WO2007080686A1 - Procede de traitement d’eau usagee contenant du selenium - Google Patents

Procede de traitement d’eau usagee contenant du selenium Download PDF

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Publication number
WO2007080686A1
WO2007080686A1 PCT/JP2006/321244 JP2006321244W WO2007080686A1 WO 2007080686 A1 WO2007080686 A1 WO 2007080686A1 JP 2006321244 W JP2006321244 W JP 2006321244W WO 2007080686 A1 WO2007080686 A1 WO 2007080686A1
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WO
WIPO (PCT)
Prior art keywords
selenium
wastewater
acid
waste water
containing wastewater
Prior art date
Application number
PCT/JP2006/321244
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English (en)
Japanese (ja)
Inventor
Yasuto Kashiwagi
Original Assignee
University Of Tsukuba
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University Of Tsukuba filed Critical University Of Tsukuba
Priority to JP2007553835A priority Critical patent/JP5211320B2/ja
Publication of WO2007080686A1 publication Critical patent/WO2007080686A1/fr

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Classifications

    • 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
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • 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
    • C02F1/68—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water
    • 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
    • C02F1/70—Treatment of water, waste water, or sewage by reduction
    • C02F1/705—Reduction by metals
    • 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
    • C02F2101/10—Inorganic compounds
    • 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
    • C02F2103/346—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 semiconductor processing, e.g. waste water from polishing of wafers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • the present invention relates to a wastewater treatment method for removing selenium and a selenium compound from wastewater containing selenium and a selenium compound efficiently and at low cost in consideration of safety in the work environment.
  • Selenium is used as a raw material, a secondary ingredient in various manufacturing processes such as semiconductors, glass, batteries including solar cells, red pigments, metal surface colorants, pharmaceuticals, flue gas desulfurization processes, and petroleum refining processes. It is handled as a product or a substance to be removed.
  • manufacturing processes such as semiconductors, glass, batteries including solar cells, red pigments, metal surface colorants, pharmaceuticals, flue gas desulfurization processes, and petroleum refining processes. It is handled as a product or a substance to be removed.
  • selenium and selenium compounds are harmful substances, selenium and selenium compounds have been revised on December 27, 1993 by the partial amendment of the Water Pollution Control Act (Decree No. 401 of 1993). Were added to the drainage standard health items, and the drainage standard value was set at 0.1 mgZ liter.
  • the drainage power treatment methods for removing selenium and selenium compounds include neutralization coagulation precipitation method, iron hydroxide precipitation method, coagulation precipitation method such as ferrite precipitation method, ion exchange membrane method, activated charcoal. Adsorption methods and the like are known.
  • selenium in waste water is usually colloidal selenium, oxidation number 4 valent selenite ion (SeO 2 ) or oxidation number 6 valent selenate ion (SeO 2 ").
  • Japanese Patent Application Laid-Open No. 2000-167572 discloses a method of evaporating and concentrating selenium-containing wastewater, adjusting the pH of the concentrated water to 6 or less, and warming it to 60 ° C or higher to form a metal.
  • a method for treating selenium-containing water by contact with iron or by adding iron ( ⁇ ) salt is another example of the coagulation precipitation method.
  • 10-218611 discloses a reduction in which sulfuric acid is added so that the concentration of sulfuric acid in the selenium-containing solution is 3.5 to 6N, and metal powder or metal ion power is also obtained.
  • a method for treating a selenium-containing solution in which selenium is precipitated as a selenide of a reducing agent metal by adding an agent and treating at a temperature of 80 ° C. or higher is disclosed.
  • Japanese Patent Application Laid-Open No. 09-239377 discloses selenate ions.
  • Selenium containing wastewater containing selenium is irradiated with light in the presence of a semiconductor photocatalyst and an organic cyclic agent to reduce the selenate ion to solid selenium and Z or gaseous selenium-hydrogen.
  • Patent Document 1 Japanese Unexamined Patent Publication No. 2000-167572
  • Patent Document 2 Japanese Patent Laid-Open No. 10-218611
  • Patent Document 3 Japanese Patent Laid-Open No. 09-239377
  • the treatment method using the ion exchange method requires irradiation with light in the presence of a semiconductor photocatalyst and an organic cyclizing agent, it requires a long time for wastewater treatment and the above-described coagulation precipitation treatment method. Similar to, a large amount of expenditure is required for wastewater treatment facilities and treatment work.
  • an object of the present invention is to provide a treatment method that effectively removes selenium and selenium compounds containing selenium and selenium compounds in a short time and at low cost. Furthermore, the present invention effectively collects selenium and a selenium compound vaporized during the treatment of the waste water and returns them to the waste water, so that the selenium and selenium can also be contained in the atmosphere and working environment air. Means for solving the problems aimed at providing a wastewater treatment method that does not release compounds
  • the present invention provides a wastewater treatment method for treating wastewater containing selenious acid and selenic acid, and (a) the inorganic waste acid is added to make the wastewater acidic at a pH of 3 or less. (B) a step of introducing iron powder into the waste water; (c) a step of stirring the waste water at room temperature; and (d) air containing gas generated in the stirring step (c) is sulfuric acid.
  • the present invention provides a method for treating selenium-containing wastewater characterized by comprising the steps of performing the treatments described in steps (a) to (c).
  • the inorganic acid used in the step (a) is hydrochloric acid or sulfuric acid, and the molar concentration of the inorganic acid with respect to the waste water is 0.03 M or more.
  • step (b) 3 to 5 grams of iron powder is injected per liter of the waste water. Further, for the stirring in the step (c), strong stirring for about 10 minutes is sufficient.
  • the sulfuric acid potassium permanganate solution used in the step (d) is 0.3 to 0.5% by weight / volume permanganese in dilute sulfuric acid having a mol concentration of 1 to 2M. Use one that contains acid potassium.
  • the step (d) when the red fading of the sulfuric acid potassium permanganate solution is lower than a predetermined level, the step (d) is performed.
  • the treatment is performed by passing through a plurality of air selenium removing means connected in series.
  • the waste water after the step (c) is subjected to coagulation sedimentation by adding an alkaline agent to pHIO or more, and the resulting precipitate is separated and concentrated in a sedimentation tank, and the concentrated precipitate is further dehydrated. .
  • the wastewater treatment method for treating wastewater containing selenious acid and selenate according to the present invention includes a facility, a semiconductor photocatalyst, and an organic cyclic agent used together with an activated carbon treatment method as in the conventional treatment method. Since there is no need to irradiate light in the presence of existing equipment and the existing wastewater treatment facility can be used as it is, it can be treated at a low cost and by simply stirring the wastewater for about 10 minutes at room temperature. This made it possible to treat wastewater containing selenious acid and selenic acid.
  • FIG. 1 shows an overview of the steps of a wastewater treatment method for treating wastewater containing selenious acid and selenic acid according to the present invention.
  • industrial wastewater containing selenium is often colloidal selenium, tetravalent oxide selenite ion (SeO 2 or less, referred to as ⁇ Se (IV) '' where appropriate) and
  • the pH of the wastewater is adjusted to 3 or less by first adding hydrochloric acid or an inorganic acid of sulfuric acid to the selenium-containing wastewater.
  • the inorganic acid is hydrochloric acid
  • the molar concentration of hydrochloric acid with respect to the wastewater is 0.03M or more.
  • iron powder is put into the wastewater adjusted to pH 3 or less (step (b)).
  • the amount of iron powder input is 3 to 5 grams per liter of wastewater, but about 5 grams is desirable.
  • throwing-in is stirred strongly (process (c)).
  • the stirring time is about 8 to 10 minutes.
  • the selenite ion having a tetravalent acid number changes to red selenium Se (0) in a very short time (a few seconds after the start of stirring). It was confirmed that the selenate ion began to turn reddish brown after depositing red selenium after about 90 seconds. From the observation of the reduction behavior of selenite and selenate, the selenate ion with an oxidation number of 6 is first reduced to a selenite ion with an oxidation number of 4 and then reduced to red selenium as a simple selenium. Was confirmed.
  • the method for treating selenium-containing wastewater according to the present invention includes a step of recovering selenium and a selenium compound transferred to the gas phase in the above-described strong stirring step. That is, air containing selenium and a selenium compound that have been transferred to the gas phase through the stirring step is passed through the potassium sulfate permanganate solution (step (d)). As a result, the selenium and the selenium compound transferred to the gas phase are collected in the sulfuric acid potassium permanganate solution. The acidic permanganate solution is reduced to the remaining potassium permanganate with a general-purpose reducing agent, returned to the selenium-containing wastewater, and reliably recovered through the above steps (a) to (c). It is.
  • the sulfuric acid potassium permanganate solution used in the above step (d) contains 0.3 to 0.5% potassium permanganate by weight to volume% in dilute sulfuric acid having a molar concentration of 1 to 2M. Contains.
  • redness of the sulfuric acid potassium permanganate solution produced by the step (d) is obtained.
  • the color fading is lower than a predetermined level, it may be processed by passing it through a plurality of air selenium removal means connected in series. However, as will be described later, a single pass process is usually sufficient.
  • the waste water after the step (c) is released into sewage or the like by a coagulating sedimentation treatment by adding a known alkali agent, separation and concentration of the precipitate, and dehydration treatment, and solid matter is sludge. Will be processed.
  • FIG. 2 schematically shows the steps constituting the selenium-containing wastewater treatment method according to the present invention shown in FIG.
  • the process illustrated in FIG. 2 is a force that describes the process that should be added as necessary in addition to the essential process of the present treatment method.
  • the description regarding the process is as described above.
  • wastewater contains harmful substances related to wastewater regulations such as arsenic, mercury, cyanide, and fluorine other than selenium that is subject to removal by the present invention, these harmful substances constitute the present invention. Needless to say, it can also be removed simultaneously by adding iron powder and intensive stirring.
  • the wastewater containing selenious acid and selenic acid is passed through the chemical reaction inlet from the chemical solution inlet to the sealed reaction tank having an intake pipe and an exhaust pipe. Put it into a pH of 3 or less, add force iron powder from the iron powder feeder, and immediately stir the selenium-containing wastewater in the reaction tank with a stirrer. Immediately after the start of the iron powder reaction by vigorous stirring, hydrochloric acid and iron powder react to generate hydrogen in the active stage, and selenite and selenic acid are reduced to room temperature by chemical conversion to single selenium. . Further, a part of the produced single selenium is vaporized by chemical reduction at room temperature to hydrogen selenide.
  • the cleaning liquid in the air cleaning tank containing hydrogen selenide gas and selenium-containing mist has an oxidizing power and uses a sulfuric acid potassium permanganate liquid that changes color according to the oxidizing power, A small amount of selenium-hydrogen gas will be absorbed by acid, and the exhaust air will be washed with water and safely discharged into the atmosphere or working environment. Under long-term use conditions or conditions that treat wastewater containing high concentrations of selenium, it is better to detect the cleaning ability easily by using the sulfuric acid potassium permanganate solution based on the degree of red fading of the cleaning solution.
  • the washing tanks are arranged in parallel, and the degree of red fading of the potassium permanganate liquid as the washing liquid Depending on the situation, by switching the introduction of exhaust air to another air cleaning tank containing unused cleaning liquid, it is possible to deal with the treatment of wastewater containing low concentration, high concentration selenium.
  • the used cleaning solution containing selenium whose fading color has faded and whose collection performance has deteriorated is returned to the reaction tank, and the remaining potassium permanganate is reduced for general water treatment such as sodium sulfite. It also has the ability to remove vaporized selenium by chemical reduction action at room temperature by the iron powder treatment method after reduction with an agent.
  • FIG. 3 is a graph showing the total residual selenium concentration in the wastewater when the above-described method for treating selenium-containing wastewater according to the present invention is carried out.
  • the unit of the horizontal axis of the graph indicates the concentration of selenium in the wastewater [Se (IV) and Se (VI) concentrations, mgZ liters], and the vertical axis of the graph shows the treatment method for this selenium-containing wastewater.
  • the total residual selenium concentration in the treated water (Se ( IV) and Se (VI) are summed, and mgZ liter) is determined.
  • the treatment conditions in the graph shown in Fig. 3 are as follows.
  • step (a) Hydrochloric acid was added to the selenium-containing wastewater to make it pHO.4 (step (a)), and 5 grams of iron powder was added per liter of wastewater ( Step (b)). Then, it was vigorously stirred for 10 minutes (step (c)).
  • Fig. 4 shows the residual concentration of selenic acid after wastewater treatment and the reaction liquid concentration due to the concentration of inorganic acid (hydrochloric acid) in the wastewater acidification treatment (step (a)) that constitutes the treatment method of this selenium-containing wastewater. It is a graph which shows the influence degree to pH. Other conditions are the same as those described in FIG.
  • the conditions of the graph shown in FIG. 4 were that hydrochloric acid was used as the inorganic acid, and the concentration of selenic acid (hexavalent selenium) in the stock solution was 50 (mgZ liter).
  • the horizontal axis of the graph shows the molar concentration of hydrochloric acid in the stock solution, and the left vertical axis of the graph shows the residual concentration of selenic acid (hexavalent selenium) in the treated water after the treatment method for this selenium-containing wastewater (mgZ liters)
  • the right vertical axis of the graph indicates the pH value of the reaction solution.
  • Fig. 5 shows that in the present method for treating selenium-containing wastewater, when iron powder is introduced into the selenium-containing wastewater and vigorously stirred (step (c)), selenite and selenate in the wastewater are vapor-phased. It shows the percentage (%) to shift to. Other conditions are the same as those described in FIG.
  • FIG. 5 shows that 0.3 to 4% of the tetravalent selenium and the hexavalent selenium migrate to the gas phase.
  • the stirring time was 10 minutes.
  • the higher the selenium content in the stock solution the lower the percentage (%) of selenium transferred to the gas phase.
  • the average selenium concentration in the gas phase is 0.59 to 23.2 mgZm 3
  • the exposure limit of selenium to humans is 0. It exceeded 2 mg / m 3 .
  • the proportion of tetravalent selenium and hexavalent selenium transferred to the gas phase is never negligible, indicating the need to collect this.
  • the method for treating selenium-containing wastewater according to the present invention further recovers tetravalent selenium and hexavalent selenium transferred to the gas phase through the iron powder charging step and the strong stirring step.
  • Process (step (d)) That is, air containing a gaseous substance is passed through the sulfuric acid potassium permanganate solution in the stirring step. As a result, the tetravalent selenium and hexavalent selenium transferred to the gas phase are collected in the sulfuric acid potassium permanganate solution.
  • the acidic permanganate sulfate solution containing the tetravalent selenium and the hexavalent selenium thus collected is reduced to the remaining potassium permanganate and then returned to the selenium-containing waste water to be reliably recovered.
  • the sulfuric acid acidic potassium permanganate solution used in the step (d) is prepared by adding 0.3 to 0.5% potassium permanganate by weight to volume% in dilute sulfuric acid having a molar concentration of 1 to 2M. It contains.
  • FIG. 6 is a graph showing the collection rate of tetravalent selenium and hexavalent selenium transferred to the gas phase by the treatment step (d). As shown in Fig. 6, it is possible to collect 98% or more of both tetravalent selenium and hexavalent selenium.
  • red fading of the sulfuric acid-acid potassium permanganate solution is achieved by one-step passage of air containing tetravalent selenium and hexavalent selenium that has been transferred to the gas phase into the potassium acid permanganate solution. If the degree of slag is significant, it may be treated by passing it through a plurality of stages of air selenium removal means connected in a plurality of stages in series.
  • the processing conditions in FIG. 6 are the same as those described in FIG.
  • the present invention relates to selenium and selenium compounds from waste water containing selenium and selenium compounds. It is related to a wastewater treatment method that removes water efficiently and at low cost in consideration of the safety of the work environment, and has industrial applicability.
  • FIG. 1 shows an outline of the steps of a wastewater treatment method for treating wastewater containing selenious acid and selenic acid according to the present invention.
  • FIG. 2 schematically shows the steps constituting the selenium-containing wastewater treatment method according to the present invention shown in FIG.
  • FIG. 3 is a graph showing the total residual selenium concentration in wastewater when the above-described method for treating selenium-containing wastewater according to the present invention is carried out.
  • FIG. 4 A graph showing the effect of inorganic acid (hydrochloric acid) concentration on the residual concentration of selenic acid after wastewater treatment and the pH of the reaction solution in the acidity treatment of wastewater that constitutes the treatment method for wastewater containing selenium. is there.
  • FIG. 5 In this selenium-containing wastewater treatment method, when iron powder is introduced into selenite and selenate-containing wastewater and stirred vigorously, selenite and selenate in the wastewater are transferred to the gas phase. It shows the result.
  • FIG. 6 is a graph showing the collection rate of selenic acid transferred to the gas phase in the present invention. Explanation of symbols

Abstract

La présente invention concerne un procédé d’élimination efficace du sélénium et de composés à base de sélénium d’une eau usagée contenant du sélénium et des composés à base de sélénium sur une période courte dans des conditions ordinaires de température à bas coût et de collecte du sélénium et de composés à base de sélénium vaporisés. Ce procédé comprend l'étape (a) consistant à ajouter un acide inorganique à une eau usagée de façon à ajuster le pH de l'eau usagée à une valeur inférieure ou égale à 3, l'étape (b) consistant à ajouter de la poudre de fer dans l'eau usagée résultante, l'étape (c) consistant à agiter l'eau usagée à une température ordinaire, l'étape (d) consistant à faire passer le gaz contenant de l’air produit dans l'étape (c) à travers une solution de permanganate de potassium acidifiée avec de l'acide sulfurique, l'étape (e) consistant à réduire le permanganate de potassium résiduel contenu dans la solution et ensuite à ajouter la solution résultante à l'eau usagée, et l'étape (f) consistant à effectuer les étapes (a), (b) et (c).
PCT/JP2006/321244 2006-01-12 2006-10-25 Procede de traitement d’eau usagee contenant du selenium WO2007080686A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2007553835A JP5211320B2 (ja) 2006-01-12 2006-10-25 セレン含有排水処理方法

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JP2006-004343 2006-01-12
JP2006004343 2006-01-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013522008A (ja) * 2010-03-10 2013-06-13 ナルコ カンパニー 製油所廃液からセレンの除去
CN103922511A (zh) * 2014-05-05 2014-07-16 哈尔滨工业大学 一种水中微量硒的去除方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3365283A4 (fr) * 2015-10-21 2019-04-03 The Texas A & M University System Procédé d'élimination d'espèces récalcitrantes de sélénium présentes dans les eaux usées

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01262930A (ja) * 1988-04-11 1989-10-19 Pure Kurieito:Kk 有害気体の連続浄化方法
JPH08309369A (ja) * 1995-05-17 1996-11-26 Kurita Water Ind Ltd セレン含有水の処理方法
JPH09239377A (ja) * 1996-03-07 1997-09-16 Agency Of Ind Science & Technol 排水中からのセレン酸イオンの除去方法
JPH10218611A (ja) * 1997-02-05 1998-08-18 Sumitomo Metal Mining Co Ltd セレン含有溶液の処理方法
JP2002011482A (ja) * 2000-06-28 2002-01-15 Kurita Water Ind Ltd セレン含有水の処理方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01262930A (ja) * 1988-04-11 1989-10-19 Pure Kurieito:Kk 有害気体の連続浄化方法
JPH08309369A (ja) * 1995-05-17 1996-11-26 Kurita Water Ind Ltd セレン含有水の処理方法
JPH09239377A (ja) * 1996-03-07 1997-09-16 Agency Of Ind Science & Technol 排水中からのセレン酸イオンの除去方法
JPH10218611A (ja) * 1997-02-05 1998-08-18 Sumitomo Metal Mining Co Ltd セレン含有溶液の処理方法
JP2002011482A (ja) * 2000-06-28 2002-01-15 Kurita Water Ind Ltd セレン含有水の処理方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013522008A (ja) * 2010-03-10 2013-06-13 ナルコ カンパニー 製油所廃液からセレンの除去
CN103922511A (zh) * 2014-05-05 2014-07-16 哈尔滨工业大学 一种水中微量硒的去除方法
CN103922511B (zh) * 2014-05-05 2015-08-19 哈尔滨工业大学 一种水中微量硒的去除方法

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