强化厌氧消化去除PhACs的特性研究

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摘要

污水污泥中存在的微量有机污染物如药理活性化合物 (Pharmaceutically active

compounds, PhACs) 给污水污泥的处理处置和资源利用带来了直接的环境危害或

潜在的环境风险。本文以检出频率高的消炎止痛药双氯芬酸、调节血脂的氯贝

酸、治疗癫痫的卡马西平和广谱抗菌剂三氯生为目标物，通过在建立有效的分离

纯化等预处理方法以及气相色谱-质谱 (GC-MS) 定量检测方法的基础上，研究其

在污水污泥厌氧消化中的行为特征，以及强化厌氧消化作用效能。

(1) 针对不同污泥停留时间 (Sludge retaining times, SRTs) 研究了污水污泥中

PhACs目标物在中、高温厌氧消化中的去除效果和特性。结果表明，SRTs的增大，一

定程度上有利于目标物的去除，特别是对于中温厌氧消化去除目标物的影响较明

显，高温厌氧消化当 SRT 15 d 以上时对目标物的去除变化不大。目标物在中、高

温厌氧消化中均有不同去除效果，尤其是三氯生，在两种温度条件下的去除率均

可达 74%，总体上，高温厌氧消化更有利于目标物的去除。厌氧消化过程中 NH3-N

的累积会影响目标物的去除，中温厌氧消化过程中其浓度在 75 mg/L 以下时，对目

标物的去除没有影响，而当浓度升高时，对目标物的去除有一定的抑制作用；高

温厌氧消化过程中，NH3-N 浓度在 85 mg/L 以下时，对目标物的去除没有影响，

高于此浓度时，则对目标物的去除产生一定的抑制。

(2) 利用超声对污水污泥强化预处理，以提高污泥絮体的解离，探讨超声强化

厌氧消化对 PhACs 的去除效果。采用前置超声和后置超声方式的强化预处理技

术，分别进行了中、高温厌氧消化 (SRT=15 d) 对照试验。超声联合高温厌氧消

化更有利于目标物的去除，尤其是对于较难去除的的卡马西平，其去除率增加

8%，达60%左右；氯贝酸去除率增长约 7%，达 67%；双氯芬酸去除率增长约 5%，达

68%；但三氯生的去除率并没有提高。

(3) 运用快速机械转盘强化对污泥絮体的预处理，探讨快速转盘联合厌氧消化

对PhACs 的去除。试验过程中采用前置转盘和后置转盘方式强化中、高温厌氧消

化工艺，SRT 设定为 15 d。厌氧消化联合后置快速转盘更有利于目标物的去除，双

氯芬酸的去除率增加约 8%，达 70%；氯贝酸去除率增加约 10%，达 70%；卡马西

平去除率增加约 12%，达 64%；但对三氯生的去除率几乎无影响。

本文的研究成果，可与污水污泥其他指标、课题研究成果相结合，对完善污

水污泥基础数据及有毒有害污染物的控制有一定的参考价值。

关键词：污泥停留时间固相萃取去除效果超声快速机械转盘

ABSTRACT

Micropollutants present in the sewage sludge like PhACs (pharmaceutically

active compounds) could exert directly environmental harms or potentially

environmental risks in the course of disposal and resource utilization of sewage sludge.

Four pharmaceuticals, i.e. anti-inflammatory painkiller diclofenac, lipid regulating

agent clofibric acid, epilepsy drugs carbamazepine, and broad-spectrum antibacterial

agent triclosan, which were frequently detected in the sewage sludge, were selected as

the target compounds in this study. Effective isolation and purification pre-treatment

to extract the target compounds were firstly established, followed by identification

and quantification of them using gas chromatography-mass spectrometry (GC/MS).

The objectives of this study were to investigate the behavior of target compounds

during the anaerobic digestion (AD) of sewage sludge and focus on their removal

characteristics using enhanced anaerobic digestion processes (EAD). The main results

obtained were as follows.

(1) The behavior and variations of PhACs during the AD of sewage sludge under

the mesophilic and thermophilic conditions with different sludge retaining times

(SRTs) were primarily investigated. The removal efficiencies of the target compounds

could be raised to a certain extent with the increase on SRTs, especially under the

mesophilic condition. The removal of target compounds under thermophilic condition

hardly varied when the SRTs were above 15 d. All the compounds could be partly

removed from the sewage sludge under the two temperature conditions, particularly

the triclosan which was obtained about 74% of removal. On the whole, it seemed that

the thermophilic condition was more conducive to their removal. The accumulation of

ammonia nitrogen in the AD process also affected the removal of the targets. When its

concentrations under the mesophilic condition were below 75 mg/L, little effects on

the removal were observed, and beyond the concentrations the inhibition to the

removal would took place. In the case of the thermophilic condition, there were no

effects on the removal below 85 mg/L of ammonia nitrogen, and some inhibitions to

the removal were found above the concentration.

(2) The EAD processes of AD combined with sonication were developed to

investigate the removal of the PhACs, where the ultrasonic treatment was used as the

pretreatment to enhance the dissociation of the flocs, and then expected to improve the

removal of the compounds. The ultrasonic units were settled before or after the

anaerobic digestion reactors which were operated under the mesophilic and

thermophilic conditions individually. SRT was set to 15 d. It could be seen that the

EAD processes were generally conductive to the removal of the targets, especially

under the thermophilic condition. Particularly, the removal efficiency of the

carbamazepine which is considered as very difficult to be removed reached about 60%

with 8% up, the clofibric acid’s was up to 67% with 7% up, and the diclofenac’s was

about 68% with 5% up, however, the removal of the triclosan was not raised at all.

(3) The EAD processes of AD combined with high-speed mechanical rotary discs

were designed and adopted to study the removal of the PhACs, where the rotary discs

were applied to break the sludge flocs. Similarly to the former EAD, the discs were

settled before or after the mesophilic and thermophilic anaerobic digestion reactors.

SRT was set to 15 d. It was found that the AD with the rear discs was more

conductive to the removal of the targets. The removal efficiency of the clofibric acid

reached about 70% with 7% up, the clofibric acid’s was up to 70% with 10% up, and

the carbamazepine was about 64% with 12% up, notwithstanding, the removal of the

triclosan was not perceivably raised.

The results achieved in this study could be combined with some research

achievements obtained from other sludge indicators and relevant projects, and

therefore to perfect the basic data of sewage sludge and present a technical support on

the sludge-related toxic pollutant management.

Key Word: sludge retaining time, solid-phase extraction, removal effect,

sonication, high-speed mechanical rotary disc

中文摘要

ABSTRACT

第一章绪论 .................................................................................................................. 1

1.1 课题来源 ............................................................................................................ 1

1.2 研究背景 ............................................................................................................ 2

1.2.1 城市污水污泥的处理 .............................................................................. 2

1.2.2 PhACs 的研究现状 ................................................................................... 7

1.2.3 厌氧污泥中的 PhACs 的研究现状 ....................................................... 12

1.3 研究意义与内容 .............................................................................................. 13

第二章试验内容和方法 .............................................................................................. 15

2.1 试验试剂与仪器 .............................................................................................. 15

2.1.1 试验药剂 ................................................................................................ 15

2.1.2 试验仪器 ................................................................................................ 16

2.1.3 标准溶液的配制 .................................................................................... 17

2.2 样品的制备 ...................................................................................................... 17

2.2.1 污泥的采集与保存 ................................................................................ 17

2.2.2 样品的预处理方法 ................................................................................ 18

2.2.3 样品的检测方法 .................................................................................... 22

2.3 试验装置 .......................................................................................................... 25

2.3.1 厌氧消化装置 ........................................................................................ 25

2.3.2 快速转盘装置 ........................................................................................ 25

2.4 常规指标检测 .................................................................................................. 26

2.5 目标物检测 ...................................................................................................... 26

2.5.1 目标物 .................................................................................................... 26

2.5.2 标准溶液的配制 .................................................................................... 27

2.5.3 目标物定性 ............................................................................................ 28

第三章厌氧消化中 PhACs 的变化规律 ..................................................................... 30

3.1 试验方案 .......................................................................................................... 30

3.2 中温厌氧消化 .................................................................................................. 30

3.2.1 污泥停留时间对常规指标的影响 ........................................................ 31

3.2.2 污泥停留时间对目标物去除的影响 .................................................... 31

3.2.3 NH3-N 对目标物去除的影响 ................................................................. 33

3.3 高温厌氧消化 .................................................................................................. 35

3.3.1 污泥停留时间对常规指标去除的影响 ................................................ 35

3.3.2 不同污泥停留时间对目标物去除的影响 ............................................ 36

3.3.3 NH3-N 对目标物去除的影响 ................................................................. 37

3.4 本章小结 .......................................................................................................... 39

第四章强化厌氧消化对 PhACs 的处理效果 ............................................................. 40

4.1 试验方法 .......................................................................................................... 40

4.2 超声联合厌氧消化对 PhACs 的去除 ............................................................. 41

4.2.1 前置超声下厌氧消化对目标物的去除 ................................................ 41

4.2.2 厌氧后超声处理回流对目标物的去除 ................................................ 44

4.2.3 对比分析 ................................................................................................ 45

4.3 快速转盘预处理联合厌氧消化对 PhACs 的去除 ......................................... 45

4.3.1 前置转盘联合厌氧消化对目标物的去除 ............................................ 46

4.3.2 后置转盘联合厌氧消化对目标物的去除 ............................................ 48

4.3.3 对比分析 ................................................................................................ 50

4.4 本章小结 .......................................................................................................... 50

第五章结论及建议 ...................................................................................................... 52

5.1 结论 .................................................................................................................. 52

5.2 建议与展望 ...................................................................................................... 53

参考文献 ........................................................................................................................ 54

在读期间公开发表论文和承担科研项目及取得成果 ................................................ 60

致谢 ................................................................................................................................ 61

第一章绪论

1.1 课题来源

污水污泥是目前全球性数量大、含水率高、污染物含量高、处理难度大的一

类固体垃圾。近年来，随着污水处理量的增加和污水处理率的提高，污泥产量有

很大的增长。据统计，2007 年污水处理厂共处理污水量为 178,012 万吨，其中生

活污水为 114,185 万吨，工业废水为 63,827 万吨，产生污泥量为 732,777 吨，平均

每天产生 2007 吨 (湿泥)[1]。根据上海市规划，到 2020 年期末，污水处理设施总

体规模将达到 1.12×107 m3/d，全市范围内规划建成 64 座污水处理厂，同时预测到

2020 年上海市污水处理厂产生的污泥量将为 6986-8383 m3/d [2]。据估算，我国目

前的城市污水处理厂年排放污泥 (干重) 约为 300 万吨，且年增长率大于 10%，特

别是在我国城市化水平较高的几个城市与地区，污泥出路问题已经十分突出。污

泥的处理处置已成为环境综合治理工作中的新难点、新挑战。

污水污泥的土地填埋、土地利用 (包括农田利用、园林绿化、填埋厂覆土等)

和堆肥仍是当前主要的污泥处理处置和资源化利用方式。据估算，到 2010 年，美

国土地利用的污水污泥达 8,200,000 万吨，占总污泥产量的 45%，另有 17%的污水

污泥进行土地填埋，约 5%的污水污泥用于堆肥[3]。此外，由于污水污泥中有机成

分含量非常高，利用污水污泥通过生物转化，生产高附加值产品[4] (VAPs，如生物

杀虫剂，工业用酶、生物聚合物等) 也是污水污泥资源化利用的新方向。

然而，由于污水污泥成分非常复杂，含量病原微生物、重金属、有机污染物

等，若不进行有效的处理，会使污水污泥的土地填埋和资源化利用带来直接的环

境危害或潜在的环境安全风险。关于污水污泥中病原微生物、重金属、多环芳香

烃 (PAHs) 、多氯联苯 (PCBs) 及毒性评价，国内外已有相当多的文献进行了研究

和报道[5-8]。但是对于一类新型的有机污染物—药品类有机污染在污水污泥中的分

布及可能的环境风险则未引起足够关注。基于污水污泥利用的日益增加以及相关

有机污染物数据的匮乏，2002 年，美国国家研究理事会 (NRC) 发布了有关污水

污泥 (生物固体) 的报告。NRC 建议有必要对污水污泥中药品和个人护理用品

(Pharmaceutical and personal care products, PPCPs) 的存在和迁移转化等进行研

究。在该报告中，NRC 特别指出虽然目前没有研究污水污泥中 PPCPs，但是其极

有可能存在于污水污泥中，需要对污水污泥的利用进行新的风险评价，并增加评

价的物质种类。

1999 年在美国环境保护总署 (EPA) 支持下，Daughton 和Ternes[9]发表了关于

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摘要：

摘要污水污泥中存在的微量有机污染物如药理活性化合物(Pharmaceuticallyactivecompounds,PhACs)给污水污泥的处理处置和资源利用带来了直接的环境危害或潜在的环境风险。本文以检出频率高的消炎止痛药双氯芬酸、调节血脂的氯贝酸、治疗癫痫的卡马西平和广谱抗菌剂三氯生为目标物，通过在建立有效的分离纯化等预处理方法以及气相色谱-质谱(GC-MS)定量检测方法的基础上，研究其在污水污泥厌氧消化中的行为特征，以及强化厌氧消化作用效能。(1)针对不同污泥停留时间(Sludgeretainingtimes,SRTs)研究了污水污泥中PhACs目标物在中、高温厌氧消化中的去除效果和特性...

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