印染污泥制备聚合硫酸铝混凝剂研究
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摘要
纺织印染业是一项污染较重的行业,其用水量大,排放污水量也很大。污水处理后产生大量污泥,由于缺乏有效处置,造成二次污染,导致我国印染污泥处理形势日益严峻。结合我国国情,开展印染污泥的处理、处置及资源化利用的应用基础研究,无疑十分必要。
本论文首先总结了印染污泥特点及国内外印染污泥资源化技术发展历史,在此基础上,选择了“酸化法+中和法”的组合工艺,尝试从印染污泥中回收铝并制备聚合硫酸铝,希望通过该研究探索出一种可行而又更加经济的从印染污泥中回收铝的方法。
本论文研究工作可以归纳成四个部分:(1)印染污泥特点分析;(2)酸浸法浸取焚烧后印染污泥中的铝;(3)中和法制备聚合硫酸铝;(4)聚合硫酸铝混凝性能研究。
本论文首先分析了印染污泥特点,探讨了酸浸法处理印染污泥焚烧残渣的最优浸出条件:主要考察了焚烧温度对印染污泥有机质和减重率的影响;考察了印染污泥焚烧前后性状、重金属含量,以及焚烧前后铝的形态;对酸种类、酸加入量、反应温度和时间以及反应液固比进行单因素实验,确定了最优浸出条件。实验结果表明:污泥焚烧残渣含有的金属元素主要包括铝、钙、铁、镁等,铝含量达248mg/g;焚烧的高温可以分解腐殖酸铝,铝以可被酸浸出的无机形式存在于污泥中;在四种常用酸的浸出实验中,磷酸对铝的浸出效果最差,硫酸、盐酸、硝酸的浸出效果相仿,但考虑到盐酸用量、挥发以及硝酸的高昂费用以及可能造成的污水处理装置富营养化问题,最终确定硫酸作为最佳浸出酸;在浓硫酸加入量0.92mL/g焚烧残渣,反应温度常温,反应时间3小时,液固比5mL/g的情况下,印染污泥焚烧残渣中铝元素的浸出率最大,达到96.7%。
然后,本论文研究了利用印染污泥焚烧残渣浸出液制备聚合硫酸铝的最优条件,主要考察了:碱化剂、加碱方式、加碱速度、原料配比、反应温度对制备得到的聚合硫酸铝中铝形态分布以及混凝效果的影响。结果表明:以氢氧化钙为碱化剂、正向方式缓慢滴加生成、氢氧化钙与硫酸铝物质的量比1.8∶1,85℃下反应制备的聚合硫酸铝Alb含量、盐基度较其他方式制备的聚合硫酸铝高,混凝性能也好;同时,得出柠檬酸是污泥浸出液制备聚合硫酸铝的最佳稳定剂,加入柠檬酸后,聚合硫酸铝稳定性较之前大大增强。
最后,本论文对比了本方法制备得到的聚合硫酸铝、商品聚合硫酸铝以及商品硫酸铝三种混凝剂对模拟印染废水以及实际印染废水的混凝效果,并研究了三种混凝剂的混凝实验后水样中铝残留问题。结果表明:这三种混凝剂的最佳pH值都在6.5～8.5之间;两种聚合硫酸铝均对实际废水有良好的处理效果,自制聚合硫酸铝处理效果比商品聚合硫酸铝稍逊;投加量从10mL/L增大至50mL/L时,残余铝含量均小于1mg/L,且使用自制和商品聚合硫酸铝的残余铝含量要小于商品硫酸铝混凝剂。
Textile industry has caused serious environmental pollution mainly because of its sewage. Dyeing sludge-by-product of wastewater treatment has been treated unsuccessfully,leading serious pollutions.The situation of the dealing of sludge is increasingly rigorous in China.So it is necessary to investigate applied research on how to deal with and recovery from dyeing sludge according to the Chinese situation.
In this paper,firstly the characteristics of dyeing sludge and the methods of its recycling at home and abroad were summarized.Based on the summarization of the recycling methods used by the predecessors,"the acid dissolution and neutralization method" combined process was chosen to prepare PAS from dyeing sludge.The objective of this research is to offer a more useful and economical process for Al recovery from dyeing sludge.
The frame of the paper is as follows:analysis of the component and content of metals in dyeing sludge,acid dissolution of Al from dyeing sludge,preparation of PAS by neutralization method,and the coagulant effect of PAS.
In first,the paper analysed the characters of dyeing sludge and discussed the optimal experiment conditions of acid dissolution of Al.The effect of temperature on organic matter and percentage of weight loss of dyeing sludge were emphatically observed.The component and content of metals,the forms of Al in the dyeing sludge before and after combustion were investigated.And single factor experiments under different kinds of acid,addition amount of acid, recation temperature,recation time and liquid-solid ratio were also conducted to find out the optimal conditions of acid dissolution of Al.The results indicated that the metals in the sludge are Al,Ca,Fe,Mg,etc.The amounts of Al are 157 and 248mg/g before and after combustion respectively.High temperature could decompose humic acid and transform Al into the form that could be leached by acid.In leaching experiments with four kinds of acid,leaching rate of Al kept similar level when HCl,HNO_3 and H_2SO_4 were used,and the rate of Al with H_3PO_4 was the lowest.But considering balance among addition amount and colatilization of HCl,and high cost and potential eutrophication caused by HNO_3,H_2SO_4 was chosen to conduct the experiment finally.The most optimized qualifications of acid leaching Al from dyeing sludge were elicited: the addition amount of H_2SO_4 0.92mL/g,the leaching time 3hr,the ratio of liquid to solid 5ml/g, leaching Al at normal temperature(25℃),Al leaching recovery can reach at 96.7%.
Secondly,the paper investigated the optimal condition of preparation of PAS in neutralization method.The effect of different kinds of basification agent,way of adding,Ca(OH)_2:Al_2(SO_4)_3 and temperature on the species distribution of Al in PAS and coagulation effect was studied.Alb%, basicity and coagulation effect were observed to be higher,when PAS was prepared by Ca(OH)_2, Ca(OH)_2:Al_2(SO_4)_3 was set 1.8:1,and its driping was positive and slow at 85℃.In addition,Citric acid was the best stabilizer for PAS prepared from leaching solution of sludge.By the addition of citric acid,PALS becomes more stabilized.
Thirdly,the paper compared the coagulation effect of PAS prepared in above mentioned way, PAS and AS purchased on simulative and practical dyeing wastewater.At last,the paper discussed the amount of residue of Al after coagulation.The results showed that the optimal pH was among 6.5～8.5.Compared with PAS prepared from dyeing sludge,PAS purchased shows higher coagulation effect.The amount of residue of Al was less than 1mg/L while addition amount of coagulation was increased from 10mL/L to 50ml/L,and theirs residue of Al was less than AS.
本论文首先总结了印染污泥特点及国内外印染污泥资源化技术发展历史,在此基础上,选择了“酸化法+中和法”的组合工艺,尝试从印染污泥中回收铝并制备聚合硫酸铝,希望通过该研究探索出一种可行而又更加经济的从印染污泥中回收铝的方法。
本论文研究工作可以归纳成四个部分:(1)印染污泥特点分析;(2)酸浸法浸取焚烧后印染污泥中的铝;(3)中和法制备聚合硫酸铝;(4)聚合硫酸铝混凝性能研究。
本论文首先分析了印染污泥特点,探讨了酸浸法处理印染污泥焚烧残渣的最优浸出条件:主要考察了焚烧温度对印染污泥有机质和减重率的影响;考察了印染污泥焚烧前后性状、重金属含量,以及焚烧前后铝的形态;对酸种类、酸加入量、反应温度和时间以及反应液固比进行单因素实验,确定了最优浸出条件。实验结果表明:污泥焚烧残渣含有的金属元素主要包括铝、钙、铁、镁等,铝含量达248mg/g;焚烧的高温可以分解腐殖酸铝,铝以可被酸浸出的无机形式存在于污泥中;在四种常用酸的浸出实验中,磷酸对铝的浸出效果最差,硫酸、盐酸、硝酸的浸出效果相仿,但考虑到盐酸用量、挥发以及硝酸的高昂费用以及可能造成的污水处理装置富营养化问题,最终确定硫酸作为最佳浸出酸;在浓硫酸加入量0.92mL/g焚烧残渣,反应温度常温,反应时间3小时,液固比5mL/g的情况下,印染污泥焚烧残渣中铝元素的浸出率最大,达到96.7%。
然后,本论文研究了利用印染污泥焚烧残渣浸出液制备聚合硫酸铝的最优条件,主要考察了:碱化剂、加碱方式、加碱速度、原料配比、反应温度对制备得到的聚合硫酸铝中铝形态分布以及混凝效果的影响。结果表明:以氢氧化钙为碱化剂、正向方式缓慢滴加生成、氢氧化钙与硫酸铝物质的量比1.8∶1,85℃下反应制备的聚合硫酸铝Alb含量、盐基度较其他方式制备的聚合硫酸铝高,混凝性能也好;同时,得出柠檬酸是污泥浸出液制备聚合硫酸铝的最佳稳定剂,加入柠檬酸后,聚合硫酸铝稳定性较之前大大增强。
最后,本论文对比了本方法制备得到的聚合硫酸铝、商品聚合硫酸铝以及商品硫酸铝三种混凝剂对模拟印染废水以及实际印染废水的混凝效果,并研究了三种混凝剂的混凝实验后水样中铝残留问题。结果表明:这三种混凝剂的最佳pH值都在6.5～8.5之间;两种聚合硫酸铝均对实际废水有良好的处理效果,自制聚合硫酸铝处理效果比商品聚合硫酸铝稍逊;投加量从10mL/L增大至50mL/L时,残余铝含量均小于1mg/L,且使用自制和商品聚合硫酸铝的残余铝含量要小于商品硫酸铝混凝剂。
Textile industry has caused serious environmental pollution mainly because of its sewage. Dyeing sludge-by-product of wastewater treatment has been treated unsuccessfully,leading serious pollutions.The situation of the dealing of sludge is increasingly rigorous in China.So it is necessary to investigate applied research on how to deal with and recovery from dyeing sludge according to the Chinese situation.
In this paper,firstly the characteristics of dyeing sludge and the methods of its recycling at home and abroad were summarized.Based on the summarization of the recycling methods used by the predecessors,"the acid dissolution and neutralization method" combined process was chosen to prepare PAS from dyeing sludge.The objective of this research is to offer a more useful and economical process for Al recovery from dyeing sludge.
The frame of the paper is as follows:analysis of the component and content of metals in dyeing sludge,acid dissolution of Al from dyeing sludge,preparation of PAS by neutralization method,and the coagulant effect of PAS.
In first,the paper analysed the characters of dyeing sludge and discussed the optimal experiment conditions of acid dissolution of Al.The effect of temperature on organic matter and percentage of weight loss of dyeing sludge were emphatically observed.The component and content of metals,the forms of Al in the dyeing sludge before and after combustion were investigated.And single factor experiments under different kinds of acid,addition amount of acid, recation temperature,recation time and liquid-solid ratio were also conducted to find out the optimal conditions of acid dissolution of Al.The results indicated that the metals in the sludge are Al,Ca,Fe,Mg,etc.The amounts of Al are 157 and 248mg/g before and after combustion respectively.High temperature could decompose humic acid and transform Al into the form that could be leached by acid.In leaching experiments with four kinds of acid,leaching rate of Al kept similar level when HCl,HNO_3 and H_2SO_4 were used,and the rate of Al with H_3PO_4 was the lowest.But considering balance among addition amount and colatilization of HCl,and high cost and potential eutrophication caused by HNO_3,H_2SO_4 was chosen to conduct the experiment finally.The most optimized qualifications of acid leaching Al from dyeing sludge were elicited: the addition amount of H_2SO_4 0.92mL/g,the leaching time 3hr,the ratio of liquid to solid 5ml/g, leaching Al at normal temperature(25℃),Al leaching recovery can reach at 96.7%.
Secondly,the paper investigated the optimal condition of preparation of PAS in neutralization method.The effect of different kinds of basification agent,way of adding,Ca(OH)_2:Al_2(SO_4)_3 and temperature on the species distribution of Al in PAS and coagulation effect was studied.Alb%, basicity and coagulation effect were observed to be higher,when PAS was prepared by Ca(OH)_2, Ca(OH)_2:Al_2(SO_4)_3 was set 1.8:1,and its driping was positive and slow at 85℃.In addition,Citric acid was the best stabilizer for PAS prepared from leaching solution of sludge.By the addition of citric acid,PALS becomes more stabilized.
Thirdly,the paper compared the coagulation effect of PAS prepared in above mentioned way, PAS and AS purchased on simulative and practical dyeing wastewater.At last,the paper discussed the amount of residue of Al after coagulation.The results showed that the optimal pH was among 6.5～8.5.Compared with PAS prepared from dyeing sludge,PAS purchased shows higher coagulation effect.The amount of residue of Al was less than 1mg/L while addition amount of coagulation was increased from 10mL/L to 50ml/L,and theirs residue of Al was less than AS.
引文
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