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CN109455842A - A kind of efficient decolorizing technique of the organic solvent containing dyestuff - Google Patents

A kind of efficient decolorizing technique of the organic solvent containing dyestuff Download PDF

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Publication number
CN109455842A
CN109455842A CN201811343961.7A CN201811343961A CN109455842A CN 109455842 A CN109455842 A CN 109455842A CN 201811343961 A CN201811343961 A CN 201811343961A CN 109455842 A CN109455842 A CN 109455842A
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Prior art keywords
organic solvent
colloid
dyestuff
technique
decoloration
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CN201811343961.7A
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CN109455842B (en
Inventor
陈新福
陈玉洪
左小新
李志强
张玉高
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Guangdong Esquel Textiles Co Ltd
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Guangdong Esquel Textiles Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/38Treatment of water, waste water, or sewage by centrifugal separation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F2001/007Processes including a sedimentation step
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents

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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)
  • Coloring (AREA)
  • Removal Of Specific Substances (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The present invention provides a kind of efficient decolorizing technique of organic solvent containing dyestuff, which stirs evenly, obtains flocculation decoloration colloid the following steps are included: (1) is soluble in water by inorganic metal salt and inorganic base;(2) under agitation, the flocculation decoloration colloid is added in the organic solvent containing dyestuff, so that the flocculation decoloration colloid inhales color precipitating.The technique prepares flocculation decoloration colloid by the way of mixing inorganic metal salt compounding inorganic base, and using the dyestuff in the charge attraction flocculation organic solvent between the flocculation decoloration colloid and dyestuff, flocculent gel natural subsidence under the effect of gravity completes the decoloration of solvent;In conjunction with the filters pressing and drying of clay, the percent of decolourization of the organic solvent containing dyestuff is up to 90% or more (90-98%), and the rate of recovery of organic solvent is close to 100%.The technological operation provided by the present invention is simple, and process energy conservation environmental protection, material is cheap and easy to get, is conducive to industrialization promotion.

Description

A kind of efficient decolorizing technique of the organic solvent containing dyestuff
Technical field
The present invention relates to a kind of efficient decolorizing techniques of organic solvent containing dyestuff, belong to dyeing and finishing technique field.
Background technique
Textile printing and dyeing industry is that water consumption is big, one of the industrial department that discharge of wastewater is more.According to statistics, China's printing and dyeing enterprise The wastewater flow rate discharged daily is up to 3,000,000-400 ten thousand tons, and the wherein high chroma, high organic content of generation during dyeing Dyeing waste-water accounting is maximum.The reason is that inevitably causing hydrolysis situation in dyestuff water-bath dyeing course, leading to 30%- 50% dyestuff remains in dyeing waste-water.These dyeing waste-waters either pollution level or processing difficulty is all higher, is current Perplex a great problem of dyeing development.
With the gradually reinforcement of the environmental regulation increasingly in short supply and domestic and international, environmental consciousness of water resource, dyeing waste water is reduced It generates, develops non-aqueous media dyeing, become a general orientation of textile industry industrial transformation.Wherein critical carbon dioxide dyeing and it is non- Aqueous solvent dyeing is two general orientation of non-aqueous media dyeing: critical carbon dioxide, which dyes, at home and abroad has more research, but by In thering is larger limitation and dyeing installation operation to need super-pressure dyestuff used and contaminated fiber, lead to answering for the technology It can not be promoted with range, industrialization process is slow;Non-aqueous media solvent dyeing is primarily referred to as that solvent is used to substitute water as dyeing Medium, avoids the hydrolysis of dyestuff in dyeing course, to realize the high usage of dyestuff and the high colour-fast rate of fabric.Due to dye Water is not used during color, and dyes and finishes nonaqueous solvents whole recycling and reusing, so in the process without dyeing waste-water, waste liquid It generates.
17 unit consolidations such as Yida Textile Co., Ltd and Zhejiang University assume responsibility for " the crucial skill of non-aqueous media dyeing Art research and production demonstration " state key researches and develops planning item, and wherein Yida Textile Co., Ltd is responsible for the " pole of exploitation Property/nonpolarity binary non-aqueous media dyeing key technology " come into the industrialization propulsion phase.Solvent after the completion of dyeing returns Find although dyes utilization rate is more than 95%, but still there is a small amount of dyestuff to remain in dicyandiamide solution in receipts.Residual dye pair Solvent recovery recycles and dyeing cycle stability, all causes to seriously affect, needs to try to remove.
Existing solvent decoloration recovery process mainly has extraction, rectification method, film filtering etc., there are certain drawbacks: Extraction is used in a solvent, and dyestuff, still with a certain concentration than being distributed, can not be removed efficiently, and commonly use organic in the mixed solvent Extractant cannot be separated from solvent completely, to become new impurity, increase the difficulty of solvent recovery;Rectification method can be complete Full removal dyestuff, but heating expends mass energy in the process, and the rate of recovery of equipment can not break through 95% at present, and solvent loss is not Only economic cost is caused to increase, also results in environmental pollution;The film of organic solvent is filtered usually using inorganic ceramic membrane, dyestuff Grain be easy to cause Pore Blocking, and film backwash and regeneration difficulty is big, and dye particle used in dyeing course differs greatly, mixing The film that dyestuff is not available single aperture efficiently removes.
The removal of residual dye in dyeing solvent becomes a great problem for hindering non-aqueous media solvent dyeing development.This hair Bright content is intended to develop a kind of efficient decolorizing technique to the organic solvent containing dyestuff, solves the decoloration in solvent recovery process Problem.
Summary of the invention
In order to solve the above shortcomings and deficiencies, the purpose of the present invention is to provide a kind of height of organic solvent containing dyestuff Imitate decoloration process.
In order to achieve the above objectives, the present invention provides a kind of efficient decolorizing technique of organic solvent containing dyestuff, wherein described Technique the following steps are included:
(1) inorganic metal salt and inorganic base is soluble in water, it stirs evenly, obtains flocculation decoloration colloid;
(2) under agitation, the flocculation decoloration colloid is added in the organic solvent containing dyestuff, so that the wadding Solidifying decoloration colloid inhales color precipitating.
Specific embodiment according to the present invention, this contains the efficient decolorizing technique of the organic solvent of dyestuff further include: to step (2) acquired solution is stood or is centrifuged.
Wherein, stand or centrifugally operated purpose be separation flocculation decoloration colloid inhale color precipitating after gained precipitating clay and on Clear liquid.
Specific embodiment according to the present invention, this contains the efficient decolorizing technique of the organic solvent of dyestuff further include: to step (2) acquired solution is filtered to separate gained after flocculation decoloration colloid inhales color precipitating and precipitate clay and supernatant, then heavy to this Shallow lake clay carries out filters pressing and drying, and carries out condensing recovery to steam obtained by drying course.
Specific embodiment according to the present invention, it is described organic in the efficient decolorizing technique of the organic solvent containing dyestuff Solvent include N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, ionic liquid, alcohol ether solvents, alkane, Combination containing one or more of chloro-alkenes, aromatic hydrocarbons, ketone, esters, ethers and alcohols;
Preferably, the alkane includes containing enpara.
Specific embodiment according to the present invention, in the efficient decolorizing technique of the organic solvent containing dyestuff, with organic molten The total volume of agent is calculating benchmark, and the concentration of dyestuff is 0.01-10g/L in the organic solvent containing dyestuff.
Specific embodiment according to the present invention, it is described inorganic in the efficient decolorizing technique of the organic solvent containing dyestuff Metal salt includes the combination of one or more of molysite, ferrous salt, magnesium salts and mantoquita;
Preferably, the inorganic metal salt includes Fe2(SO4)3、FeCl3、FeSO4、FeCl2、MgSO4、MgCl2One of Or several combination.
Specific embodiment according to the present invention, in the efficient decolorizing processing step (1) of the organic solvent containing dyestuff, institute It is 6.5-7.5 with the pH value of water.
Specific embodiment according to the present invention, in the efficient decolorizing technique of the organic solvent containing dyestuff, with the water Total volume be calculating benchmark, the dosage of the inorganic metal salt is 10-200g/L.
Specific embodiment according to the present invention, it is described inorganic in the efficient decolorizing technique of the organic solvent containing dyestuff Alkali includes Na2CO3、NaOH、K2CO3、KOH、CaCO3And Ca (OH)2One or more of combination.
Specific embodiment according to the present invention, in the efficient decolorizing technique of the organic solvent containing dyestuff, with the water Total volume be calculating benchmark, the dosage of the inorganic base is 5-100g/L.
Specific embodiment according to the present invention, in the efficient decolorizing processing step (2) of the organic solvent containing dyestuff, often The dosage for rising the corresponding flocculation decoloration colloid of organic solvent containing dyestuff is 5mL-150mL.
It is provided by the present invention this contain the organic solvent of dyestuff efficient decolorizing technique it is pre- by using a small amount of water first Flocculation decoloration colloid is produced, and controls the charge ratio of flocculation decoloration colloid (the application mainly passes through inorganic metal salt and inorganic The usage ratio of alkali adjusts the charge ratio of control flocculation decoloration colloid, secondly also needs water used in material in rate-determining steps (1) Acid-base property close to neutrality, i.e., the pH value of water used is 7 or so), then directly distributed it under mechanical agitation containing dye In the organic solvent of material.Wherein, prefabricated flocculation decoloration colloid has had charge neutrality property, prints and dyes in the prior art without experience The generating process of hydroxide metal ion in wastewater treatment process;Further, since the aquation of colloid, is dispersed in organic molten Colloid in agent carries certain density moisture, and mechanical stirring is carried out during charging, this part water entrained by colloid Ionize the dyestuff close to colloidal dispersion, charge neutrality absorption occurs for colloid and dyestuff at this time, completes the decoloration of solvent.
Provided by the present invention this contains the efficient decolorizing technique of the organic solvent of dyestuff using mixing inorganic metal salt compounding The mode of inorganic base prepares flocculation decoloration colloid, utilizes the charge attraction flocculation organic solvent between the flocculation decoloration colloid and dyestuff In dyestuff, flocculent gel natural subsidence under the effect of gravity completes the decoloration of solvent;In conjunction with the filters pressing and drying of clay, containing dye The percent of decolourization of the organic solvent of material is up to 90% or more (90-98%), and the rate of recovery of organic solvent is close to 100%.Institute of the present invention The technological operation provided is simple, and process energy conservation environmental protection, material is cheap and easy to get, is conducive to industrialization promotion.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now in conjunction in detail below Embodiment carries out following detailed description to technical solution of the present invention, but should not be understood as the limit to enforceable range of the invention It is fixed.
Embodiment 1
Present embodiments provide a kind of efficient decolorizing technique of organic solvent containing dyestuff, wherein the technique includes following Step:
4g FeCl is weighed respectively2、6g MgCl2、2g MgSO4It with 4g KOH, is dissolved in 140mL water, stirs evenly, be made Flocculation decoloration colloid;
The dyeing residual solvent that measurement 3L Yellow containing L-Brilliant CA dye strength is 0.5g/L, mechanical stirring, It is slowly uniformly added into made flocculation decoloration colloid, persistently stirs 30min, stands for 24 hours, filters out supernatant and clay, clay filters pressing Solid content is 30% afterwards, dries clay condensing recovery steam;Whole solvents are collected, dye strength is reduced to 0.01g/L, containing dyestuff The percent of decolourization of organic solvent is up to 98%;Removal introduce water, recycling design total amount (after supernatant, clay filters pressing gained liquid and The total amount of the condensed liquid of steam) it is 2.97L, the rate of recovery of organic solvent is 99.0%.
Embodiment 2
Present embodiments provide a kind of efficient decolorizing technique of organic solvent containing dyestuff, wherein the technique includes following Step:
4g FeCl is weighed respectively2、8g MgCl2It with 4g NaOH, is dissolved in 160mL water, stirs evenly obtained flocculation decoloration Colloid;
The dyeing residual solvent that 3L Red containing SE dye strength is 0.6g/L is measured, mechanical stirring is slowly uniformly added into institute Flocculation decoloration colloid processed persistently stirs 30min, stands for 24 hours, filters out supernatant and clay, and solid content is 35% after clay filters pressing, Dry clay condensing recovery steam;Whole solvents are collected, dye strength is reduced to 0.01g/L, the decoloration of the organic solvent containing dyestuff Rate is up to 98.3%;Removal introduces water, and recycling design total amount is 2.98L, and the rate of recovery of organic solvent is 99.3%.
Embodiment 3
Present embodiments provide a kind of efficient decolorizing technique of organic solvent containing dyestuff, wherein the technique includes following Step:
8g FeCl is weighed respectively2、4g MgCl2、2g MgSO4It with 5g NaOH, is dissolved in 160mL water, stirs evenly obtained Flocculation decoloration colloid;
The dyeing residual solvent that 3L Supra containing Sumifix Br.Red 3BF dye strength is 3g/L is measured, machinery stirs It mixes, is slowly uniformly added into made flocculation decoloration colloid, persistently stir 30min, stand 48h, filter out supernatant and clay, clay pressure Solid content is 20% after filter, dries clay condensing recovery steam;Whole solvents are collected, dye strength is reduced to 0.05g/L, contains dyestuff Organic solvent percent of decolourization up to 98.3%;Removal introduces water, and recycling design total amount is 2.95L, the rate of recovery of organic solvent It is 98.3%.
Embodiment 4
Present embodiments provide a kind of efficient decolorizing technique of organic solvent containing dyestuff, wherein the technique includes following Step:
2g Fe is weighed respectively2(SO4)3、6g MgCl2、2g MgSO4With 3g NaOH, 3gKOH, it is dissolved in 120mL water, stirs Mix uniformly obtained flocculation decoloration colloid;
The dyeing residual solvent that 3L Blue containing EVERZOL LX dye strength is 0.5g/L is measured, mechanical stirring is slowly equal It is even that made flocculation decoloration colloid is added, 30min is persistently stirred, stands for 24 hours, filters out supernatant and clay, containing solid after clay filters pressing Amount is 35%, dries clay condensing recovery steam;Whole solvents are collected, dye strength is reduced to 0.01g/L, organic molten containing dyestuff The percent of decolourization of agent is up to 98%;Removal introduces water, and recycling design total amount is 2.98L, and the rate of recovery of organic solvent is 99.3%.
The present invention is described by way of example above, but the present invention is not limited to examples detailed above, as long as being based on this hair Any changes or modifications that bright content is done belong to present invention content claimed.

Claims (10)

1. a kind of efficient decolorizing technique of the organic solvent containing dyestuff, which is characterized in that the technique the following steps are included:
(1) inorganic metal salt and inorganic base is soluble in water, it stirs evenly, obtains flocculation decoloration colloid;
(2) under agitation, the flocculation decoloration colloid is added in the organic solvent containing dyestuff, so that the flocculation is de- Coloring agent body inhales color precipitating.
2. technique according to claim 1, which is characterized in that the technique further include: carried out to step (2) acquired solution quiet It sets or is centrifuged.
3. technique according to claim 2, which is characterized in that the technique further include: carried out to step (2) acquired solution Filter precipitates clay and supernatant to separate gained after flocculation decoloration colloid inhales color precipitating, then carries out filters pressing and baking to the precipitating clay It is dry, and condensing recovery is carried out to steam obtained by drying course.
4. technique according to claim 1-3, which is characterized in that the organic solvent includes N, N- dimethyl methyl Amide, dimethyl sulfoxide, ionic liquid, alcohol ether solvents, alkane, contains chloro-alkenes, aromatic hydrocarbons, ketone, ester at DMAC N,N' dimethyl acetamide The combination of one or more of class, ethers and alcohols;
Preferably, the alkane includes containing enpara.
5. technique according to claim 1-3, which is characterized in that with the total volume of organic solvent be calculate base Standard, the concentration of dyestuff is 0.01-10g/L in the organic solvent containing dyestuff.
6. technique according to claim 1-3, which is characterized in that the inorganic metal salt includes molysite, ferrous iron The combination of one or more of salt, magnesium salts and mantoquita;
Preferably, the inorganic metal salt includes Fe2(SO4)3、FeCl3、FeSO4、FeCl2、MgSO4、MgCl2One of or it is several The combination of kind;
It is further preferred that the pH value of water used is 6.5-7.5 in step (1).
7. technique according to claim 1-3, which is characterized in that using the total volume of the water as calculating benchmark, The dosage of the inorganic metal salt is 10-200g/L.
8. technique according to claim 1-3, which is characterized in that the inorganic base includes Na2CO3、NaOH、 K2CO3、KOH、CaCO3And Ca (OH)2One or more of combination.
9. technique according to claim 1-3, which is characterized in that using the total volume of the water as calculating benchmark, The dosage of the inorganic base is 5-100g/L.
10. technique according to claim 1-3, which is characterized in that in step (2), containing dyestuff described in every liter The dosage of the corresponding flocculation decoloration colloid of organic solvent is 5mL-150mL.
CN201811343961.7A 2018-11-13 2018-11-13 Efficient decoloring process for dye-containing organic solvent Active CN109455842B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112499853A (en) * 2020-10-23 2021-03-16 广东溢达纺织有限公司 Method for recycling hydrolyzed dye in dyeing wastewater

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1336335A (en) * 2000-07-29 2002-02-20 詹伯君 Decoloring coagulant of composite iron salt
CN1792853A (en) * 2005-11-17 2006-06-28 上海交通大学 Combined treating process for waste water of basic printing and dyeing
JP2011016048A (en) * 2009-07-07 2011-01-27 Act Co Ltd Method of decoloring and purifying wastewater containing lignin and/or tannin
JP4840330B2 (en) * 2006-11-14 2011-12-21 コニカミノルタビジネステクノロジーズ株式会社 Decolorization method for colored wastewater
CN104724863A (en) * 2015-03-27 2015-06-24 达州军华环保科技有限公司 Novel efficient flocculating decolorization method
CN104787864A (en) * 2015-03-30 2015-07-22 湖南科技大学 Preparation method of composite decoloring flocculant for printing and dyeing wastewater treatment
CN108083483A (en) * 2016-11-19 2018-05-29 湖南唯美环境工程股份有限公司 A kind of papermaking or the decoloration treatment method of dyeing waste water
CN108147516A (en) * 2018-01-12 2018-06-12 常州华禹环保科技有限公司 Handle composite flocculation agent of dyeing waste water and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1336335A (en) * 2000-07-29 2002-02-20 詹伯君 Decoloring coagulant of composite iron salt
CN1792853A (en) * 2005-11-17 2006-06-28 上海交通大学 Combined treating process for waste water of basic printing and dyeing
JP4840330B2 (en) * 2006-11-14 2011-12-21 コニカミノルタビジネステクノロジーズ株式会社 Decolorization method for colored wastewater
JP2011016048A (en) * 2009-07-07 2011-01-27 Act Co Ltd Method of decoloring and purifying wastewater containing lignin and/or tannin
CN104724863A (en) * 2015-03-27 2015-06-24 达州军华环保科技有限公司 Novel efficient flocculating decolorization method
CN104787864A (en) * 2015-03-30 2015-07-22 湖南科技大学 Preparation method of composite decoloring flocculant for printing and dyeing wastewater treatment
CN108083483A (en) * 2016-11-19 2018-05-29 湖南唯美环境工程股份有限公司 A kind of papermaking or the decoloration treatment method of dyeing waste water
CN108147516A (en) * 2018-01-12 2018-06-12 常州华禹环保科技有限公司 Handle composite flocculation agent of dyeing waste water and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112499853A (en) * 2020-10-23 2021-03-16 广东溢达纺织有限公司 Method for recycling hydrolyzed dye in dyeing wastewater

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