反应器中光照0min、2min、5min、10min、20min。
(4)将光照后的溶液分别取样用高效液相色谱测定三溴苯酚的浓度并记录数据。
在三溴苯酚初始质量浓度100mg·L-1,初始pH值10.0±0.2,考察SO3 2-浓度分别为1、5、10、20和40mmol·L-1时三溴苯酚的降解情况,结果如图2所示。由图2可知,随SO3 2-浓度的增加,三溴苯酚的降解率均有较大的提升,当SO3 2-浓度从1mmol·L-1提高至5mmol·L-1时,三溴苯酚的降解率相似,提高SO3 2-浓度至10mmol·L-1时,反应终点的三溴苯酚的降解率明显提高,进一步提高SO3 2-浓度至40mmol·L-1时,三溴苯酚的降解率明显降低。因此UV/Na2SO3光还原降解2,4,6-三溴酚,亚硫酸钠浓度优选采用10mmol/L。
实施例3
一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,步骤如下:
(1)称取100mg2,4,6-三溴苯酚,放入烧杯中加蒸馏水以及适量氢氧化钠搅拌后放入KH-100E型超声波清洗器直到三溴苯酚完全溶解定容至1L容量瓶中。
(2)用AE124型电子天平称取0. 1260g亚硫酸钠,放入烘干的烧杯中,加入配置好的100mg/L的三溴苯酚将其溶解,用三溴苯酚溶液定容到1L容量瓶中,反应溶液用高纯氮气曝气8min以出溶解氧,避光保存。
(3)取四个烘干的烧杯分别倒入10mmol/L亚硫酸钠+100mg/L三溴苯酚溶液用NaOH、HCl溶液调节pH值到6、8、10、12。
(4)将调节好pH值的溶液分别取20ml至石英试管中光照0min、2min、3.5min、5min、7.5min、10min。
(5)将光照后的溶液分别取样用高效液相色谱测定三溴苯酚的浓度并记录数据。
在2,4,6-三溴苯酚初始质量浓度100mg·L-1,SO3 2- 浓度为10 mmol·L-1,用氢氧化钠(1mol/L)或盐酸( 2.8 mol·L-1)调节溶液的pH值分别为6.0、8.0、10.0和12.0,三溴苯酚的降解情况如图3所示,在光照2min时,三溴苯酚在pH=6的降解效果最佳,降解率为19.04%,其次是pH=12的降解效果较好,pH=8和pH=10的降解效果不明显。
如图4所示,在光照3.5min时,三溴苯酚在pH=6、pH=10、pH=12的降解效果比较明显,其中pH=6的降解效果最佳,降解率为31.91%,pH=8的降解效果不明显。
图5所示,在光照5min时,三溴苯酚在pH=6、pH=8、pH=12的降解效果比较明显,其中pH=6的降解效果最佳,降解率为53.61%,pH=10的降解效果不明显。
如图6所示,在光照7.5min时,三溴苯酚在pH=6、pH=10的降解效果相似,pH=6的降解率是77.94%,pH=10的降解率是76.75%,pH=8的降解效果不明显。
如图7所示,在光照10min时,三溴苯酚在pH=6、pH=8、 pH=10的降解效果相似,都比较明显,pH=6的降解率是94.22%,pH=8的降解率是92.36%,pH=10的降解率是96.14%,pH=12降解效果不明显。
Claims (7)
1.一种采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,其特征在于,在含有2,4,6-三溴酚的水中,加入亚硫酸钠,曝气除去溶解氧,控制溶液pH,进行紫外光照反应,实现降解2,4,6-三溴酚。
2.根据权利要求1所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,其特征在于,所述的亚硫酸钠的浓度为5~10mmol/L。
3.根据权利要求1所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,其特征在于,用高纯氮气曝气,除去溶解氧。
4.根据权利要求1所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,其特征在于,pH值为6~12。
5.根据权利要求1所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,其特征在于,pH值为6。
6.根据权利要求1所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,其特征在于,光照2~20min。
7.根据权利要求1所述的采用UV/Na2SO3光还原降解2,4,6-三溴酚的方法,其特征在于,光照10min。
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