CN1251973C - Method of treating reduction water of DSD acid producing process by ion exchange adsoption - Google Patents

Method of treating reduction water of DSD acid producing process by ion exchange adsoption Download PDF

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Publication number
CN1251973C
CN1251973C CN 200410020217 CN200410020217A CN1251973C CN 1251973 C CN1251973 C CN 1251973C CN 200410020217 CN200410020217 CN 200410020217 CN 200410020217 A CN200410020217 A CN 200410020217A CN 1251973 C CN1251973 C CN 1251973C
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China
Prior art keywords
waste water
resin
reducing waste
dsd acid
basic anion
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Expired - Fee Related
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CN 200410020217
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Chinese (zh)
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CN1597543A (en
Inventor
张凤宝
柴丽敏
张国亮
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Tianjin University
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Tianjin University
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  • Treatment Of Water By Ion Exchange (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The present invention discloses a method for reducing waste water in the production of DSD acid in an ion exchange adsorption treatment method, which belongs to a polluted water treatment technology for producing DSD acid. The method comprises the procedures: DSD acid is filtered for recovering suspended DSD acid in waste water by reducing waste water; the pH value of reduced waste water is regulated to 4 to 6 by base; adsorption operation is carried out to treated reduced waste water through a bed filled with macroporous weak basic anion-exchange resin; elution and regeneration are carried out to macroporous weak basic anion-exchange resin with sodium hydroxide solution. The present invention has the advantages of favourable removing effect of the COD<Cr> and the chromaticity of treated reduced waste water, low treatment cost, simple device and technology and convenient operation.

Description

The method of the reducing waste water in the ion-exchange absorption process for producing DSD acid process
Technical field
The present invention relates to the method for the reducing waste water in a kind of ion-exchange absorption process for producing DSD acid process, belong to the polluted water treatment technology of producing DSD acid.
Background of invention
4,4 '-diaminobenzil-2,2 '-disulfonic acid are called for short DSD acid (molecular formula C 14H 14N 2O 6S 2) be important dyestuff intermediate, be yellow needle-like water absorbability crystal, industrial goods are light yellow paste or Powdered thing, its production technique comprises three operations: the para-nitrotoluene sulfonation prepares sodium p-nitrotoluene-2-sulfonic acid (NTS), NTS prepares 4 with atmospheric oxidation in alkaline aqueous medium or in the alkaline organic medium, 4 '-dinitrobenzene toluylene-2,2 '-disulfonic acid (DNS), DNS prepares DSD acid with iron powder reducing.Except that the sulfonation operation produces concentration is the sulfur waste acid of 50-55%, and oxidation operation and reduction operation all produce a large amount of trade effluents.In reducing waste water, except that containing certain density DSD acid, DNS, 2-sulfonic group-organic impuritys such as 4-benzaminic acid, also contain higher inorganic salt (about 4%).Because the organism in the reducing waste water all has sulfonic group, water-soluble better, thereby conventional coagulating/flocculating method for processing poor effect; Because the organism in the reducing waste water all has nitro, and toxicity is stronger, the salts contg of waste water is higher in addition, thereby biodegradability is relatively poor, is one of more unmanageable industrial organic waste water again.Domestic improvement technology for this waste water is to add flocculation agents such as quaternary ammonium salt, molysite, aluminium salt and polyacrylamide to carry out flocculation decoloration in waste water at present, adopt sedimentation, air supporting or press filtration to carry out mud-water separation then, water outlet is discharged behind sorbing material such as charcoal absorption or thin up.Its main drawback is a wastewater treatment expense height, and the phenyl amines pollutants removal rate is low, and chromophoric group destroys not exclusively, and treat effluent is easily returned look maybe need waste a large amount of precious water resource.
Summary of the invention
The object of the present invention is to provide the method for the reducing waste water in a kind of ion-exchange absorption process for producing DSD acid process, this treatment process expense is low, effective.
The present invention takes following technical scheme to be realized, the method for the reducing waste water in a kind of ion-exchange absorption process for producing DSD acid process is characterized in that may further comprise the steps:
1, the millipore filter with aperture 30-200 μ m filters the DSD acid that the reducing waste water recovery wherein suspends.
2, the initial pH value of the reducing waste water of step 1 being handled with alkali transfers to 4-6, and keeps room temperature.
3, the reducing waste water that step 2 is handled carries out adsorption operations by the bed that is filled with macroporous weakly basic anion exchange resin.
4, with mass concentration be the sodium hydroxide solution of 4.0-8.0%, at room temperature, macroporous weakly basic anion exchange resin carried out wash-out after, 3 pairs of next batch reducing waste waters carry out adsorption operations set by step again.
Above-mentioned macroporous weakly basic anion exchange resin is homemade D301 resin, D370 resin, D380 resin, or in the Amberlite series of producing by U.S. Rohm-Haas company with homemade D301 resin, D370 resin, macroporous weakly basic anion exchange resin that the D380 resin is corresponding.
The alkali of above-mentioned steps 2 is sodium hydroxide solution or particle, potassium hydroxide solution or particle.
Adopt the technology of the present invention to handle reducing waste water, can make COD in the reducing waste water CrContent is reduced to 100mg/L by 600-700mg/L, and clearance is greater than 74%; Reducing waste water is become near colourless by yellow-green colour, and processing costs is low; Equipment, technology are simple, easy to operate.
Embodiment
Embodiment 1:
Get D301, D370, each 2ml of D380 wet resin adds respectively in the 250ml Erlenmeyer flask, and then adds 200ml DSD acid reducing waste water in each Erlenmeyer flask, at room temperature fully vibrates to balance (about 6h of time).Get liquid phase and survey its COD Cr, being respectively 109mg/L, 124mg/L, 131mg/L, its clearance is respectively 74%, 70.1%, and 68.4%.
Embodiment 2:
With 8ml D301 resin (Chemical Plant of Nankai Univ.'s production) Φ 11 * 250mm glass adsorption column of packing into.Under the room temperature, DSD acid reducing waste water at first filtered with the millipore filter of aperture 30-200 μ m and with sodium hydroxide solution or particle adjust pH to 4-6, then with the flow velocity of 4ml/min by resin bed, the average COD of water outlet CrBe 112mg/L.
As desorbing agent, at room temperature the flow velocity with 4mL/min carries out desorption by resin bed, has realized the effective regeneration of bed with 40ml 1mol/L sodium hydroxide solution.
Embodiment 3:
Change the resin kind, Φ 11 * 250mm glass adsorption column of respectively D370 resin and D380 resin 8ml (Chemical Plant of Nankai Univ.'s production) being packed into.DSD acid reducing waste water at first filtered with the millipore filter of aperture 30-200 μ m and with sodium hydroxide solution or particle adjust pH to 4-6, then at room temperature with the flow velocity of 4ml/min by above two kinds of resin bed, the average COD of water outlet CrBe respectively 133mg/L and 156mg/L.
Embodiment 4:
DSD acid reducing waste water at first filtered with the millipore filter of aperture 30-200 μ m and with sodium hydroxide solution or particle adjust pH to 4-6, then with the flow velocity of 4mL/min by among the embodiment 2 desorption and regeneration the D301R resin bed, the average COD of water outlet CrBe 128mg/L.

Claims (3)

1. the method for the reducing waste water in the ion-exchange absorption process for producing DSD acid process is characterized in that may further comprise the steps:
1) millipore filter with aperture 30-200 μ m filters the DSD acid that the reducing waste water recovery wherein suspends;
2) initial pH value of the reducing waste water of step 1) being handled with alkali transfers to 4-6, and keeps room temperature;
3) with step 2) reducing waste water handled carries out adsorption operations by the bed that is filled with macroporous weakly basic anion exchange resin;
4) with mass concentration be the sodium hydroxide solution of 4.0-8.0%, at room temperature, macroporous weakly basic anion exchange resin carried out wash-out after, more set by step 3) the next batch reducing waste water is carried out adsorption operations.
2. the method for adsorbing the reducing waste water in the process for producing DSD acid process by the described ion-exchange of claim 1, it is characterized in that: used macroporous weakly basic anion exchange resin is homemade D301 resin, D370 resin, D380 resin in the step 3), or in the Amberlite series of producing by U.S. Rohm-Haas company with homemade D301 resin, D370 resin, the corresponding macroporous weakly basic anion exchange resin of D380 resin model.
3. by the method for the reducing waste water in the described ion-exchange of the claim 1 absorption process for producing DSD acid process, it is characterized in that: step 2) in alkali be sodium hydroxide solution or particle, potassium hydroxide solution or particle.
CN 200410020217 2004-07-30 2004-07-30 Method of treating reduction water of DSD acid producing process by ion exchange adsoption Expired - Fee Related CN1251973C (en)

Priority Applications (1)

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CN 200410020217 CN1251973C (en) 2004-07-30 2004-07-30 Method of treating reduction water of DSD acid producing process by ion exchange adsoption

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200410020217 CN1251973C (en) 2004-07-30 2004-07-30 Method of treating reduction water of DSD acid producing process by ion exchange adsoption

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CN1597543A CN1597543A (en) 2005-03-23
CN1251973C true CN1251973C (en) 2006-04-19

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102295393B (en) * 2011-08-22 2012-09-05 山西阳煤丰喜肥业(集团)有限责任公司 Treatment process for production wastewater of DSD acid
US8986503B2 (en) 2013-03-13 2015-03-24 Kadant Inc. Whitewater recovery process
CN105110537B (en) * 2015-08-21 2017-06-06 山西青山化工有限公司 A kind for the treatment of of DSD acid oxidized waste water and its recovery method as resource
CN108217814A (en) * 2018-02-12 2018-06-29 浙江工业大学 A kind of method using brilliant glue adsorption treatment on sewage

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