复合阴离子改性铁盐絮凝剂处理稠油石化污水研究
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摘要
稠油石化污水除具有一般稠油污水污染物含量高、成分复杂,可生化性差等特点外,还因在加工过程中添加了大量的化学助剂使得稠油石化污水中污染物更为稳定,难以去除,同时水质水量变化也较大。辽河流域稠油加工企业众多,稠油石化污水已成为辽河的重要污染源。为了处理稠油石化污水,石化企业建设了大量的污水处理工程,但是,随着地方环保法规的日益严格化,现有的污水处理设施难以满足环保要求,为此,寻找一条经济可行的稠油石化污水处理途径,尤其是对现有污水处理工艺进行强化使其达标,是稠油加工企业所面临的共同难题和急需解决的问题。
本文针对稠油石化原污水和生化处理后出水的水质特点,结合现有污水处理工艺与设施状况,采用新型聚合阳离子型絮凝剂,通过提高稠油石化污水生化前预处理效能与生化出水强化絮凝相结合的方法,解决了达标排放与处理成本高之间的矛盾。
絮凝剂效能是影响稠油石化污水处理效果的关键因素,因此,分析现有絮凝剂存在的不足并结合实际水质情况,通过复合阴离子改性共聚的方法,合成了一种以聚硅硫酸铁(PFSiS)为主的新型聚合硅磷硫酸铁(PFSiSp)絮凝剂,并通过模拟水样和实际稠油石化污水,对其合成条件、组分配比、特性等进行了研究。
经试验确定了聚硅酸(PS)合成条件:Si含量为0.5 mol·L-1,活化pH=4,合成温度为25℃;PFSiS合成条件为:初始Fe离子浓度为0.3 mol·L-1,碱化剂为NaHCO3,熟化温度控制在60℃,熟化时间为2h。采用不同碱化度(B值)和铁硅摩尔比(Fe/Si)的PFSiS对高岭土模拟水样除浊试验结果表明,当B值和Fe/Si在适宜的范围内PFSiS具有较好的絮凝性能,采用B=1.0,Fe/Si=5.0条件下合成的1.0PFSiS5.0在试验范围内具有最好的絮凝效果;稳定性试验表明,采用NaH2PO4为稳定剂,在Fe/P=10条件下,可使1.0PFSiS5.0稳定存放在60天以上,并可提高其絮凝性能,因此得到了优化配比的PFSiSp为:B=1.0,Fe/Si=5.0,Fe/P=10。
对实际稠油石化污水预处理试验表明,在适宜的投加量与pH范围内,PFSiSp对COD和油的去除率分别可达65%和96%以上,经处理后污水的B/C(BOD/COD)值可提高10%,表明PFSiSp对稠油石化污水中难降解有机物具有较好的去除效果;对生化出水强化絮凝试验表明,在投加量为120 mg·L-1,沉降时间为120 min的条件下,PFSiSp对生化出水的中COD去除率为50%,处理后污水达到了排放要求。
采用表面响应RSM试验方法研究了合成条件对PFSiSp中Fe(Ⅲ)水解/聚合产物组成的影响,建立了B值和Fe/Si与Fea、Feb和Fec含量关系的多元回归分析模型;在试验范围内模型预测值与实际测定值的误差小于5%;应用该模型可有效缩小合成条件的选择范围;PFSiSp絮凝剂的FTIR、XRD和SEM表征结果显示,Si参与了Fe(Ⅲ)水解/聚合反应并通过Fe—Si和Fe—O—Si与铁原子相连;PFSiSp中除含有少量种类的六角晶及斜方晶外,大多为无定形物;SEM试验结果表明,PFSiSp中物质主要为以两种结构的无定形物和多晶混生构成。
采用等离子体原子发射光谱法(ICP-AES),离子色谱法(IC)和气象色谱质谱联用法(GC-MS)对常减压蒸馏工艺、催化裂化工艺、焦化工艺和污水总入口的水质进行了分析,结果显示稠油石化污水中重金属含量低,磷元素缺乏,有机污染物以含碳在10个以上烷烃类、甲基苯酚类、小分子有机酸类和胺类为主;各点源均不同程度的含有多环芳烃类(PAHs)有机物,多为萘、蒽、菲、芘等及其衍生物。
现场对比试验表明,PFSiSp用于生化前预处理时,对稠油石化污水中油的去除率为92%;对COD的去除率为60%;对酚类的去除率为39.3%,其处理效果和处理稳定性均优于现场使用的单一聚合铁盐絮凝剂LHSH-1;对硫化物的去除率在85%与LHSH-1持平;PFSiSp用于生化出水强化絮凝处理时,COD的去除效果稳定,平均去除率为44.35%,经处理后污水COD含量在50 mg·L-1以下,达到了辽宁省地方排放标准;采用PFSiSp絮凝剂处理每吨污水的药剂成本为0.83元。
Beside the characteristics of general heavy oil wastewater, such as high concentration of pollutants, complex composition and relatively poor biochemical characteristics, Heavy Oil Petrochemical Wastewater (HOPW) is more complex and stable than heavy oil wastewater, due to using many chemicals additives in the refining process and fluctuation of quality and quantity. Because many heavy oil refineries located in the Liaohe River basin, HOPW has become important pollution sources of Liaohe River. To treat the HOPW, the refineries have built a large number of wastewater treatment facilities. However, as the local environmental laws and regulations stringent increasingly, the treatment effect of the facilities cannot meet the requirements of environmental protection. It has become a common problem for many petrochemical enterprises to find an economical and feasible way to treat the HOPW, especially to enhance the existing wastewater treatment process.
Based on the status of the HOPW treatment technology and the characteristics of raw water and biochemical treated water, a new kind of cationic polymer flocculants were synthesized to improve the efficiency of pre-processing and enhanced flocculation of the bio-treaded water and resolved the contradiction between the meeting the pollutant emission standards and the high cost of the HOPW treatment.
The efficiency of flocculants is key factor to effect HOWP treatment. Therefore, according to the shortcomings of the current flocculants and the water characteristics, new kinds of Poly Ferric Silicate Sulphate phosphate (PFSiSp) were synthesized by composite anions modified copolymerization method base on Poly Ferric Silicate Sulphate (PFSiS). Moreover, the synthesis factors, component ratios and application conditions properties of PFSiSp discussed by investigating the pollutants’removal efficiency of treating the simulated water and the actual HOPW samples.
The polysilicate (PS) synthesis conditions were determined by experiments as follows: Si concentration of 0.5 mol·L-1; activation pH of 4, synthesis temperature of 25℃. PFSiS synthesis conditions as follows: initial Fe ion concentration of 0.3 mol·L-1, NaHCO3 as alkalization agent, aging temperature at 60℃and aging time of 2h. Using the PFSiS to treat simulated wastewater and HOPW, at different basicities (B value) and Fe/Si molar ratios, the results showed that PFSiS had a good flocculation performance in appropriate scale of B value and Fe/Si. The 1.0PFSiS5.0 (B=1.0, Fe / Si=5.0) had the best performance in the all flocculants. The same conclusions were obtained in treating the actual HOPW. The 1.0PFSiS5.0 is the most effective to remove oil and COD than the others in the experimental scale. Experiment results of the 1.0PFSiS5.0 Stability indicated that it can storage stably more than 60 days when NaH2PO4 was used as the stabilizer and the Fe/P value of 10. Moreover, adding phosphate can improve the floccunlant efficiency. Finally, the optimal ratios of PFSiSp were selected as follows: B = 1.0, Fe/Si = 5.0, Fe/P = 10.
The pretreatment results of the actual HOPW exhibited that PFSiSp can remove 65% COD and 96% oil in the appropriate scale of dosages and suitable pH values conditions. The B/C (BOD/COD) value of the pretreated wastewater can be increased 10% than the raw wastewater. The change of B/C values indicated that PFSiSp can remove the nonbiodegradable COD efficiently. To optimize the application conditions, PFSiSp also was used as flocculant to decrease COD remaining in bio-treated HOPW by enhanced flocculation method. The results proved that nearly 50% COD can be removed under the dosage at 40 mg·L-1 and the setting time of 120 min conditions.
To study the impact of the synthesis conditions on the composition of Fe (Ⅲ) hydrolysis and polymerization products, RSM experiment method was adopted. Using the method, the multiple regression analysis models were established between the B value and Fe / Si corresponds to Fea, Feb and Fec respectively. In experiment scales, the errors between the models predicted values and the measured values less than 5%. Using the models can decrease the selecting range of synthesis conditions. Furthermore, PFSiS flocculants were characterized by FTIR, XRD and SEM methods. The results indicated that Si participate the Fe (Ⅲ) hydrolysis and polymerization processes and conjoin with Fe atoms through the Fe-Si and Fe-O-Si bonds. Besides a few of hexagonal and orthorhombic crystals, most of the substances in PFSiSp were amorphous materials. SEM results exhibited that main substance existing in PFSiSp is two kinds of amorphous materials and mixed crystals.
Using ICP-AES, IC, and GC-MS methods, the characteristics of HOPW were analyzed. The HOPW samples were collceted from the distillation, catalytic cracking, coking processes and the treatment plant’s inlet. The results showed that it is low heavy metals content, lack of phosphorus and the major organic pollutants are composited of alkanes, methyl phenols, small molecular organic acids and amines. Most of the alkanes contained more than ten carbon atoms. All the HOPW samples contain Polycyclic Aromatic Hydrocarbons (PAHs) in different degrees and the majority of PAHs are naphthalenes, anthracenes, phenanthrenes, pyrenes and their derivatives.
Field experiments results showed that more than 92% of oil, nearly 60% COD and 39.3% of phenols can be removed using the PFSiSp as flocculant in the pretreatment of the actual HOPW. All the PFSiSp performance and removal rates stability are superior to LHSH-1 flocculant, which is a single component polymer of iron salt and used in this field. On the aspect of removing sulfide, PFSiSp and LHSH-1 can remove about 85% of sulfide. During the field experiments of enhanced flocculation for bio-treated HOPW, PFSiSp can remove COD steadily and the average COD removal rate is 44.35%; The COD remains in supernatant less than 50 mg·L-1 and meet the local emission standards in Liaoning Province. The running cost of PFSiSp is 0.83 RMB·t -1.
本文针对稠油石化原污水和生化处理后出水的水质特点,结合现有污水处理工艺与设施状况,采用新型聚合阳离子型絮凝剂,通过提高稠油石化污水生化前预处理效能与生化出水强化絮凝相结合的方法,解决了达标排放与处理成本高之间的矛盾。
絮凝剂效能是影响稠油石化污水处理效果的关键因素,因此,分析现有絮凝剂存在的不足并结合实际水质情况,通过复合阴离子改性共聚的方法,合成了一种以聚硅硫酸铁(PFSiS)为主的新型聚合硅磷硫酸铁(PFSiSp)絮凝剂,并通过模拟水样和实际稠油石化污水,对其合成条件、组分配比、特性等进行了研究。
经试验确定了聚硅酸(PS)合成条件:Si含量为0.5 mol·L-1,活化pH=4,合成温度为25℃;PFSiS合成条件为:初始Fe离子浓度为0.3 mol·L-1,碱化剂为NaHCO3,熟化温度控制在60℃,熟化时间为2h。采用不同碱化度(B值)和铁硅摩尔比(Fe/Si)的PFSiS对高岭土模拟水样除浊试验结果表明,当B值和Fe/Si在适宜的范围内PFSiS具有较好的絮凝性能,采用B=1.0,Fe/Si=5.0条件下合成的1.0PFSiS5.0在试验范围内具有最好的絮凝效果;稳定性试验表明,采用NaH2PO4为稳定剂,在Fe/P=10条件下,可使1.0PFSiS5.0稳定存放在60天以上,并可提高其絮凝性能,因此得到了优化配比的PFSiSp为:B=1.0,Fe/Si=5.0,Fe/P=10。
对实际稠油石化污水预处理试验表明,在适宜的投加量与pH范围内,PFSiSp对COD和油的去除率分别可达65%和96%以上,经处理后污水的B/C(BOD/COD)值可提高10%,表明PFSiSp对稠油石化污水中难降解有机物具有较好的去除效果;对生化出水强化絮凝试验表明,在投加量为120 mg·L-1,沉降时间为120 min的条件下,PFSiSp对生化出水的中COD去除率为50%,处理后污水达到了排放要求。
采用表面响应RSM试验方法研究了合成条件对PFSiSp中Fe(Ⅲ)水解/聚合产物组成的影响,建立了B值和Fe/Si与Fea、Feb和Fec含量关系的多元回归分析模型;在试验范围内模型预测值与实际测定值的误差小于5%;应用该模型可有效缩小合成条件的选择范围;PFSiSp絮凝剂的FTIR、XRD和SEM表征结果显示,Si参与了Fe(Ⅲ)水解/聚合反应并通过Fe—Si和Fe—O—Si与铁原子相连;PFSiSp中除含有少量种类的六角晶及斜方晶外,大多为无定形物;SEM试验结果表明,PFSiSp中物质主要为以两种结构的无定形物和多晶混生构成。
采用等离子体原子发射光谱法(ICP-AES),离子色谱法(IC)和气象色谱质谱联用法(GC-MS)对常减压蒸馏工艺、催化裂化工艺、焦化工艺和污水总入口的水质进行了分析,结果显示稠油石化污水中重金属含量低,磷元素缺乏,有机污染物以含碳在10个以上烷烃类、甲基苯酚类、小分子有机酸类和胺类为主;各点源均不同程度的含有多环芳烃类(PAHs)有机物,多为萘、蒽、菲、芘等及其衍生物。
现场对比试验表明,PFSiSp用于生化前预处理时,对稠油石化污水中油的去除率为92%;对COD的去除率为60%;对酚类的去除率为39.3%,其处理效果和处理稳定性均优于现场使用的单一聚合铁盐絮凝剂LHSH-1;对硫化物的去除率在85%与LHSH-1持平;PFSiSp用于生化出水强化絮凝处理时,COD的去除效果稳定,平均去除率为44.35%,经处理后污水COD含量在50 mg·L-1以下,达到了辽宁省地方排放标准;采用PFSiSp絮凝剂处理每吨污水的药剂成本为0.83元。
Beside the characteristics of general heavy oil wastewater, such as high concentration of pollutants, complex composition and relatively poor biochemical characteristics, Heavy Oil Petrochemical Wastewater (HOPW) is more complex and stable than heavy oil wastewater, due to using many chemicals additives in the refining process and fluctuation of quality and quantity. Because many heavy oil refineries located in the Liaohe River basin, HOPW has become important pollution sources of Liaohe River. To treat the HOPW, the refineries have built a large number of wastewater treatment facilities. However, as the local environmental laws and regulations stringent increasingly, the treatment effect of the facilities cannot meet the requirements of environmental protection. It has become a common problem for many petrochemical enterprises to find an economical and feasible way to treat the HOPW, especially to enhance the existing wastewater treatment process.
Based on the status of the HOPW treatment technology and the characteristics of raw water and biochemical treated water, a new kind of cationic polymer flocculants were synthesized to improve the efficiency of pre-processing and enhanced flocculation of the bio-treaded water and resolved the contradiction between the meeting the pollutant emission standards and the high cost of the HOPW treatment.
The efficiency of flocculants is key factor to effect HOWP treatment. Therefore, according to the shortcomings of the current flocculants and the water characteristics, new kinds of Poly Ferric Silicate Sulphate phosphate (PFSiSp) were synthesized by composite anions modified copolymerization method base on Poly Ferric Silicate Sulphate (PFSiS). Moreover, the synthesis factors, component ratios and application conditions properties of PFSiSp discussed by investigating the pollutants’removal efficiency of treating the simulated water and the actual HOPW samples.
The polysilicate (PS) synthesis conditions were determined by experiments as follows: Si concentration of 0.5 mol·L-1; activation pH of 4, synthesis temperature of 25℃. PFSiS synthesis conditions as follows: initial Fe ion concentration of 0.3 mol·L-1, NaHCO3 as alkalization agent, aging temperature at 60℃and aging time of 2h. Using the PFSiS to treat simulated wastewater and HOPW, at different basicities (B value) and Fe/Si molar ratios, the results showed that PFSiS had a good flocculation performance in appropriate scale of B value and Fe/Si. The 1.0PFSiS5.0 (B=1.0, Fe / Si=5.0) had the best performance in the all flocculants. The same conclusions were obtained in treating the actual HOPW. The 1.0PFSiS5.0 is the most effective to remove oil and COD than the others in the experimental scale. Experiment results of the 1.0PFSiS5.0 Stability indicated that it can storage stably more than 60 days when NaH2PO4 was used as the stabilizer and the Fe/P value of 10. Moreover, adding phosphate can improve the floccunlant efficiency. Finally, the optimal ratios of PFSiSp were selected as follows: B = 1.0, Fe/Si = 5.0, Fe/P = 10.
The pretreatment results of the actual HOPW exhibited that PFSiSp can remove 65% COD and 96% oil in the appropriate scale of dosages and suitable pH values conditions. The B/C (BOD/COD) value of the pretreated wastewater can be increased 10% than the raw wastewater. The change of B/C values indicated that PFSiSp can remove the nonbiodegradable COD efficiently. To optimize the application conditions, PFSiSp also was used as flocculant to decrease COD remaining in bio-treated HOPW by enhanced flocculation method. The results proved that nearly 50% COD can be removed under the dosage at 40 mg·L-1 and the setting time of 120 min conditions.
To study the impact of the synthesis conditions on the composition of Fe (Ⅲ) hydrolysis and polymerization products, RSM experiment method was adopted. Using the method, the multiple regression analysis models were established between the B value and Fe / Si corresponds to Fea, Feb and Fec respectively. In experiment scales, the errors between the models predicted values and the measured values less than 5%. Using the models can decrease the selecting range of synthesis conditions. Furthermore, PFSiS flocculants were characterized by FTIR, XRD and SEM methods. The results indicated that Si participate the Fe (Ⅲ) hydrolysis and polymerization processes and conjoin with Fe atoms through the Fe-Si and Fe-O-Si bonds. Besides a few of hexagonal and orthorhombic crystals, most of the substances in PFSiSp were amorphous materials. SEM results exhibited that main substance existing in PFSiSp is two kinds of amorphous materials and mixed crystals.
Using ICP-AES, IC, and GC-MS methods, the characteristics of HOPW were analyzed. The HOPW samples were collceted from the distillation, catalytic cracking, coking processes and the treatment plant’s inlet. The results showed that it is low heavy metals content, lack of phosphorus and the major organic pollutants are composited of alkanes, methyl phenols, small molecular organic acids and amines. Most of the alkanes contained more than ten carbon atoms. All the HOPW samples contain Polycyclic Aromatic Hydrocarbons (PAHs) in different degrees and the majority of PAHs are naphthalenes, anthracenes, phenanthrenes, pyrenes and their derivatives.
Field experiments results showed that more than 92% of oil, nearly 60% COD and 39.3% of phenols can be removed using the PFSiSp as flocculant in the pretreatment of the actual HOPW. All the PFSiSp performance and removal rates stability are superior to LHSH-1 flocculant, which is a single component polymer of iron salt and used in this field. On the aspect of removing sulfide, PFSiSp and LHSH-1 can remove about 85% of sulfide. During the field experiments of enhanced flocculation for bio-treated HOPW, PFSiSp can remove COD steadily and the average COD removal rate is 44.35%; The COD remains in supernatant less than 50 mg·L-1 and meet the local emission standards in Liaoning Province. The running cost of PFSiSp is 0.83 RMB·t -1.
引文
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