CN1597546A - Method of treating waste water of DSD acid producing process by oxidation /flocculation - Google Patents
Method of treating waste water of DSD acid producing process by oxidation /flocculation Download PDFInfo
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- CN1597546A CN1597546A CN 200410020218 CN200410020218A CN1597546A CN 1597546 A CN1597546 A CN 1597546A CN 200410020218 CN200410020218 CN 200410020218 CN 200410020218 A CN200410020218 A CN 200410020218A CN 1597546 A CN1597546 A CN 1597546A
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- waste water
- ferric sulfate
- iron vitriol
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- reducing waste
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
A process for treating the reduced waste water generated in the production of DSD acid by oxidizing/flocculating method includes such steps as filtering to recover the suspended DSD acid, adding heptahydrated ferrous sulfate or iron sulfate or their mixture, regulating pH=1-4, three stages of adding hydrogen peroxide and oxidizing reaction, adding flocculant, flocculating, filtering, flocculating again to obtain filtered cake to be used as the flocculant further.
Description
Technical field
The present invention relates to a kind of oxidation/flocculation treatment and produce the method for the reducing waste water in the 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 has flocculation agents such as adding quaternary ammonium salt, molysite, aluminium salt and polyacrylamide in waste water to carry out flocculation decoloration 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 a kind of oxidation/flocculation treatment to produce the method for the reducing waste water in the DSD acid process, this method processing costs is low, effective.
The present invention is realized that by following technical proposals a kind of oxidation/flocculation treatment is produced the method for the reducing waste water in the DSD acid process, it is characterized in that may further comprise the steps:
1, the strainer with aperture 30-200 μ m filters the DSD acid that the reducing waste water recovery wherein suspends.
2, filter the reducing waste water obtain to step 1 and add a certain amount of iron vitriol or ferric sulfate, or the mixture of iron vitriol and ferric sulfate, the pH value of adjusting waste water is 1-4,1-2 preferably, and temperature remains on more than 65 ℃, preferably 70-80 ℃.
3, the reducing waste water that obtains to step 2 divides three periods to add hydrogen peroxide to carry out oxidizing reaction, and when the hydrogen peroxide mass concentration was 30%, three times dosage was followed successively by 0.25ml/L waste water, 0.25ml/L waste water, 0.5ml/L waste water; Be spaced apart 5-15 minute at every turn.
4, press 0.02-0.025 mole/L waste water in the reducing waste water after step 3 oxidizing reaction and add iron vitriol or ferric sulfate, or the mixture of iron vitriol and ferric sulfate and transfer to pH value＞10 with milk of lime and carry out flocculating the first time.
5, filter to remove the flocculation filter cake, and in the reducing waste water that leaches, add iron vitriol or ferric sulfate again by 0.02-0.025 mole/L waste water, or the mixture of iron vitriol and ferric sulfate and transfer to pH value＞10 with milk of lime and carry out flocculating the second time.
6, filter and to tell the flocculation filter cake, discharge after with sulfuric acid the pH value of reducing waste water being transferred to 6-9.
When 7, carrying out the reducing waste water processing of next batch, add iron vitriol or ferric sulfate by 0.01-0.0125 mole/L waste water when flocculating for the first time, or the mixture of iron vitriol and ferric sulfate, add simultaneously and flocculate last consignment of handles filter cake for the second time and transfer to pH value＞10 with milk of lime, when carrying out flocculating the second time, 5 operations set by step.
Add iron vitriol or ferric sulfate in the above-mentioned steps 2, or the mole number of the mixture of iron vitriol and ferric sulfate be step 3 add the hydrogen peroxide mole number 1/20 to 1/5.
Reaction principle of the present invention is: a, at Fe
2+Under the catalyst action, H
2O
2Can produce two kinds of active hydroxyl free radical OH and HO
2Thereby, cause and the propagation radical chain reaction, accelerate the oxidation of organism and reducing substances, destroy chromophoric group.In b, the oxidising process, the effect of OH is the phenyl ring that destroys in the aromatics, and OH is at first with the phenyl ring hydroxylation, then with O
2Effect generates the hydrogen peroxide free radical on the phenyl ring, and then open loop generates fatty compounds, and along with the intensification of degree of oxidation, carbochain ruptures gradually, and final product is CO
2
Technical progress effect of the present invention shows the following aspects:
Processing costs is low, and medicament expense is lower than 4 yuan of/ton waste water; Colourity and COD remove good, reach emission request; Equipment, technology are simple, easy to operate.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment 1
Get 800ml waste water, be placed in the beaker, drive agitator and stir, water sample is heated to 70-80 ℃, in waste water, add 0.2gFeSO with the B filtration
47H
2O adds H then
2O
20.8ml, divide 3 each intervals to add in 5 minutes, dosage is followed successively by 0.2ml, 0.2ml, 0.4ml reacted 30 minutes.Flocculate twice after the oxidation, flocculation for the first time adds to go up criticizes the filter cake of flocculation for the second time, with Ca (OH)
2Water sample is transferred to alkalescence (pH＞10, down together), stir, sedimentation is filtered.Flocculation for the second time adds 5g FeSO47H2O, with Ca (OH)
2Water sample is transferred to alkalescence, stir, sedimentation is filtered, and promptly gets to handle back finished product water sample.Measuring its COD is 102mg/L, and colourity is 50 times.
Embodiment 2
Reducing waste water is discharged through the workshop, at first enters the settling bowl sedimentation, squeezes into millipore filter with pump then, reclaims the DSD acid that suspends in the waste water, with the waste water 4m after filtering
3Pump into the reactor of a diameter 1.8m, high 2.0m, start to stir, open the steam-pipe heating, treat that wastewater temperature rises to 80 ℃ after, add iron vitriol 1.0kg (0.25kg/m
3Waste water) and 30% hydrogen peroxide 4.0kg (1kg/m
3Waste water), dosing method and reaction times are with embodiment 1.Reaction back water flows to flocculation basin I, the filter cake and the 13.0kg (3.25kg/m of batch flocculation in the adding
3Waste water) lime, stirring, mixing, sedimentation is with flowing into flocculation basin II behind the Plate Filtration; In flocculation basin II, add ferrous sulfate 25.0kg (6.25kg/m
3Waste water) and lime 13.0kg (3.25kg/m
3Waste water), stir, sedimentation is respectively 110mg/L and 55 times with COD that measures filtrate behind the Plate Filtration and colourity, all reaches discharging standards, can discharge after regulating pH to 6-9 with sulfuric acid.
Claims (2)
1. an oxidation/flocculation treatment is produced the method for the reducing waste water in the DSD acid process, it is characterized in that may further comprise the steps:
1) strainer with aperture 30-200 μ m filters the DSD acid that the reducing waste water recovery wherein suspends;
2) filter the reducing waste water obtain to step 1) and add a certain amount of iron vitriol or ferric sulfate, or the mixture of iron vitriol and ferric sulfate, the pH value of adjusting waste water is 1-4,1-2 preferably, and temperature remains on more than 65 ℃, preferably 70-80 ℃;
3) to step 2) reducing waste water that obtains divides three periods to add hydrogen peroxide to carry out oxidizing reaction, and when the hydrogen peroxide mass concentration was 30%, three times dosage was followed successively by 0.25ml/L waste water, 0.25ml/L waste water, 0.5ml/L waste water; Be spaced apart 5-15 minute at every turn;
4) press 0.02-0.025 mole/L waste water in the reducing waste water after the step 3) oxidizing reaction and add iron vitriol or ferric sulfate, or the mixture of iron vitriol and ferric sulfate and transfer to pH value＞10 with milk of lime and carry out flocculating the first time;
5) filter to remove the flocculation filter cake, and in the reducing waste water that leaches, add iron vitriol or ferric sulfate again by 0.02-0.025 mole/L waste water, or the mixture of iron vitriol and ferric sulfate and transfer to pH value＞10 with milk of lime and carry out flocculating the second time;
6) filter and to tell the flocculation filter cake, discharge after with sulfuric acid the pH value of reducing waste water being transferred to 6-9;
When 7) carrying out the reducing waste water processing of next batch, add iron vitriol or ferric sulfate by 0.01-0.0125 mole/L waste water when flocculating for the first time, or the mixture of iron vitriol and ferric sulfate, add simultaneously and flocculate last consignment of handles filter cake for the second time and transfer to pH value＞10 with milk of lime, when carrying out flocculating the second time, set by step 5) operation.
2. produce the method for the reducing waste water in the DSD acid process by the described oxidation of claim 1/flocculation treatment, it is characterized in that step 2) in the institute add iron vitriol or ferric sulfate, or the mole number of the mixture of iron vitriol and ferric sulfate be step 3) add the hydrogen peroxide mole number 1/20 to 1/5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020218 CN1244502C (en) | 2004-07-30 | 2004-07-30 | Method of treating waste water of DSD acid producing process by oxidation /flocculation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020218 CN1244502C (en) | 2004-07-30 | 2004-07-30 | Method of treating waste water of DSD acid producing process by oxidation /flocculation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1597546A true CN1597546A (en) | 2005-03-23 |
| CN1244502C CN1244502C (en) | 2006-03-08 |
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|---|---|---|---|
| CN 200410020218 Expired - Fee Related CN1244502C (en) | 2004-07-30 | 2004-07-30 | Method of treating waste water of DSD acid producing process by oxidation /flocculation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100478284C (en) * | 2007-09-10 | 2009-04-15 | 张国平 | Preparation method of polymeric aluminum ferric sulfate water purifying agent and product thereof |
| CN101693571B (en) * | 2009-10-21 | 2011-07-13 | 中国石油化工集团公司 | Wastewater pretreatment method |
| CN105692952A (en) * | 2016-01-22 | 2016-06-22 | 南通海陵环境检测有限公司 | Treatment method of textile wastewater |
| CN110590024A (en) * | 2019-10-25 | 2019-12-20 | 北京盖雅环境科技有限公司 | Method for treating DSD acid oxidative condensation wastewater |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101700941B (en) * | 2009-11-20 | 2011-11-09 | 上海应用技术学院 | Method for demulsifying and purifying waste emulsion produced by dyeing high-end ribbons |
-
2004
- 2004-07-30 CN CN 200410020218 patent/CN1244502C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100478284C (en) * | 2007-09-10 | 2009-04-15 | 张国平 | Preparation method of polymeric aluminum ferric sulfate water purifying agent and product thereof |
| CN101693571B (en) * | 2009-10-21 | 2011-07-13 | 中国石油化工集团公司 | Wastewater pretreatment method |
| CN105692952A (en) * | 2016-01-22 | 2016-06-22 | 南通海陵环境检测有限公司 | Treatment method of textile wastewater |
| CN105692952B (en) * | 2016-01-22 | 2018-06-01 | 南通海陵环境检测有限公司 | The processing method of textile waste |
| CN110590024A (en) * | 2019-10-25 | 2019-12-20 | 北京盖雅环境科技有限公司 | Method for treating DSD acid oxidative condensation wastewater |
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| Publication number | Publication date |
|---|---|
| CN1244502C (en) | 2006-03-08 |
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