6-硝生产废水的治理技术研究
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摘要
6-硝基-1,2重氮氧基萘-4-磺酸(6-硝),是制造酸性媒介染料的中间体。6-硝废水是6-硝生产过程产生的废水,包括1,2,4-酸和1,2,4-酸氧体两种废水,两种废水的COD、pH值相近,去除难度差异不大,在废水处理时可将2种废水混合后加以处理。本文以1,2,4-酸废水为研究对象,该废水有机物含量高、毒性大、色度高,难以采用生物法处理。
本课题采用以下几种方法研究1,2,4-酸废水治理:(1)三辛胺-正辛醇-煤油络合萃取体系处理1,2,4-酸母液废水(2)有机膨润土处理1,2,4-酸母液废水(3)铁/炭微电解-Fenton氧化技术处理1,2,4-酸生产废水(4)絮凝-络合萃取处理1,2,4-酸废水(5)絮凝-吸附处理1,2,4-酸废水研究。研究结果表明:
三辛胺-正辛醇-煤油络合萃取体系处理1,2,4-酸母液废水:萃取的最佳工艺参数为:三辛胺与正辛醇、煤油的体积比为4:1:5。废水pH值为1.7,萃取相比O/A为1:5。反萃的最佳工艺参数为:NaOH质量分数为15%,反萃体系相比为2:1,反萃温度为40oC恒温搅拌60min,静置6h分相,反萃效率为84%。
膨润土有机化改性及其在6-硝生产废水治理中的应用:该部分研究了三种有机膨润土体系:CTMAB改性膨润土(阳离子表面活性剂体系)、三辛胺改性膨润土(有机胺体系)、阳离子淀粉改性膨润土(有机高分子体系),通过比较,得出以下结论:制备的难易程度为:阳离子表面活性剂体系>有机胺体系>有机高分子体系;制备的有机膨润土对1,2,4-酸废水的吸附能力依次为:阳离子表面活性剂体系(COD去除率75%)>有机胺体系(COD去除率68%)>有机高分子体系(COD去除率35%);相应的1m~3废水处理成本为:9.5元、65.7元、11元。表面活性剂作为有机改性剂或者辅助改性剂,相应制得的有机膨润土吸附性能大小依次为:阳离子型表面活性剂>非离子型表面活性剂>阴离子型表面活性剂。
铁/炭微电解-Fenton氧化技术处理1,2,4-酸生产废水:其工艺参数为: 1,2,4-酸母液废水调节pH值=1,活性炭用量1%,Fe/C=3:1,在常温,微电解反应3h;将微电解后的滤液调pH值=3,加入H_2O_22.5%进行1h的Fenton反应。
絮凝-络合萃取处理1,2,4-酸废水研究:以自制的双氰胺-甲醛絮凝剂絮凝处理1,2,4-酸母液废水,主要参数为:废水pH值=3,絮凝剂用量为1%,在70℃下快速搅拌2min,慢搅10min,再静置40min。三辛胺-正辛醇组成的萃取体系主要参数为:pH值=1.5、相比为1:6、萃取剂浓度为40%,常温下振荡两分钟,静置分层15min。采用NaOH溶液作反萃取剂,反萃取过程的主要参数为:NaOH浓度为15%,相比(B/O)=1:2,反应温度为40℃。
絮凝-吸附处理1,2,4-酸废水研究:在絮凝实验中,采用自制双氰胺-甲醛絮凝剂絮凝,当废水pH值=3,絮凝剂用量为1%。在吸附实验中,用自制的AEO-9插层改性制得的有机膨润土进行吸附,吸附工艺条件为:pH值为8,吸附时间30min,吸附剂用量为5%。先絮凝后吸附较先吸附后絮凝效果更好。
技术经济指标比较:从技术上看,处理效果依次为:絮凝-络合萃取工艺(COD降至50 mg/L)>絮凝-吸附工艺(COD降至253 mg/L) >铁炭微电解-Fenton氧化工艺(COD降至860 mg/L) >三辛胺-正辛醇-煤油络合萃取工艺(COD降至1840 mg/L) >CTMAB改性膨润土吸附工艺(COD降至4300 mg/L);经济上看,处理成本依次为:铁炭微电解-Fenton氧化工艺(处理费用5.4元/ m~3)< CTMAB改性膨润土吸附工艺(处理费用9.5元/ m~3) <絮凝-吸附工艺(处理费用25元/ m~3) <三辛胺-正辛醇-煤油络合萃取工艺(处理费用55.8元/ m~3) <絮凝-络合萃取工艺(处理费用114.2元/ m~3)。
处理6-硝生产废水的技术经济要求为COD降至2000 mg/L以下,处理费用降至低于50元/ m~3,因此絮凝-吸附工艺(优先考虑技术因素时可选)、铁炭微电解-Fenton氧化工艺可满足要求(优先考虑经济因素时可选)。
6-Nitro-1,2-azoxynaphthalene-4-sulfonic acid(i.e.6-Nitry) is an intermediate for producing acid medium dye. 6-nitry wastewater which comes from 6-nitry producttion, and the wastewater comprises two kinds of wastewater, 1,2,4-acid wastewater and 1,2-Naphthoxydiazole-4-sulfonic acid wastewater. COD, pH value, and treatment difficulty of the two kinds of wastewater are very similar . So the two kinds of wastewater can be mixed before wastewater treatment. This theses mainly studied on the treatment processes of 1,2,4-acid wastewater,and the wastewater composes of high concentration organics, has high toxicity and is difficult to be biochemical treated.
This topic took the following methods to treat1,2,4-acid wastewater: (1) TOA-Octanol- Kerosene complex extraction process (2) organic bentonite adsorption process (3) Ferric-Carbon microelectrolysis combined with Fenton oxidation process (4) Flocculation Combined with complex extraction process (5) Flocculation combined with adsorption process.The experiment results indicated that:
TOA-Octanol-Kerosene complex extraction process:under the optimum conditions that TOA:Octanol:Kerosene of 4:1:5, Wastewater pH value of 1.7, O/A of 1:5; the optimum parameters of back extraction are follow: NaOH concentration of 15%, phase volume ratio O/B of 2:1, and temperature of 40℃, stirred for 60min and standing for 6h to separate phase, the back extraction efficiency can reach for is 84%.
In organic modification of bentonite and its application in 6-nitrate wastewater treatment, three kinds of organic bentonite system were studied: CTMAB modified bentonite (cationic surfactant system), TOA modified bentonite (organic amine system), cationic starch modification bentonite (organic polymer system),by comparison, we got the following conclusions: the difficulty level of the three system from easy to difficult: cationic surfactant system > organic amine system>organic polymer system; the adsorption ability of organic bentonite: the cationic surfactant system (COD removal rate 75%) > organic amine system (COD removal rate 68%) > organic polymer system (COD removal rate 35%); The cost of 1m~3 wastewater treatment is RMB9.5, RMB65.7, RMB11 respectively. surfactants are as organic modifier or assist modifier, the corresponding adsorption ability of the organic bentonite is as follow: cationic surfactant > nonionic surfactant > anionic surfactant.
In Ferric-Carbon microelectrolysis combined with fenton oxidation process, the optimum experiment conditions are as follows: adjusted wastewater pH value to 1, added activated carbon dosage of 1%, Fe/C = 3:1,microelectrolysis reacted for 3h at room temperature; adjusted the filtrate pH value to 3, added H_2O_2 for 2.5% dosage, then Fenton reaction for 1h.
Flocculation combined with complexation extraction process:self-made dicyandiamide-formaldehyde polymer as flocculant, the main parameters are : adjusted wastewater pH value to 3, added flocculant of 1%, rapidly stirring at 70℃for 2 min, slow stirring for 10min, and then standing for 40min; TOA-Octanol extraction system at the following parameters: pH value is 1.5, phase ratio is 1:6, 40% extractants concentration , extracted at room temperature for two minutes, let it stand to layer for 15min. NaOH solution as back extractant, the main parameters of back extractant are:NaOH concentration is for 15%, phase ratio (B/O) is 1:2, reacted at 40℃.
Treatment of 1,2,4-acid wastewater combined flocculation with adsorption process: In the flocculation experiments, use synthetic dicyandiamide-formalin polymer as flocculent, wastewater pH value is 3, flocculant dosage is 1%. In the adsorption experiments, employ synthetic organo modified bentonite as adsorbent, AEO-9 surfactant as modifier.the adsorption conditions are: The wastewater pH value is 8, adsorption time is for 30 min, adsorbent dosage is 5%, operated at room temperature. The process that adsorption after flocculation is more effective than the process flocculation after adsorption.
Compared with the main technological and economic index, the treatment effect is as follows:From a technical viewpoint,the treatment effects are: Coagulation-Complex extraction process (COD dropped to 50 mg/L)> Flocculation-Adsorption process (COD dropped to 253 mg/L)> Ferric/Carbon microelectrolysis-Fenton oxidation process ( COD reduced to 860 mg/L)> TOA-octanol-kerosene complex extraction process (COD dropped to 1840 mg/L)> CTMAB bentonite adsorption process (COD dropped to 4300 mg/L); From economic viewpoint, the treatment results are:Ferric-Carbon microelectrolysis -Fenton oxidation process (treatment costs RMB 5.4/m~3) Technical and economic requirements in treatment of 6-Nitry wastewater were: COD dropped to 2000 mg/L below, processing costs reduced to less than RMB 50/m~3, so flocculation-adsorption Process (preferred when technical factor is top priority), Ferric/Carbon micro-electrolysis-Fenton oxidation process can meet the requirements (preferred when economic factor is priority ).
本课题采用以下几种方法研究1,2,4-酸废水治理:(1)三辛胺-正辛醇-煤油络合萃取体系处理1,2,4-酸母液废水(2)有机膨润土处理1,2,4-酸母液废水(3)铁/炭微电解-Fenton氧化技术处理1,2,4-酸生产废水(4)絮凝-络合萃取处理1,2,4-酸废水(5)絮凝-吸附处理1,2,4-酸废水研究。研究结果表明:
三辛胺-正辛醇-煤油络合萃取体系处理1,2,4-酸母液废水:萃取的最佳工艺参数为:三辛胺与正辛醇、煤油的体积比为4:1:5。废水pH值为1.7,萃取相比O/A为1:5。反萃的最佳工艺参数为:NaOH质量分数为15%,反萃体系相比为2:1,反萃温度为40oC恒温搅拌60min,静置6h分相,反萃效率为84%。
膨润土有机化改性及其在6-硝生产废水治理中的应用:该部分研究了三种有机膨润土体系:CTMAB改性膨润土(阳离子表面活性剂体系)、三辛胺改性膨润土(有机胺体系)、阳离子淀粉改性膨润土(有机高分子体系),通过比较,得出以下结论:制备的难易程度为:阳离子表面活性剂体系>有机胺体系>有机高分子体系;制备的有机膨润土对1,2,4-酸废水的吸附能力依次为:阳离子表面活性剂体系(COD去除率75%)>有机胺体系(COD去除率68%)>有机高分子体系(COD去除率35%);相应的1m~3废水处理成本为:9.5元、65.7元、11元。表面活性剂作为有机改性剂或者辅助改性剂,相应制得的有机膨润土吸附性能大小依次为:阳离子型表面活性剂>非离子型表面活性剂>阴离子型表面活性剂。
铁/炭微电解-Fenton氧化技术处理1,2,4-酸生产废水:其工艺参数为: 1,2,4-酸母液废水调节pH值=1,活性炭用量1%,Fe/C=3:1,在常温,微电解反应3h;将微电解后的滤液调pH值=3,加入H_2O_22.5%进行1h的Fenton反应。
絮凝-络合萃取处理1,2,4-酸废水研究:以自制的双氰胺-甲醛絮凝剂絮凝处理1,2,4-酸母液废水,主要参数为:废水pH值=3,絮凝剂用量为1%,在70℃下快速搅拌2min,慢搅10min,再静置40min。三辛胺-正辛醇组成的萃取体系主要参数为:pH值=1.5、相比为1:6、萃取剂浓度为40%,常温下振荡两分钟,静置分层15min。采用NaOH溶液作反萃取剂,反萃取过程的主要参数为:NaOH浓度为15%,相比(B/O)=1:2,反应温度为40℃。
絮凝-吸附处理1,2,4-酸废水研究:在絮凝实验中,采用自制双氰胺-甲醛絮凝剂絮凝,当废水pH值=3,絮凝剂用量为1%。在吸附实验中,用自制的AEO-9插层改性制得的有机膨润土进行吸附,吸附工艺条件为:pH值为8,吸附时间30min,吸附剂用量为5%。先絮凝后吸附较先吸附后絮凝效果更好。
技术经济指标比较:从技术上看,处理效果依次为:絮凝-络合萃取工艺(COD降至50 mg/L)>絮凝-吸附工艺(COD降至253 mg/L) >铁炭微电解-Fenton氧化工艺(COD降至860 mg/L) >三辛胺-正辛醇-煤油络合萃取工艺(COD降至1840 mg/L) >CTMAB改性膨润土吸附工艺(COD降至4300 mg/L);经济上看,处理成本依次为:铁炭微电解-Fenton氧化工艺(处理费用5.4元/ m~3)< CTMAB改性膨润土吸附工艺(处理费用9.5元/ m~3) <絮凝-吸附工艺(处理费用25元/ m~3) <三辛胺-正辛醇-煤油络合萃取工艺(处理费用55.8元/ m~3) <絮凝-络合萃取工艺(处理费用114.2元/ m~3)。
处理6-硝生产废水的技术经济要求为COD降至2000 mg/L以下,处理费用降至低于50元/ m~3,因此絮凝-吸附工艺(优先考虑技术因素时可选)、铁炭微电解-Fenton氧化工艺可满足要求(优先考虑经济因素时可选)。
6-Nitro-1,2-azoxynaphthalene-4-sulfonic acid(i.e.6-Nitry) is an intermediate for producing acid medium dye. 6-nitry wastewater which comes from 6-nitry producttion, and the wastewater comprises two kinds of wastewater, 1,2,4-acid wastewater and 1,2-Naphthoxydiazole-4-sulfonic acid wastewater. COD, pH value, and treatment difficulty of the two kinds of wastewater are very similar . So the two kinds of wastewater can be mixed before wastewater treatment. This theses mainly studied on the treatment processes of 1,2,4-acid wastewater,and the wastewater composes of high concentration organics, has high toxicity and is difficult to be biochemical treated.
This topic took the following methods to treat1,2,4-acid wastewater: (1) TOA-Octanol- Kerosene complex extraction process (2) organic bentonite adsorption process (3) Ferric-Carbon microelectrolysis combined with Fenton oxidation process (4) Flocculation Combined with complex extraction process (5) Flocculation combined with adsorption process.The experiment results indicated that:
TOA-Octanol-Kerosene complex extraction process:under the optimum conditions that TOA:Octanol:Kerosene of 4:1:5, Wastewater pH value of 1.7, O/A of 1:5; the optimum parameters of back extraction are follow: NaOH concentration of 15%, phase volume ratio O/B of 2:1, and temperature of 40℃, stirred for 60min and standing for 6h to separate phase, the back extraction efficiency can reach for is 84%.
In organic modification of bentonite and its application in 6-nitrate wastewater treatment, three kinds of organic bentonite system were studied: CTMAB modified bentonite (cationic surfactant system), TOA modified bentonite (organic amine system), cationic starch modification bentonite (organic polymer system),by comparison, we got the following conclusions: the difficulty level of the three system from easy to difficult: cationic surfactant system > organic amine system>organic polymer system; the adsorption ability of organic bentonite: the cationic surfactant system (COD removal rate 75%) > organic amine system (COD removal rate 68%) > organic polymer system (COD removal rate 35%); The cost of 1m~3 wastewater treatment is RMB9.5, RMB65.7, RMB11 respectively. surfactants are as organic modifier or assist modifier, the corresponding adsorption ability of the organic bentonite is as follow: cationic surfactant > nonionic surfactant > anionic surfactant.
In Ferric-Carbon microelectrolysis combined with fenton oxidation process, the optimum experiment conditions are as follows: adjusted wastewater pH value to 1, added activated carbon dosage of 1%, Fe/C = 3:1,microelectrolysis reacted for 3h at room temperature; adjusted the filtrate pH value to 3, added H_2O_2 for 2.5% dosage, then Fenton reaction for 1h.
Flocculation combined with complexation extraction process:self-made dicyandiamide-formaldehyde polymer as flocculant, the main parameters are : adjusted wastewater pH value to 3, added flocculant of 1%, rapidly stirring at 70℃for 2 min, slow stirring for 10min, and then standing for 40min; TOA-Octanol extraction system at the following parameters: pH value is 1.5, phase ratio is 1:6, 40% extractants concentration , extracted at room temperature for two minutes, let it stand to layer for 15min. NaOH solution as back extractant, the main parameters of back extractant are:NaOH concentration is for 15%, phase ratio (B/O) is 1:2, reacted at 40℃.
Treatment of 1,2,4-acid wastewater combined flocculation with adsorption process: In the flocculation experiments, use synthetic dicyandiamide-formalin polymer as flocculent, wastewater pH value is 3, flocculant dosage is 1%. In the adsorption experiments, employ synthetic organo modified bentonite as adsorbent, AEO-9 surfactant as modifier.the adsorption conditions are: The wastewater pH value is 8, adsorption time is for 30 min, adsorbent dosage is 5%, operated at room temperature. The process that adsorption after flocculation is more effective than the process flocculation after adsorption.
Compared with the main technological and economic index, the treatment effect is as follows:From a technical viewpoint,the treatment effects are: Coagulation-Complex extraction process (COD dropped to 50 mg/L)> Flocculation-Adsorption process (COD dropped to 253 mg/L)> Ferric/Carbon microelectrolysis-Fenton oxidation process ( COD reduced to 860 mg/L)> TOA-octanol-kerosene complex extraction process (COD dropped to 1840 mg/L)> CTMAB bentonite adsorption process (COD dropped to 4300 mg/L); From economic viewpoint, the treatment results are:Ferric-Carbon microelectrolysis -Fenton oxidation process (treatment costs RMB 5.4/m~3)
引文
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