WO2024075518A1 - Procédé de décoloration de déchets liquides industriels - Google Patents

Procédé de décoloration de déchets liquides industriels Download PDF

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Publication number
WO2024075518A1
WO2024075518A1 PCT/JP2023/033958 JP2023033958W WO2024075518A1 WO 2024075518 A1 WO2024075518 A1 WO 2024075518A1 JP 2023033958 W JP2023033958 W JP 2023033958W WO 2024075518 A1 WO2024075518 A1 WO 2024075518A1
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supernatant
cationic polymer
liquid
industrial wastewater
wastewater
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PCT/JP2023/033958
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English (en)
Japanese (ja)
Inventor
哲也 足立
順治 中野
正男 中野
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中国環境株式会社
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Publication of WO2024075518A1 publication Critical patent/WO2024075518A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/01—Separation of suspended solid particles from liquids by sedimentation using flocculating agents
    • 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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • 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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56—Macromolecular compounds

Definitions

  • the present invention relates to a method for decolorizing industrial wastewater such as livestock wastewater, food factory wastewater, dye factory wastewater, etc. More specifically, the present invention relates to a method for decolorizing industrial wastewater that is useful for decolorizing highly colored wastewater such as coffee wastewater.
  • decolorization techniques include biological treatment (biological treatment), ozone ( O3 ) treatment, sodium hypochlorite treatment, electrolysis, and precipitation treatment by adding a coagulant.
  • biological treatment may not be effective enough in reducing color
  • ozone treatment and electrolysis require a large initial investment to achieve a sufficient color reduction effect.
  • sodium hypochlorite treatment has a high decolorization effect, but it has high running costs, has a negative effect on activated sludge treatment, and also contaminates the treated water with chlorine, which has a negative effect on fish in rivers and the like.
  • Patent Document 1 a method for decolorization of livestock wastewater (Patent Document 1) is known, which includes adding an iron-based flocculant to livestock wastewater, flocculating suspended matter and coagulating soluble coloring matter to perform primary decolorization treatment, treating the treated liquid with a solid-liquid separation method such as sedimentation separation or filtration to make it clear, and then performing secondary decolorization treatment with ultraviolet light including natural light or ultraviolet light and a photocatalyst.
  • Patent Document 1 includes adding an iron-based flocculant to livestock wastewater, flocculating suspended matter and coagulating soluble coloring matter to perform primary decolorization treatment, treating the treated liquid with a solid-liquid separation method such as sedimentation separation or filtration to make it clear, and then performing secondary decolorization treatment with ultraviolet light including natural light or ultraviolet light and a photocatalyst.
  • a water treatment method (Patent Document 2) is characterized in that three types of chemicals, at least one of soluble aluminum salts or soluble iron salts, an arbitrary amount of alkali metal carbonate, and an arbitrary amount of a reaction moderator, are administered to the liquid to be treated and stirred at approximately the same time to flocculate, decolorize, and/or desalt suspended matter in the treated liquid.
  • a method for treating a dye- or pigment-containing liquid (Patent Document 3) is known, which includes adding a treatment agent containing one or more inorganic flocculants or polymer flocculants to the dye- or pigment-containing liquid.
  • any of these methods adequately balances the cost of the decolorization treatment with the decolorization effect, and it is necessary to find a better method.
  • the Ministry of the Environment has set a uniform discharge standard for the phosphorus content of wastewater discharged into the environment at 16 mg/L (daily average 8 mg/L) or less in order to prevent eutrophication of lakes, ponds, and coastal seas.
  • a livestock wastewater treatment device which comprises a pretreatment tank which mainly performs solid-liquid separation, a first digestion tank which mainly performs acidic fermentation and alkaline fermentation, a second digestion tank which also performs acidic fermentation and alkaline fermentation and has a contact material installed inside, a digestion filter tank which decomposes nitrate nitrogen with anaerobic bacteria and removes suspended matter and particles, and a soil treatment tank which has an infiltrative member buried in breathable soil, arranged in this order, and which is characterized by having a floating impeller installed in the second digestion tank (Patent Document 4).
  • biological treatments such as acid fermentation and alkaline fermentation require frequent maintenance to adjust to optimal treatment conditions.
  • JP 2010-201279 A Japanese Patent Application Laid-Open No. 2-099185 Japanese Patent Application Laid-Open No. 11-276809 JP 2002-45885 A
  • the objective of the present invention is to provide a method for efficiently decolorizing colored industrial wastewater.
  • the inventors discovered that the coloring of the first supernatant liquid obtained by mixing an iron-based inorganic flocculant and a cationic polymer flocculant and then performing solid-liquid separation can be significantly reduced by adjusting the pH of the first supernatant liquid to a predetermined range and then adding an iron-based inorganic flocculant and a cationic polymer flocculant again, and thus completed the present invention.
  • the gist of the present invention is [1] A method for decolorizing industrial wastewater, comprising the steps of: a first precipitation treatment step in which an iron-based inorganic flocculant and a cationic polymer flocculant are mixed with the industrial wastewater, followed by solid-liquid separation to extract a first supernatant liquid; an alkali treatment step of mixing an alkaline agent with the first supernatant to adjust the pH of the first supernatant to 8 or more; a second precipitation treatment step of mixing an iron-based inorganic flocculant with the pH-adjusted first supernatant, then mixing an alkaline agent to adjust the pH to 6 or more, then mixing a cationic polymer flocculant therewith, and subjecting the mixture to solid-liquid separation to extract a second supernatant, said second precipitation treatment step comprising the steps of: [2] The method for decolorizing industrial wastewater according to [1], wherein the iron-based inorganic flocculant is ferrous chloride, ferr
  • the present invention makes it possible to efficiently decolorize industrial wastewater such as livestock wastewater, food factory wastewater, and dye factory wastewater.
  • the present invention can reduce impurities, such as phosphorus, in the industrial wastewater, so that even if the decolorized industrial wastewater is discharged into the environment, the impact on the environment can be significantly reduced.
  • the method for decolorizing industrial wastewater comprises the steps of: a first precipitation treatment step in which an iron-based inorganic flocculant and a cationic polymer flocculant are mixed with the industrial wastewater, followed by solid-liquid separation to extract a first supernatant liquid; an alkali treatment step of mixing an alkaline agent with the first supernatant to adjust the pH of the first supernatant to 8 or more;
  • the method is characterized by having a second precipitation treatment step in which an iron-based inorganic flocculant is mixed with the pH-adjusted first supernatant liquid, an alkaline agent is then added to adjust the pH to 6 or more, a cationic polymer flocculant is then added, and a second supernatant liquid is taken out by solid-liquid separation.
  • the industrial waste liquid refers to colored waste liquid discharged from industrial sites such as livestock farms, food factories, dye factories, etc.
  • Livestock wastewater refers to wastewater containing excrement and the wastewater from washing it, discharged from livestock farms that breed, raise or fatten livestock such as cows, pigs, horses, sheep, and goats, and poultry such as chickens, ducks, and quails.
  • Food factory wastewater refers to wastewater discharged during the food manufacturing process in various food factories, including beverages, dairy products, confectioneries, grain products, sweeteners, spices, brewed foods, fresh foods, meat products, and fish and marine products.
  • Dye factory effluent refers to effluent discharged from dye factories.
  • the industrial wastewater contains various impurities such as organic and inorganic substances, and it is generally required to reduce the concentration of impurities in the industrial wastewater to a predetermined value by precipitation treatment or the like before discharging the industrial wastewater into the environment.
  • the industrial waste liquid used in the present invention includes not only colored raw waste liquid, but also colored waste liquid that has been treated to reduce the concentration of impurities, and colored waste liquid obtained by concentrating and dehydrating sludge separated from raw waste liquid.
  • the degree of color of the industrial wastewater may be, for example, 600 degrees or more when measured based on the transmitted light measurement method in Section 2, Chapter 2, Section 4, Paragraph 2 of the Sewage Testing Methods.
  • This step is a step for precipitating and removing impurities such as organic matter and inorganic matter in the industrial wastewater using an iron-based inorganic flocculant and a cationic polymer flocculant, and recovering a first supernatant liquid.
  • the iron-based inorganic flocculants include ferrous chloride, ferric chloride, polyferric sulfate, etc.
  • the iron-based inorganic flocculants may be used alone or in combination of two or more kinds.
  • the amount of the iron-based inorganic coagulant to be mixed with the industrial wastewater may be appropriately determined depending on the type of industrial wastewater to be treated, and is not particularly limited. From the viewpoint of high impurity removal effect, the amount is preferably 100 mg/L or more, more preferably 300 mg/L or more, and even more preferably 500 mg/L or more. From the viewpoint of excellent economy, the amount is preferably 10,000 mg/L or less, more preferably 5,000 mg/L or less, and even more preferably 2,000 mg/L or less.
  • the cationic polymer flocculant is used to make the flocculants formed by using the iron-based inorganic flocculant larger and to facilitate precipitation.
  • the cationic polymer flocculant may be an acrylic or methacrylic cationic polymer flocculant.
  • the acrylic polymer flocculant include Mannich modified polyacrylamide.
  • the methacrylic polymer flocculant include homopolymers of cationic methacrylic acid ester compounds, quaternary salts thereof, and copolymers of acrylamide and cationic methacrylic acid ester compounds.
  • the cationic polymer flocculants may be used alone or in combination of two or more kinds.
  • the amount of the cationic polymer flocculant to be mixed with the industrial wastewater may be appropriately determined depending on the type of industrial wastewater to be treated, the type of iron-based inorganic flocculant to be used in combination, etc., and is not particularly limited. From the viewpoint of high impurity removal effect, it is preferably 10 mg/L or more, and more preferably 20 mg/L or more, and from the viewpoint of excellent economy, it is preferably 200 mg/L or less, and more preferably 100 mg/L or less.
  • the method of solid-liquid separation in this process may be any method commonly used for industrial wastewater, and is not particularly limited, but examples include coagulation sedimentation, filtration, centrifugation, squeezing, membrane separation, etc.
  • the first supernatant contains dissolved iron-based inorganic flocculants and cationic polymer flocculants, so its pH is adjusted to 5 or less, making it an acidic solution.
  • the first supernatant liquid has fewer impurities than the industrial wastewater used as the raw material for treatment, making it a colored liquid with reduced chromaticity.
  • Alkaline treatment step This step is a step of adjusting the pH of the first supernatant to 8 or more using an alkaline agent. By carrying out the alkaline treatment and the subsequent second precipitation treatment in this manner, it is possible to facilitate aggregation of the colored components in the first supernatant.
  • the alkaline agent is not particularly limited, but examples thereof include sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, and the like.
  • the type and amount of the alkaline agent are not particularly limited as long as they can adjust the pH of the first supernatant to 8 or higher.
  • This process is a process in which an iron-based inorganic flocculant is mixed with the first supernatant liquid adjusted to alkaline as described above, then an alkaline agent is added to adjust the pH to 6 or more, and then a cationic polymer flocculant is added, followed by solid-liquid separation to extract a second supernatant liquid.
  • the iron-based inorganic flocculant used in this step may be any one that can be used in the first precipitation treatment step.
  • the type of iron-based inorganic flocculant used in this step may be the same as or different from that used in the first precipitation treatment step.
  • the amount of the iron-based inorganic flocculant to be mixed with the first supernatant may be appropriately determined depending on the type of industrial wastewater to be treated, and is not particularly limited. From the viewpoint of high effectiveness in removing colored components, the amount is preferably 100 mg/L or more, and more preferably 300 mg/L or more. From the viewpoint of excellent economy, the amount is preferably 10,000 mg/L or less, more preferably 5,000 mg/L or less, and even more preferably 2,000 mg/L or less.
  • the pH of the first supernatant to which the iron-based inorganic flocculant has been added is preferably adjusted to an acidic pH of 5 or less.
  • an alkaline agent is added to the first supernatant.
  • the pH of the first supernatant liquid which has been reduced by adding an iron-based inorganic flocculant, is raised again by adding an alkaline agent, which has the effect of making it easier to precipitate the colored components when a cationic polymer flocculant is added.
  • the alkaline agent used in this step may be any agent that can be used in the alkaline treatment step.
  • the type of alkaline agent used in this step may be the same as or different from that used in the alkaline treatment step.
  • the type and amount of the alkaline agent should be sufficient to adjust the pH of the first supernatant to 6 or higher.
  • the cationic polymer flocculant used in this step may be any one that can be used in the first precipitation treatment step.
  • the type of cationic polymer flocculant used in this step may be the same as or different from that used in the first precipitation treatment step.
  • the amount of the cationic polymer flocculant to be mixed with the first supernatant may be appropriately determined depending on the type of industrial wastewater to be treated, the type of iron-based inorganic flocculant to be used in combination, etc., and is not particularly limited. From the viewpoint of high effectiveness in removing colored components, the amount is preferably 10 mg/L or more, and more preferably 20 mg/L or more, and from the viewpoint of excellent economy, the amount is preferably 200 mg/L or less, and more preferably 100 mg/L or less.
  • the method of solid-liquid separation in this step is not particularly limited as long as it is a method that can be used in the first precipitation treatment step.
  • the second supernatant liquid obtained in this process is a liquid in which the degree of coloration has been significantly reduced; for example, when measuring the chromaticity, it is possible to reduce the chromaticity of even coffee waste liquid to less than 140 degrees.
  • the second supernatant liquid is a liquid that can be discharged into the environment more safely because the content of coloring components has been significantly reduced in addition to impurities.
  • the stirring conditions may be performed at room temperature, and there are no particular limitations on the stirring speed, etc.
  • the solid matter separated by the method of the present invention can be disposed of according to conventional methods.
  • the method of the present invention has the advantages of being simple and economical in that the coloring components can be significantly reduced from industrial wastewater by repeatedly performing solid-liquid separation using an iron-based inorganic flocculant and a cationic polymer flocculant while adjusting the pH conditions, without using other treatments such as biological treatment. Furthermore, the method of the present invention can reduce impurities in the industrial wastewater, such as phosphorus, in addition to the coloring components, so that even if the decolorized treatment liquid is discharged into the environment, the impact on the environment can be significantly reduced.
  • Example 1 Method for decolorizing livestock wastewater
  • effluent obtained by treating livestock wastewater with activated sludge was used as raw water.
  • the raw water was a brown liquid with a pH of 7.1 (color index: 850 degrees).
  • the degree of light yellow to yellowish brown color of the sample was measured by absorptiometry using a spectrophotometer (Shimadzu Corporation, UV-1800) based on the transmitted light measurement method described in Section 4, Chapter 2, Part 2 of the Sewage Testing Methods.
  • the absorbance at around 390 nm was measured.
  • the chromaticity was measured according to the following procedure. (Test method) The sample is filtered through filter paper type 5C or a filter material with a pore size of 1 ⁇ m or less, or centrifuged at about 3,000 rpm for 20 minutes to remove turbidity.
  • a portion of 100 ml of this sample is placed in an absorption cell (path length 50 nm) and the absorbance at a wavelength of about 390 nm is measured using a spectrophotometer. If the color of the sample is 100 degrees or more, take an appropriate amount of the sample and add water to make it 100 ml. (Creating a calibration curve) Put 1.0 to 100 ml of the color standard solution (100 degrees) into several 100 ml volumetric flasks in stages and add water up to the mark. Then, measure the absorbance in the same manner as in the test procedure, and obtain the relationship between color and absorbance. The quantification range of this method is 0 to 100 degrees, with the minimum unit being 1 degree.
  • Ferric chloride was added to the raw water so as to give a concentration of 536 mg/L, and the mixture was stirred at 500 rpm for 5 minutes (pH 3.0).
  • a cationic polymer flocculant cationic polyacrylamide
  • a concentration of 40 mg/L was added to the solution to give a concentration of 40 mg/L, and the solution was stirred at 250 rpm for 5 minutes.
  • solid-liquid separation was performed using filter paper to obtain a first supernatant liquid (pH 3.0, light brown). The first supernatant was adjusted to pH 10.0 by adding an aqueous solution of sodium hydroxide.
  • ferric chloride was added to the first supernatant to a concentration of 322 mg/L, and the mixture was stirred at 500 rpm for 5 minutes (pH 3.3).
  • an aqueous solution of sodium hydroxide was added to the first supernatant to adjust the pH to 6.7, and the mixture was stirred at 500 rpm for 5 minutes.
  • a cationic polymer flocculant (cationic polyacrylamide) was added to the first supernatant to a concentration of 80 mg/L, and the mixture was stirred at 250 rpm for 5 minutes.
  • solid-liquid separation was performed using filter paper to obtain a second supernatant liquid (pH 6.7, light brown, color degree 75 degrees).
  • the obtained second supernatant liquid had a pH adjusted to approximately neutral and a significantly lower color than the raw water, and could be safely discharged into the environment as is without dilution.
  • the decolorization of the waste liquid as described above can be achieved in a short time, and therefore the decolorization effect is excellent.
  • the decolorization can be carried out by simply adding an iron-based inorganic flocculant and a cationic polymer flocculant, no other special equipment is required, and therefore the decolorization method is simple and has excellent practicality.
  • Example 2 Method for decolorizing wastewater (raw water) from a coffee factory)
  • the raw water used for the food processing plant was wastewater discharged from a coffee factory.
  • the raw water was a black liquid with a pH of 5.8 (color degree 3400 degrees).
  • Ferric chloride was added to the raw water so as to give a concentration of 536 mg/L, and the mixture was stirred at 500 rpm for 5 minutes (pH 4.5).
  • a cationic polymer flocculant (cationic polyacrylamide) was added to the solution so as to give a concentration of 40 mg/L, and the solution was stirred at 250 rpm for 5 minutes.
  • solid-liquid separation was performed using filter paper to obtain a first supernatant liquid (pH 4.5, pale green).
  • an aqueous solution of sodium hydroxide was added to the first supernatant to adjust the pH to 8.4.
  • ferric chloride was added to the first supernatant to a concentration of 322 mg/L, and the mixture was stirred at 500 rpm for 5 minutes (pH 6.0).
  • an aqueous solution of sodium hydroxide was added to the first supernatant to adjust the pH to 7.0.
  • a cationic polymer flocculant (cationic polyacrylamide) was added to the first supernatant to give a concentration of 40 mg/L, and the mixture was stirred at 250 rpm for 5 minutes.
  • solid-liquid separation was performed using filter paper to obtain a second supernatant liquid (pH 7.0, light brown, color degree 130 degrees).
  • the obtained second supernatant liquid had a pH adjusted to near neutral and a significantly lower color value of less than 140 compared to the raw water, and could be safely discharged into the environment as is without dilution.
  • the decolorization of the waste liquid as described above can be achieved in a short time, and therefore the decolorization effect is excellent.
  • the decolorization can be carried out by simply adding an iron-based inorganic flocculant and a cationic polymer flocculant, no other special equipment is required, and therefore the decolorization method is simple and has excellent practicality.
  • Example 3 Method for decolorizing livestock wastewater
  • the colored wastewater discharged from a cowshed was subjected to a general biological treatment, and the raw water was subjected to a decolorization treatment in the same manner as in Example 1.
  • the color and TP (total phosphorus) of the raw water (pH 8.61) and the decolorized water (pH 5.85) are shown in Table 1.
  • the amount of phosphorus was measured as the total phosphorus concentration (T-P) using the potassium peroxodisulfate decomposition method described in the phosphorus measurement method "JIS K 0102-46.3.1.”

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

L'invention concerne un procédé de décoloration de déchets liquides industriels, ledit procédé comprenant : une première étape de traitement de précipitation pour mélanger un floculant inorganique à base de fer et un floculant polymère cationique dans des déchets liquides industriels et mettre en œuvre une séparation solide-liquide afin d'extraire un premier liquide surnageant ; une étape de traitement alcalin pour mélanger un agent alcalin dans le premier liquide surnageant afin d'ajuster le pH du premier liquide surnageant à 8 ou plus ; et une seconde étape de traitement de précipitation pour mélanger un floculant inorganique à base de fer dans le premier liquide surnageant à pH ajusté, puis mélanger un agent alcalin afin d'ajuster le pH à 6 ou plus, puis mélanger un floculant polymère cationique, et mettre en œuvre une séparation solide-liquide afin d'extraire un second liquide surnageant.
PCT/JP2023/033958 2022-10-06 2023-09-19 Procédé de décoloration de déchets liquides industriels WO2024075518A1 (fr)

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JP2022161541 2022-10-06

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54156341A (en) * 1978-05-31 1979-12-10 Ebara Corp Treatment of waste water
JPH0623369A (ja) * 1992-01-27 1994-02-01 Sandoz Ag 使用済水性アルミニウム液の廃棄方法
JPH06165993A (ja) * 1992-08-27 1994-06-14 Shikoku Chem Corp 染料及び染色工業廃水用脱色薬剤並びにその脱色方法
JPH09174061A (ja) * 1995-12-28 1997-07-08 Hodogaya Chem Co Ltd 着色物質含有廃水の処理方法
JP2001269504A (ja) * 2000-03-28 2001-10-02 Nittetsu Mining Co Ltd 新規の凝集剤及びその製造方法
JP2008055277A (ja) * 2006-08-30 2008-03-13 Konica Minolta Business Technologies Inc 着色排水の脱色方法
JP2011050900A (ja) * 2009-09-03 2011-03-17 Fuji Xerox Co Ltd 水処理装置および水処理方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54156341A (en) * 1978-05-31 1979-12-10 Ebara Corp Treatment of waste water
JPH0623369A (ja) * 1992-01-27 1994-02-01 Sandoz Ag 使用済水性アルミニウム液の廃棄方法
JPH06165993A (ja) * 1992-08-27 1994-06-14 Shikoku Chem Corp 染料及び染色工業廃水用脱色薬剤並びにその脱色方法
JPH09174061A (ja) * 1995-12-28 1997-07-08 Hodogaya Chem Co Ltd 着色物質含有廃水の処理方法
JP2001269504A (ja) * 2000-03-28 2001-10-02 Nittetsu Mining Co Ltd 新規の凝集剤及びその製造方法
JP2008055277A (ja) * 2006-08-30 2008-03-13 Konica Minolta Business Technologies Inc 着色排水の脱色方法
JP2011050900A (ja) * 2009-09-03 2011-03-17 Fuji Xerox Co Ltd 水処理装置および水処理方法

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