WO2015109901A1 - 处理焦化废水的萃取剂 - Google Patents

处理焦化废水的萃取剂 Download PDF

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WO2015109901A1
WO2015109901A1 PCT/CN2014/093866 CN2014093866W WO2015109901A1 WO 2015109901 A1 WO2015109901 A1 WO 2015109901A1 CN 2014093866 W CN2014093866 W CN 2014093866W WO 2015109901 A1 WO2015109901 A1 WO 2015109901A1
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extracting agent
extractant
coking wastewater
wastewater
extracting
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PCT/CN2014/093866
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English (en)
French (fr)
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宁朋歌
曹宏斌
张懿
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中国科学院过程工程研究所
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/26—Treatment of water, waste water, or sewage by extraction
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/32—Hydrocarbons, e.g. oil
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C02F2101/345—Phenols
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)

Definitions

  • This invention relates to extractants, and more particularly to multifunctional extractants for treating coking wastewater.
  • Coking wastewater is formed during high-temperature dry distillation of coal, gas purification and chemical product refining. It is a typical toxic and refractory organic wastewater, including dust-removing sewage, final cold sewage, and residual ammonia. Due to the different processes used in coking plants, the amount and quality of coking wastewater vary widely.
  • the main pollutants in coking wastewater are phenols, heterocyclic compounds such as pyridine, quinoline and anthracene, as well as small amounts of alcohols and aromatic hydrocarbons. These substances are highly toxic, difficult to biodegrade, and cause serious pollution to the environment, but also directly threaten human health. It has always been a difficult problem in coking wastewater treatment.
  • the current coking wastewater treatment methods are generally: (1) dephenolization: recovery of phenol in high-concentration phenol-containing wastewater by solvent extraction; (2) deamination: after ammonia removal of residual ammonia water, the concentration of ammonia is still high The volatile ammonia in the remaining ammonia water can be removed by steam stripping; (3) harmless treatment: subsequent biological treatment.
  • the process of dephenolation and denitrification in the treatment process is stepwise and complicated.
  • the extractant used can only extract phenolic substances, and has high solubility in water and is difficult to recycle.
  • the activated sludge process is currently the most widely used coking wastewater biological treatment technology, and is commonly used as the second-stage treatment process in wastewater treatment systems.
  • the suspended solids and colloidal substances in the wastewater are adsorbed by the activated sludge, and the soluble organic matter in the wastewater is used as a self-propagating nutrient by the microorganisms in the activated sludge, metabolized into biological cells, and oxidized to become the final product (mainly carbon dioxide). ).
  • Undissolved organic matter needs to be converted into dissolved organic matter before it is metabolized and utilized, and the wastewater is purified.
  • this method has a poor effect on the treatment of pollutants such as cyanide and ammonia nitrogen, and when the wastewater is cyanide or ammonia nitrogen.
  • pollutants such as cyanide and ammonia nitrogen
  • concentration of the pollutants is high, the activity of the microorganisms in the activated sludge is destroyed, the microorganisms are killed, and the treatment effect of the activated sludge coking wastewater is affected. Further processing of biological law investment costs and equipment operating costs are very expensive and difficult for most manufacturers to adopt.
  • the extractant extracts other N, S heterocyclic compounds, alcohols, lipids and aromatic hydrocarbons in the wastewater while extracting phenol.
  • the extracting agent of the invention breaks through the technical obstacle that the traditional extracting agent can only extract phenols, and other pollutants must be separately processed.
  • the two steps of dephenolization and denitrification of coking wastewater are combined into one, which not only simplifies the operation process, saves operating cost, but also has excellent extraction performance, low solubility, low loss, easy regeneration, recycling, and greatly improved coking wastewater treatment effect. .
  • An extracting agent for treating coking wastewater which comprises the following components by mass fraction: neutral phosphorus-containing extracting agent 4 to 25%, for example, 6%, 10%, 14%, 18%, 21%, 24% Etc.; acidic phosphorus-containing extractant 0.5 to 10%, for example, 0.8%, 1.5%, 4%, 6%, 9%, etc.; cosolvent 0.5 to 5%, for example, 0.7%, 1.1%, 1.8%, 2.5 %, 4%, 4.8%, etc.; diluent 60 to 95%, for example, 65%, 71%, 77%, 80%, 85%, 90%, 94%, and the like.
  • the extracting agent of the present invention contains the following components according to the mass fraction: 7-11% of the neutral phosphorus-containing extracting agent, 1 to 3% of the acidic phosphorus-containing extracting agent, and 1.4 to 1.6% of the auxiliary solvent. , thinner 86 ⁇ 92%.
  • the neutral phosphorus-containing extractant in the extractant of the invention contains a strong polar group and can destroy the compound in the sewage Hydrogen bond with water to complete the extractant for phenolic substances.
  • the neutral and acidic phosphorus-containing extractants have a synergistic effect.
  • strong self-polymerization is easy to occur, and the N, S heterocyclic compound and alcohol in the sewage are extracted by the reverse micelle extraction mechanism. Classes, esters, aromatic hydrocarbons, thus completing the efficient extraction of various organic substances in wastewater.
  • the extracting agent of the invention can simultaneously extract phenols, N-, S-heterocyclic compounds, and compounds such as alcohols, lipids, aromatic hydrocarbons and the like in wastewater.
  • the extractant of the present invention has a structural formula of the neutral phosphorus-containing extractant.
  • R 1 and R 3 are independently selected from RO, RCO or ROH, and R is a linear, branched or cyclic alkane or alkene group having 3 to 7 carbons, for example, a propane group, an isobutyl group, Cyclobutyl, pentenyl, n-hexyl or the like, and R 2 is a linear, branched or cyclic alkane or alkene group having 8 to 15 carbons, for example, 10, 12, 14 or the like.
  • At least one of R 1 and R 3 is RO.
  • the acidic phosphorus-containing extractant is 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester and/or di(2-ethylhexyl)phosphoric acid. .
  • the cosolvent may be one or a mixture of two or more of 3-heptanone, dichloromethane or propylene glycol butyl ether.
  • the co-solvent may be 3-heptanone.
  • the extracting agent of the present invention is benzene and/or kerosene.
  • the extracting agent of the present invention is prepared by thoroughly mixing the components at a temperature ratio of 20 ° C to 40 ° C and cooling to room temperature.
  • the extractant is multifunctional. It can simultaneously extract phenols, heterocyclic compounds, alcohols, esters and aromatic hydrocarbons in wastewater; it can simultaneously complete the process of dephenolization and denitrification of coking wastewater, expand the application range of extractant, and simplify the treatment process of coking wastewater. .
  • the boiling range of the extractant is 110-180 °C, which is similar to the boiling range of the extractant used by most current manufacturers, and does not need to be replaced when used.
  • the extraction process is mature, the process is simple, and the economic benefits are obvious.
  • Extractant 1 8 g of dimethyl heptyl methacrylate, 3 g of 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester, 0.8 g of 3-heptanone, 0.4 g of propylene glycol butyl ether, 87.8 g of kerosene, 30 ° C The mixture is uniformly mixed, and cooling to room temperature is the multifunctional extractant 1 of the present invention.
  • Extractant 2 Take 20g of cyclopropyldimethylhexyl ester, 1g of di(2-ethylhexyl)phosphoric acid, 0.5g of 3-heptanone, 0.2g of dichloromethane, 78.3g of benzene, and mix evenly at room temperature.
  • the multifunctional extractant 2 of the invention Take 20g of cyclopropyldimethylhexyl ester, 1g of di(2-ethylhexyl)phosphoric acid, 0.5g of 3-heptanone, 0.2g of dichloromethane, 78.3g of benzene, and mix evenly at room temperature.
  • the multifunctional extractant 2 of the invention Take 20g of cyclopropyldimethylhexyl ester, 1g of di(2-ethylhexyl)phosphoric acid, 0.5g of 3-heptanone, 0.2g of dichloromethane, 78.3g of benzene, and mix evenly at room
  • Extractant 3 14 g of isoamyldimethylammonate, 4 g of 2-ethylhexylphosphonic acid mono-2-ethylhexyl- and 5 g of di(2-ethylhexyl)phosphoric acid, 2 g of 3-heptanone, 0.3 g propylene glycol butyl ether, 74.7 g kerosene, uniformly mixed at 40 ° C, and cooled to room temperature is the multifunctional extractant 3 of the present invention.
  • the coking wastewater provided by the three manufacturers is used, and the wastewater quality is shown in Table 1.
  • COD removal rate (%) (chemical oxygen demand of untreated wastewater - chemical oxygen demand of wastewater treated with extractant) / chemical oxygen demand of untreated wastewater * 100.
  • the chemical oxygen demand is the chemical oxygen demand of all reducing substances in the sewage.
  • the multifunctional extractant disclosed by the present invention has a wide application range and can not only have The phenolic compound is removed effectively, and the quinoline and pyridine compounds which are difficult to be treated in the coking wastewater are removed, and the removal rate is high, and the minimum removal rate is not less than 92%. After tertiary extraction, the COD (chemical oxygen demand) value can be reduced by more than 98%.
  • the above extractant was recovered by distillation, and the recovery rate was about 99.5%.
  • the above experiment was repeated, and the COD removal rate was still above 98%. It can be seen that the multifunctional extraction has low solubility in water and high recycling value, and can be applied to large-scale industrial production.
  • the present invention illustrates the detailed process equipment and process flow of the present invention by the above embodiments, but the present invention is not limited to the above detailed process equipment and process flow, that is, does not mean that the present invention must rely on the above detailed process equipment and The process can only be implemented. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitution of the various materials of the products of the present invention, addition of auxiliary components, selection of specific means, and the like, are all within the scope of the present invention.

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Activated Sludge Processes (AREA)
  • Removal Of Specific Substances (AREA)
  • Physical Water Treatments (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

本发明涉及用于处理焦化废水的萃取剂，按质量分数含以下组分：中性含磷类萃取剂4～25％，酸性含磷类萃取剂0.5～10％，助溶剂0.5～5％，稀释剂60～95％。本发明的萃取剂可在较宽范围内使用，能同时萃取焦化废水中的酚、杂环化合物、酯、芳香烃等多种污染物，实现焦化废水脱酚处理和脱氮处理同步实现；且该种萃取剂溶解度小，可高效重复循环使用。本发明的萃取剂解决了焦化废水处理步骤繁琐，设备众多，萃取效率低下，萃取剂损失严重等问题，实现了萃取剂的高效性。

Description

处理焦化废水的萃取剂 技术领域
本发明涉及萃取剂，尤其涉及用于处理焦化废水的多功能型萃取剂。
背景技术
焦化废水是煤高温干馏、煤气净化和化学产品精制过程中形成的，是一种典型的有毒难降解有机废水，包括除尘污水、终冷污水、剩余氨水等。由于焦化厂采用的工艺不同，焦化废水的数量和水质差别很大。焦化废水中的主要污染物为酚类，吡啶、喹啉、吲哚类等杂环化合物，以及少量醇、芳烃类。这些物质毒性大，生物降解难，对环境造成严重污染的同时也直接威胁到人类健康，一直是焦化废水处理的难点问题。
现行焦化废水处理方法一般为：(1)脱酚：对高浓度含酚废水中的酚用溶剂萃取法进行回收；(2)脱氨：剩余氨水经脱酚处理后，氨的浓度还很高，采用蒸汽吹脱法可除去剩余氨水中的挥发氨；(3)无害化处理：即后续的生物处理等。
该处理流程中脱酚、脱氮分步处理，程序繁琐复杂。所应用的萃取剂只能萃取酚类物质，且在水中溶解度大，回收利用困难。
此外，活性污泥法是目前应用最广泛的焦化废水生物处理技术，常用为废水处理系统中的第二级处理工艺。废水中的悬浮固体和胶状物质被活性污泥吸附，而废水中的可溶性有机物被活性污泥中的微生物用作自身繁殖的营养，代谢转化为生物细胞，并氧化成为最终产物(主要为二氧化碳)。非溶解性有机物需先转化成溶解性有机物，而后才被代谢和利用，废水由此得到净化。但是此方法对氰化物、氨氮等污染物的处理效果较差，并且当废水中氰化物、氨氮 等污染物的浓度较高时，会破坏活性污泥中微生物的活动，使微生物死亡，影响活性污泥对焦化废水的处理效果。进一步处理的生物法投资费用及设备运转费用都十分昂贵，多数厂家难以采用。
废水经上述工艺处理后，大量高毒有机物依然留存水中，不能达到《钢铁工业污染物排放标准》所规定的排放标准。因此，有必要发展多功能型高效萃取剂，简化焦化废水处理流程，提高污水处理效率。
发明内容
本发明的目的在于提供一种用于处理焦化含酚废水的多功能型萃取剂。该种萃取剂在萃取酚的同时能萃取废水中的其它N、S杂环化合物、醇、脂和芳香烃类物质。本发明的萃取剂突破了传统萃取剂只能萃取酚类，其他污染物必须另行处理的技术障碍。将焦化废水脱酚和脱氮两步合二为一，不但简化了操作过程，节约操作成本，而且萃取性能优异，溶解度低，损失小，易于重生，可循环利用，大大提高了焦化废水处理效果。
为达上述目的，本发明采用如下技术方案：
一种用于处理焦化废水的萃取剂，按质量分数含以下组分：中性含磷类萃取剂4～25％，例如为6％、10％、14％、18％、21％、24％等；酸性含磷类萃取剂0.5～10％，例如为0.8％、1.5％、4％、6％、9％等；助溶剂0.5～5％，例如为0.7％、1.1％、1.8％、2.5％、4％、4.8％等；稀释剂60～95％，例如为65％、71％、77％、80％、85％、90％、94％等。
作为优选技术方案，本发明所述的萃取剂，按质量分数含以下组分：中性含磷类萃取剂7～11％，酸性含磷类萃取剂1～3％，助溶剂1.4～1.6％，稀释剂86～92％。
本发明萃取剂中的中性含磷萃取剂含极强的极性基，能破坏污水中化合物 与水的氢键，完成对酚类物质的萃取剂。同时其中的中性与酸性含磷萃取剂有协同作用，在助溶剂与稀释剂的作用下，易发生强烈自聚，以反胶团萃取机理萃取污水中的含N、S杂环化合物、醇类、酯类、芳香烃类化合物，从而完成对废水中各种有机物的高效萃取。
本发明的萃取剂能同时萃取废水中的酚类、含N、S杂环化合物，以及醇类、脂类、芳香烃类等化合物。
作为优选技术方案，本发明所述的萃取剂，所述中性含磷类萃取剂结构式为
Figure PCTCN2014093866-appb-000001
式中R1、R3独立的任选自RO、RCO或ROH，R为具有3-7个碳的直链、支链或环的烷烃基或烯烃基，例如为丙烷基、异丁基、环丁基、戊烯基、正己基等，R2为具有8-15个碳，例如为10个、12个、14个等的直链、支链或环的烷烃基或烯烃基。
优选地，R1、R3中至少有一个为RO。
作为优选技术方案，本发明所述的萃取剂，所述的酸性含磷类萃取剂为2-乙基己基膦酸单-2-乙基己基酯和/或二(2-乙基己基)磷酸。
作为优选技术方案，本发明所述的萃取剂，所述助溶剂为3-庚酮、二氯甲烷或丙二醇丁醚中的1种或2种以上的混合，例如助溶剂可以为3-庚酮或丙二醇丁醚，或者为二氯甲烷与丙二醇丁醚的混合物，或者为3-庚酮、二氯甲烷与丙二醇丁醚三者的混合物。
作为优选技术方案，本发明所述的萃取剂，所述稀释剂为苯和/或煤油。
本发明所述萃取剂的制备方法为，按重量配比将所述成分在20℃～40℃下充分混合，冷却至室温即得。
与现有技术相比，本发明的有益效果如下：
(1)该萃取剂具有多功能性。能同步萃取废水中的酚类、杂环化合物、醇、酯和芳香烃等物质；能将焦化废水脱酚、脱氮等工艺同步完成，拓展了萃取剂应用范围，简化了焦化废水的处理工艺。
(2)萃取剂沸程为110-180℃，与现行大部分厂家所采用的萃取剂沸程相近，使用时不需更换设备。萃取工艺成熟，流程简单，具有明显的经济效益。
(3)该萃取剂在水中溶解度极低，＜0.001％，远低于目前使用的大部分萃取剂；萃取过程中损失小，循环利用价值高。
(3)萃取性能优异。经过三级萃取剂，该萃取剂对焦化废水中有机污染物最低去除率＞92％，COD去除率＞98％，具有高效性。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案。下列实施例是对本发明的进一步解释和补充，对本发明不构成任何限制。
1、萃取剂的制备
萃取剂1：取8g甲基磷酸二甲庚酯，3g 2-乙基己基膦酸单-2-乙基己基酯，0.8g 3-庚酮，0.4g丙二醇丁醚，87.8g煤油，30℃下混合均匀，冷却至室温即为本发明的多功能型萃取剂1。
萃取剂2：取20g环丙基二甲己酯，1g二(2-乙基己基)磷酸，0.5g 3-庚酮，0.2g二氯甲烷，78.3g苯，室温下混合均匀，即为本发明的多功能型萃取剂2。
萃取剂3：取14g异戊基二甲戊酯，4g 2-乙基己基膦酸单-2-乙基己基酯-和5g二(2-乙基己基)磷酸，2g 3-庚酮，0.3g丙二醇丁醚，74.7g煤油，40℃下混合均匀，冷却至室温即为本发明的多功能型萃取剂3。
2、废水的来源和水质
采用三家厂家提供的焦化废水，废水水质如表1所示。
表1
Figure PCTCN2014093866-appb-000002
3、萃取实验
分别取等体积的焦化废水和萃取剂1加入分液漏斗中；室温震荡0.5h，静置1h。经三级萃取，取下层水相，进行检测，并计算去除率。萃取剂1的萃取结果见表2。萃取剂2的结果见表3。萃取剂3的结果见表4。
表2
Figure PCTCN2014093866-appb-000003
Figure PCTCN2014093866-appb-000004
表3
Figure PCTCN2014093866-appb-000005
表4
Figure PCTCN2014093866-appb-000006
COD去除率(％)＝(不经处理的废水的化学需氧量-用萃取剂处理后的废水的化学需氧量)/不经处理的废水的化学需氧量*100。
其中，化学需氧量是污水中所有还原性物质的化学需要氧量。
从以上结果可知，本发明公布的多功能型萃取剂适用范围较广，不仅能有 效去除酚类化合物，而且能去除焦化废水中较难处理的喹啉、吡啶类化合物，并且去除率高，最小去除率不低于92％。三级萃取后，COD(化学需氧量)值可降低98％以上。
精馏法回收上述萃取剂，回收率大约为99.5％。重复上述实验，萃取结果，COD去除率依然达98％以上。可见该多功能型萃取在水中溶解度小，回收利用价值高，可运用于大规模工业生产。
申请人声明，本发明通过上述实施例来说明本发明的详细工艺设备和工艺流程，但本发明并不局限于上述详细工艺设备和工艺流程，即不意味着本发明必须依赖上述详细工艺设备和工艺流程才能实施。所属技术领域的技术人员应该明了，对本发明的任何改进，对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等，均落在本发明的保护范围和公开范围之内。

Claims (7)

  1. 一种用于处理焦化废水的萃取剂，其特征在于，按质量分数含以下组分：中性含磷类萃取剂4～25％，酸性含磷类萃取剂0.5～10％，助溶剂0.5～5％，稀释剂60～95％。
  2. 根据权利要求1所述的萃取剂，其特征在于，按质量分数含以下组分：中性含磷类萃取剂7～11％，酸性含磷类萃取剂1～3％，助溶剂1.4～1.6％，稀释剂86～92％。
  3. 根据权利要求1或2所述的萃取剂，其特征在于，所述中性含磷类萃取剂结构式为
    Figure PCTCN2014093866-appb-100001
    式中R1、R3独立的任选自RO、RCO或ROH，R为具有3-7个碳的直链、支链或环的烷烃基或烯烃基，R2为具有8-15个碳的直链、支链或环的烷烃基或烯烃基。
  4. 根据权利要求3所述的萃取剂，其特征在于，R1、R3中至少有一个为RO。
  5. 根据权利要求1-4任一项所述的萃取剂，其特征在于，所述的酸性含磷类萃取剂为2-乙基己基膦酸单-2-乙基己基酯和/或二(2-乙基己基)磷酸。
  6. 根据权利要求1-5任一项所述的萃取剂，其特征在于，所述助溶剂为3-庚酮、二氯甲烷或丙二醇丁醚中的1种或2种以上的混合。
  7. 根据权利要求1-6任一项所述的萃取剂，其特征在于，所述稀释剂为苯和/或煤油。
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