直接氧化法制备改性聚合硫酸铁脱色剂的工艺及应用研究
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摘要
印染废水的治理，特别是印染废水脱色，是一个具有重大实用价值的研究课题。本文在阐述印染废水的来源、特征及国内外各种印染废水处理方法的基础上。完整地论述了在添加改性剂-乙酸，通过氯酸钠直接氧化法制备改性聚合硫酸铁脱色剂的合成反应的工艺条件，并对合成工艺条件进行了优化，还就改性聚合硫酸铁脱色剂在印染废水中的应用进行了研究。结果表明：实验室制备的产品具有优良的絮凝脱色性能，并且制备工艺简单，易于控制。本论文为印染废水的絮凝沉降处理方法提供了一种新型的性能优良的脱色剂，具体内容有：
(1)采用七水硫酸亚铁、硫酸、氯酸钠等原料，通过氧化、水解、聚合反应，制备了改性聚合硫酸铁脱色剂。实验证明在反应体系中添加适量的改性剂-乙酸，可以起到缓冲反应液的pH值，有助于提高产品的盐基度。
(2)对产品的盐基度含量和总铁含量进行了测定，结果表明：实验室制备的产品是一种盐基度含量比较高的液体产品，在水溶液中呈现阳离子聚电解质的特性，产品的物理性质良好，三个月内无沉淀，与水可以以任何比例混合，适合于在废水处理中的应用。
(3)参照COD的标准测定法及相关资料，通过多次试验，并参照标准曲线，建立了印染废水中COD快速测定的工作曲线。后续实验中COD的测定照此方法进行，这样不但节约了大量试剂，提高了工作效率，而且减轻了对环境的污染。
(4)本论文考察了硫酸用量、乙酸用量、氯酸钠用量、反应时间等因素对产品性能的影响及变化规律。在对上述因素的单因素初选的基础上，进行正交设计试验，并以对模拟染料废水的脱色率及COD_(Cr)去除效果为评价指标，确定了最优的合成工艺条件：七水硫酸亚铁用量15.66g，硫酸用量0.7mL，氯酸钠用量1.2g，乙酸用量0.3mL，反应时间为20min。由实验可以知道：在制备过程中，硫酸用量对产品性能影响最大。
(5)在最佳合成工艺条件下制得了实验产品，并将它应用于模拟染料废水的处理，分别考察了改性聚合硫酸铁脱色剂对分散染料、酸性染料和活性染料废水的脱色效果和COD_(Cr)去除情况，并与普通聚合硫酸铁作了比较，由此体现出实验产
品优良的絮凝脱色性能，并研究了它在上述染料废水处理中的应用规律。
(6)进行了改性聚合硫酸铁脱色剂对实际印染废水处理的可行性试验研究。实
验分别考察了药剂投加量、废水的pH值以及与助凝剂配合使用等工艺条件对絮凝
脱色效果的影响。实验结果表明:废水出水中含有的CODcr值己经低于国家一级
排放标准，色度接近无色，由此可知本实验产品是一种高效的脱色剂。
Treating the printing and dyeing wastewater, especially decoloring, is an important task with practical value. On the basis of surveying the resource, characteristic and treatment approaches inside and outside of the country of printing and dyeing wastewater, reaction which natrium chlorate oxidates directly with acetic acid to synthesize modified polymerized ferric sulphate decoloring agent is studied systematically in this paper .The synthetic condition is optimized and the application performance of modified polymerized ferric sulphate decoloring agent on printing and dyeing wastewater is also studied. Results show the excellent performance of decolourization and flocculation and operation is simple, convenient and controlled easily. It provides a new-type decoloring agent with high efficiency applying in printing and dyeing wastewater treatment. The main contents of experiment as following:
(1) Modified polymerized ferric sulphate decoloring agent is made through oxidation, hydrolyzation, polymerization with ferrous sulphate heptahydrate, sulphate acid, natrium chlorate etc. Experiment shows appropriate acetic acid is feasible to adjust pH value of reactive solution and can improve alkalinity degree of the product.
(2) By the measurement of content of alkalinity degree and total iron, the product is indicated to be a kind of liquid with high alkalinity degree. The product shows the characteristic of electrolytical and is adapt to applying in wastewater treatment with fine physical property. It is without deposition in three months and mixed with water by unlimited scale.
(3) The curve of work in rapid determination of COD of printing and dyeing is settled through lots of expemiments, referencing normal curve and data involved. It is applied to following experiments in determination of COD of wastewater.
(4) It researchs effect and variational rule of the factors including the dosage of sulphate acid, the dosage of acetic acid, the dosage of natrium chlorate, reactive time, etc. Orthogonal experiment is arranged on the basis of selection of the range of experiment condition. The optimum symthetic condition is determined by the evaluation criterion of the removal of CODCr and decolourization. The optimization is
to be: the dosage of sulphate acid:0.7mL; the dosage of natrium chlorate: 1.2g; the dosage of acetic acid:0.3mL; reaction time:20 minutes. Experiments show the dosage of sulphate acid is the most important factor on property of the product.
(5) The performance of the removal of CODcr and decolourization of modified polymerized ferric sulphate decoloring agent prepared in the optimum condition applying in disperse, acid and reactive dye-containing wastewater treatment are researched, comparing with ordinary polymerized ferric sulphate. Results show it is more excellent than ordinary polymerized ferric sulphate in flocculation and decolourization. The application rule in dyeing and printing wastewater is studied.
(6) The feasibility of modified polymerized ferric sulphate decoloring agent applying in practical printing and dyeing wastewater is also studied. The rules influenced by technologic conditions such as dosage, pH value of wastewater and the use of assistant flocculant are studied respectively through experiments. The result of treatment shows: discharging water of content in CODcr under discharge of national standard and decoloured almost. The product is a kind of high effective decoloring agent and applied to printing and dyeing wastewater with the best effect of treatment.
(1)采用七水硫酸亚铁、硫酸、氯酸钠等原料，通过氧化、水解、聚合反应，制备了改性聚合硫酸铁脱色剂。实验证明在反应体系中添加适量的改性剂-乙酸，可以起到缓冲反应液的pH值，有助于提高产品的盐基度。
(2)对产品的盐基度含量和总铁含量进行了测定，结果表明：实验室制备的产品是一种盐基度含量比较高的液体产品，在水溶液中呈现阳离子聚电解质的特性，产品的物理性质良好，三个月内无沉淀，与水可以以任何比例混合，适合于在废水处理中的应用。
(3)参照COD的标准测定法及相关资料，通过多次试验，并参照标准曲线，建立了印染废水中COD快速测定的工作曲线。后续实验中COD的测定照此方法进行，这样不但节约了大量试剂，提高了工作效率，而且减轻了对环境的污染。
(4)本论文考察了硫酸用量、乙酸用量、氯酸钠用量、反应时间等因素对产品性能的影响及变化规律。在对上述因素的单因素初选的基础上，进行正交设计试验，并以对模拟染料废水的脱色率及COD_(Cr)去除效果为评价指标，确定了最优的合成工艺条件：七水硫酸亚铁用量15.66g，硫酸用量0.7mL，氯酸钠用量1.2g，乙酸用量0.3mL，反应时间为20min。由实验可以知道：在制备过程中，硫酸用量对产品性能影响最大。
(5)在最佳合成工艺条件下制得了实验产品，并将它应用于模拟染料废水的处理，分别考察了改性聚合硫酸铁脱色剂对分散染料、酸性染料和活性染料废水的脱色效果和COD_(Cr)去除情况，并与普通聚合硫酸铁作了比较，由此体现出实验产
品优良的絮凝脱色性能，并研究了它在上述染料废水处理中的应用规律。
(6)进行了改性聚合硫酸铁脱色剂对实际印染废水处理的可行性试验研究。实
验分别考察了药剂投加量、废水的pH值以及与助凝剂配合使用等工艺条件对絮凝
脱色效果的影响。实验结果表明:废水出水中含有的CODcr值己经低于国家一级
排放标准，色度接近无色，由此可知本实验产品是一种高效的脱色剂。
Treating the printing and dyeing wastewater, especially decoloring, is an important task with practical value. On the basis of surveying the resource, characteristic and treatment approaches inside and outside of the country of printing and dyeing wastewater, reaction which natrium chlorate oxidates directly with acetic acid to synthesize modified polymerized ferric sulphate decoloring agent is studied systematically in this paper .The synthetic condition is optimized and the application performance of modified polymerized ferric sulphate decoloring agent on printing and dyeing wastewater is also studied. Results show the excellent performance of decolourization and flocculation and operation is simple, convenient and controlled easily. It provides a new-type decoloring agent with high efficiency applying in printing and dyeing wastewater treatment. The main contents of experiment as following:
(1) Modified polymerized ferric sulphate decoloring agent is made through oxidation, hydrolyzation, polymerization with ferrous sulphate heptahydrate, sulphate acid, natrium chlorate etc. Experiment shows appropriate acetic acid is feasible to adjust pH value of reactive solution and can improve alkalinity degree of the product.
(2) By the measurement of content of alkalinity degree and total iron, the product is indicated to be a kind of liquid with high alkalinity degree. The product shows the characteristic of electrolytical and is adapt to applying in wastewater treatment with fine physical property. It is without deposition in three months and mixed with water by unlimited scale.
(3) The curve of work in rapid determination of COD of printing and dyeing is settled through lots of expemiments, referencing normal curve and data involved. It is applied to following experiments in determination of COD of wastewater.
(4) It researchs effect and variational rule of the factors including the dosage of sulphate acid, the dosage of acetic acid, the dosage of natrium chlorate, reactive time, etc. Orthogonal experiment is arranged on the basis of selection of the range of experiment condition. The optimum symthetic condition is determined by the evaluation criterion of the removal of CODCr and decolourization. The optimization is
to be: the dosage of sulphate acid:0.7mL; the dosage of natrium chlorate: 1.2g; the dosage of acetic acid:0.3mL; reaction time:20 minutes. Experiments show the dosage of sulphate acid is the most important factor on property of the product.
(5) The performance of the removal of CODcr and decolourization of modified polymerized ferric sulphate decoloring agent prepared in the optimum condition applying in disperse, acid and reactive dye-containing wastewater treatment are researched, comparing with ordinary polymerized ferric sulphate. Results show it is more excellent than ordinary polymerized ferric sulphate in flocculation and decolourization. The application rule in dyeing and printing wastewater is studied.
(6) The feasibility of modified polymerized ferric sulphate decoloring agent applying in practical printing and dyeing wastewater is also studied. The rules influenced by technologic conditions such as dosage, pH value of wastewater and the use of assistant flocculant are studied respectively through experiments. The result of treatment shows: discharging water of content in CODcr under discharge of national standard and decoloured almost. The product is a kind of high effective decoloring agent and applied to printing and dyeing wastewater with the best effect of treatment.
引文
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