CN103708667B - A kind of substantive dyestuff method of wastewater treatment - Google Patents
A kind of substantive dyestuff method of wastewater treatment Download PDFInfo
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- CN103708667B CN103708667B CN201310731336.0A CN201310731336A CN103708667B CN 103708667 B CN103708667 B CN 103708667B CN 201310731336 A CN201310731336 A CN 201310731336A CN 103708667 B CN103708667 B CN 103708667B
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Abstract
The present invention relates to a kind of substantive dyestuff mother liquor waste water treatment process, belong to disposal of three wastes technical field.Comprise pre-treatment → staticly settle → light electrolysis → Fenton oxidation → flocculation → filtration → evaporative crystallization, staticly settle and cross and filter large particulate matter, the organism in iron-carbon micro-electrolysis redox waste water, flocculation sediment removing organism, removes colourity simultaneously.Apply the present invention to the process of substantive dyestuff mother liquor waste water, have that technique is simple, running cost is low, organic clearance advantages of higher.
Description
Technical field
The present invention relates to a kind of substantive dyestuff method of wastewater treatment, belong to disposal of three wastes technical field.
Background technology
Dye mother solution waste water has the features such as high COD, high salinity, high potential of hydrogen, serious environment pollution, is a difficult problem of administering always, governs the development of enterprise.At present the process main method of dye wastewater is had following several:
Absorption method: the most frequently used activated carbon method is by the water-insoluble and insoluble organism of a large amount of hole wall absorbed portions on gac and is with chromophoric organism.All 10% is not reached, poor effect to the colourity of substantive dyestuff mother liquor waste water of more complicated and the removal of COD.
Flocculence: flocculation is also common process means, many organic waste water flocculations can obtain good outlet effect.But the effect separately for the process of substantive dyestuff mother liquor waste water does not reach requirement, and flocculant usage is large, generation solid waste amount is large, also economical not.
Biological process: biological process utilizes microbial metabolism to realize pollutent minimizing, innoxious promising approach, effectively can remove the COD in sewage.But because organic components in dye wastewater is complicated and normal with features such as high toxicity, peracid alkali content and supersalinitys, the existence of microorganism difficulty or the long-term domestication of needs.In addition, microorganism is responsive to life condition, and waste water from dyestuff water quality is stable not, and this makes the efficiency of microbiological treatment unstable, and the running cost for the treatment of system is high.
Chemical oxidization method: chemical oxidization method has Fenton method, hydrogen peroxide oxidation method etc.Although Fenton method has the clearance of about 40% to substantive dyestuff waste water COD, high cost, general enterprises is difficult to accept.Peroxide passivation effect is poor, and hydrogen peroxide can be combined with the vitriol oil and at high temperature use by general dye wastewater treatment, and the effect of oxidation of organic compounds is better, but cost is still higher, is commonly used in the waste water reclamation spent acid of high spent acid content.
Therefore, existing substantive dyestuff enterprise carries out biotreatment after generally can only adopting advanced oxidation, thin up several times, finally causes that cost is high, system cloud gray model is unstable.
Summary of the invention
The present invention is a kind of substantive dyestuff mother liquor waste water treatment process: first collect substantive dyestuff mother liquor waste water, then filters after waste water being adjusted to acid flocculation; Filtrate carries out micro-electrolysis reaction; Add hydrogen peroxide in waste water after light electrolysis to be oxidized further; Afterwards, regulate waste water to neutrality or alkalescence and stir flocculation; Filter the filtrate obtained and carry out evaporating, concentrating and crystallizing, obtain the inorganic salt tide product of high-quality, can use salt as saltouing in direct reuse to substantive dyestuff production technique, the waste water produced in concentration process and used heat is recycling capable of circulation also, reaches the effect of abatement resource.
Specifically, technical scheme of the present invention is as follows:
A kind of substantive dyestuff mother liquor waste water treatment process, comprises the steps:
(1) pre-treatment: to collect and the pH value adjusting waste water is 2-5, continues to employ;
(2) light electrolysis: waste water for subsequent use is carried out iron-carbon micro-electrolysis reaction 2-10 hour, and the acidity controlled in reaction process is stabilized in acidity (pH value controls at 2-5);
(3) Fenton oxidation: stablize waste water acidity acid (pH value controls at 2-5), add excessive H in the waste water after light electrolysis
2o
2the Fenton oxidation 0.5-8 hour carried out, H
2o
2mass concentration is 30%, and addition is 0.01-1%;
(4) flocculate: the waste water acidity after Fenton oxidation process is stabilized in neutrality or weakly alkaline (pH value controls at 7-10), flocculate after 0.5-4 hour, filter, remove and residue and throw out;
(5) evaporative crystallization: the filtrate after previous step being filtered carries out evaporation concentration, is separated and obtains damp product sodium salt, the mother liquor concentrations liquid reuse of separation.
Wherein, in technique scheme:
Described waste water comprises acid waste water and alkaline waste water, and in acid waste water, the mass content of sulfuric acid or hydrochloric acid is 0.1-40%, and in alkaline waste water, the mass content of alkali is 0.1-10%.
Described light electrolysis reagent is add the mixture that copper and other metal powders formed in the mixture of finished iron carbon reagent, 2-10% iron powder and 0.05-1% gac or 2-10% iron powder and 0.05-1% gac.
The mode of described evaporative crystallization is the concentrated or Multi-effect concentration of MVR evaporation concentration, single-action, evaporative condenser hot water for the production of in washing, moisturizing and heat exchange.
In described pH regulator, adjustment acid used is sulfuric acid or hydrochloric acid, and adjustment alkali used is sheet alkali, soda ash, sodium bicarbonate or its combination.
Light electrolysis and Fenton oxidation reaction all can consumption acids, therefore need online mediation system acidity; When adding alkali flocculation stirring, after first rapid stirring 0.5-1h, monitoring pH, if pH<7, to need to add after certain alkali stirring at low speed again, keeps flocculation system all the time in neutral or alkaline.
The mode of evaporation concentration is the concentrated or Multi-effect concentration of MVR evaporation concentration, single-action, and evaporative condenser gained hot water can be used for washing in industrial production, moisturizing or heat exchange.
Principle of work of the present invention and beneficial effect as follows:
1. pretreated waste water first staticly settles, and crosses and filters large particulate matter, guarantee that COD clearance can reach 1%-50%, alleviate intensity and the difficulty of subsequent disposal.
2. pretreated waste water adopts the organism in iron-carbon micro-electrolysis redox waste water, cut-off the ring of aromatics, larger molecular organics is decomposed into small molecules, then adds a small amount of hydrogen peroxide and just can form Fenton reagent, further oxygenolysis organism.
3. the waste water after fully oxidized decomposition (Fenton oxidation) is adjusted to neutrality or alkalescence, carries out flocculation sediment, removing organism, removes colourity simultaneously.
4. the chroma in waste water after flocculation and COD eliminate major part, can directly enter MVR system, be recovered to clean salt and be back to industrial production, distillation condenses phlegma COD is less than 200mg/L, color is as clear as crystal, meet standards for industrial water usage completely, cooling water can recycle, and also can be used as thermal source and uses.
Its technological effect of such scheme is far longer than the simple combination of each technique, concise in technology, simple to operate, organic clearance can reach more than 80%, the solid waste produced also obtains molysite or other products by certain process regeneration, not only reach the target of wastewater treatment, also obtain a lot of valuable byproduct, running cost is lower; Larger advantage is present invention process, and almost non-secondary pollution produce are raw, and enterprise can realize " cleaner production ".
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
By the substantive dyestuff mother liquor waste water of acidity, (COD is between 11000-13000mg/L, pH=5) filter after leaving standstill 0.5h, filtrate pump enter in micro-electrolysis reaction pond add 0.5%(wt after normal temperature (20-25 DEG C) stirring reaction 4h) hydrogen peroxide (mass concentration 30%, lower with) with 40-60 DEG C at stirring reaction 3h, add liquid caustic soda again and regulate pH=9, filter after stirring flocculation 1h, record liquor C OD and be about 2500mg/L, clearance reaches about 80%, filtrate evaporation concentration, separation obtains sodium-chlor, meet sodium chloride salt industrial standards after testing, concentrated mother liquor is mixed with stoste and again enters treatment system.The COD of water of condensation, can reuse at about 110mg/L.
Embodiment 2
Substantive dyestuff mother liquor sewage (COD is between the 9000-11000mg/L) pH of neutrality is adjusted to 4, filter after stirring 0.5h, filtrate pump is entered in micro-electrolysis reaction pond the hydrogen peroxide (30%) adding 0.2% after normal temperature (20-25 DEG C) stirring reaction 4h, stirring reaction 2h at 40-60 DEG C, add alkali again regulate wastewater pH=7 and stir flocculation 0.5h, recording liquor C OD is 2008mg/L, clearance reaches more than 82%, the transparent micro-Huang of filtrate, filtrate carries out evaporation concentration, isolate sodium chloride salt, meet sodium chloride salt industrial standards after testing, parting liquid after thickening filtration is turned back in original mother liquor, again carry out next batch process through foregoing schemes.The COD of distillation water of condensation, can reuse at about 150mg/L.
Embodiment 3
By the substantive dyestuff sewage of alkalescence, (COD is about 23000mg/L, pH>14) add hydrochloric acid and pH is transferred to 5, filter after stirring flocculation 1h, filtrate pump is entered normal temperature (20-25 DEG C) stirring reaction 4h in micro-electrolysis reaction pond, add the hydrogen peroxide (30%) of 1%, stirring reaction 2h at 40-60 DEG C, add alkali again regulate wastewater pH=7 and stir flocculation 0.5h, recording liquor C OD is 4108mg/L, clearance reaches more than 80%, the transparent micro-Huang of filtrate, filtrate carries out evaporation concentration, isolate sodium chloride salt, meet sodium chloride salt industrial standards after testing, parting liquid after thickening filtration is turned back in original mother liquor, again carry out next batch process through foregoing schemes.The COD of distillation water of condensation, can reuse at about 180mg/L.
Embodiment 4
Alkaline substantive dyestuff sewage in example 3 is added hydrochloric acid pH is transferred to 3, filter after flocculation stirring 1h, 4% reduced iron powder and 0.4% activity charcoal powder mix reagent is added in filtrate, at normal temperatures after stirring reaction 4h, add 0.5% hydrogen peroxide (30%) and with 40-60 DEG C at stirring reaction 1h, then waste liquor PH is adjusted to 7, filters after continuously stirring 0.5h, sampling and testing liquor C OD is 1700mg/L, COD clearance about 93%.Filtrate is carried out evaporation concentration, isolates sodium chloride salt, meet sodium chloride salt industrial standards after testing, the parting liquid after thickening filtration is turned back in original mother liquor, again carry out the process of next batch through foregoing schemes.The COD of distillation water of condensation, can reuse at about 80mg/L.
Embodiment 5
By three kinds of different substantive dyestuff sewage by volume 1:1:1 mix (combined sewage COD about 15000-20000mg/L, pH=6), add hydrochloric acid and pH is transferred to 5, filter after leaving standstill 18h after stirring flocculation 1h, filtrate pump is entered in micro-electrolysis reaction pond the hydrogen peroxide (30%) adding 0.05% after normal temperature (20-25 DEG C) stirring reaction 4h, stirring reaction 2h at normal temperatures, add alkali again regulate wastewater pH=7 and stir flocculation 2h, recording liquor C OD is 3808mg/L, clearance reaches more than 82%, the transparent micro-Huang of filtrate, filtrate carries out evaporation concentration, isolate sodium chloride salt, meet sodium chloride salt industrial standards after testing, parting liquid after thickening filtration is turned back in original mother liquor, again carry out next batch process through foregoing schemes.The COD of distillation water of condensation, can reuse at about 200mg/L.
Embodiment 6
Substantive dyestuff sewage is added hydrochloric acid according to volume ratio 1:1:1 mixing (combined sewage COD is 15000-20000mg/L) pH is transferred to 5, 1h is left standstill after stirring flocculation 1h, filter the filtrate pump obtained and enter in micro-electrolysis reaction pond the hydrogen peroxide (30%) adding 0.8% after normal temperature (20-25 DEG C) stirring reaction 4h, stirring reaction 2h at normal temperatures, add alkali again regulate wastewater pH=7 and stir flocculation 0.5h, recording liquor C OD is 3008mg/L, clearance reaches more than 80%, the transparent micro-Huang of filtrate, filtrate carries out evaporation concentration, isolate sodium chloride salt, meet sodium chloride salt industrial standards after testing, parting liquid after thickening filtration is turned back in original mother liquor, again carry out next batch process through foregoing schemes.The COD of distillation water of condensation, can reuse at about 190mg/L.
Embodiment 7
Substantive dyestuff sewage is added hydrochloric acid according to volume ratio 1:1:1 mixing (combined sewage COD about 15000-20000mg/L) pH is transferred to 2, 8h is left standstill after stirring flocculation 1h, filter the filtrate pump obtained and enter in micro-electrolysis reaction pond the hydrogen peroxide (30%) adding 0.8% after normal temperature (20-25 DEG C) stirring reaction 4h, stirring reaction 2h at 50-70 DEG C, add alkali again regulate wastewater pH=10 and stir flocculation 0.5h, recording liquor C OD is 2208mg/L, clearance reaches more than 85%, the transparent micro-Huang of filtrate, filtrate carries out evaporation concentration, isolate sodium chloride salt, meet sodium chloride salt industrial standards after testing, parting liquid after thickening filtration is turned back in original mother liquor, again carry out next batch process through foregoing schemes.The COD of distillation water of condensation, can reuse at about 140mg/L.
Embodiment 8
Substantive dyestuff sewage is mixed (combined sewage COD about 15000-20000mg/L according to volume ratio 1:1:1, pH=6) add hydrochloric acid and pH is transferred to 4, 2h is left standstill after stirring flocculation 1h, the hydrogen peroxide (30%) of 0.5% is added after filtering filtrate normal temperature (20-25 DEG C) the micro-electrolysis reaction 8h obtained, stirring reaction 4h at 50-70 DEG C, add alkali again regulate wastewater pH=7 and stir flocculation 1h, recording liquor C OD is 3100mg/L, clearance reaches more than 80%, the transparent micro-Huang of filtrate, filtrate carries out evaporation concentration, isolate sodium chloride salt, meet sodium chloride salt industrial standards after testing, parting liquid after thickening filtration is turned back in original mother liquor, again carry out next batch process through foregoing schemes.The COD of distillation water of condensation, can reuse at about 160mg/L.Comparative example 1: conventional micro-electrolysis method
By substantive dyestuff sewage, according to volume ratio 1:1:1 mixing, (combined sewage COD is about 15000-20000mg/L, pH=6) add hydrochloric acid and pH is transferred to 4,2h is left standstill after stirring flocculation 1h, add alkali after filtering filtrate normal temperature (20-25 DEG C) the micro-electrolysis reaction 8h obtained regulate wastewater pH=7 and stir flocculation 1h, recording liquor C OD is 8060mg/L, clearance about 50%, filtrate is transparent micro-red, filtrate carries out evaporation concentration, isolate sodium chloride salt, parting liquid after thickening filtration is turned back in original mother liquor, again carries out next batch process through foregoing schemes.
Comparative example 2: conventional Fenton oxidation method
Substantive dyestuff sewage is mixed (combined sewage COD about 15000-20000mg/L according to volume ratio 1:1:1, pH=6) add hydrochloric acid and pH is transferred to 4, 2h is left standstill after stirring flocculation 1h, filter the filtrate obtained and add the ferrous sulfate of 3% and the hydrogen peroxide (30%) of 0.3%, stirring reaction 4h at 50-70 DEG C, add alkali again regulate wastewater pH=7 and stir flocculation 1h, recording liquor C OD is 7600mg/L, clearance reaches about 53%, filtrate is transparent slightly black, filtrate carries out evaporation concentration, isolated sodium chloride salt color is darker, parting liquid after thickening filtration is turned back in original mother liquor, again carry out next batch process through foregoing schemes.
To the various embodiments described above according to industrial standard HG3255-2001 carry out sodium-chlor detect analyze, result gathers as shown in table 1.
In each enforcement case of table 1, sodium-chlor detects analytical table
Above-mentioned contrast can be found out, adopt technical solution of the present invention, the decreasing ratio of COD is all more than 80%, and the decreasing ratio of the oxidation style of routine and micro-electrolysis method is only about 50%, regular oxidation method and micro-electrolysis method to deviate from cost high, process loaded down with trivial details, remove the cycle long.The technological effect of technical solution of the present invention is adopted to be far longer than the simple combination of each technique, concise in technology, simple to operate, organic clearance can reach more than 80%, the solid waste produced also obtains molysite or other products by certain process regeneration, not only reach the target of wastewater treatment, also obtain a lot of valuable byproduct, running cost is lower; Larger advantage is present invention process, and almost non-secondary pollution produce are raw, and enterprise can realize " cleaner production ".
Claims (1)
1. a substantive dyestuff mother liquor waste water treatment process, is characterized in that, comprises the steps:
(1) pre-treatment: to collect and the pH value adjusting waste water is 2-5, continue to employ, waste water comprises acid waste water and alkaline waste water, and in acid waste water, the mass content of sulfuric acid or hydrochloric acid is 0.1-40%, and in alkaline waste water, the mass content of alkali is 0.1-10%;
(2) light electrolysis: waste water for subsequent use is carried out iron-carbon micro-electrolysis reaction 2-10 hour, and the pH value controlled in reaction process is 2-5, light electrolysis reagent is wherein the mixture of 2-10% iron powder and 0.05-1% gac or the mixture of 2-10% iron powder, 0.05-1% gac and copper powder, in described pH regulator, adjustment acid used is sulfuric acid or hydrochloric acid, and adjustment alkali used is sheet alkali, soda ash, sodium bicarbonate or its combination;
(3) Fenton oxidation: add H in the waste water after previous step process
2o
2the Fenton oxidation 0.5-8 hour carried out, H
2o
2mass concentration be 30%, addition is 0.01-1%, and the waste water ph controlled in reaction process is between 2-5;
(4) flocculate: the waste water ph after previous step process is stabilized in 7-10, flocculates after 0.5-4 hour, filter, disgorging;
(5) evaporative crystallization: the filtrate after previous step being filtered carries out evaporation concentration, the mode of evaporative crystallization is MVR evaporation concentration, single-action concentrates or Multi-effect concentration, evaporative condenser hot water for the production of in washing, moisturizing and heat exchange, be separated and obtain damp product sodium salt, the mother liquor concentrations liquid reuse of separation.
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| CN104556521A (en) * | 2014-12-31 | 2015-04-29 | 绍兴奇彩化工有限公司 | Treatment method for condensed wastewater in disperse blue 56 production process |
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| CN104591449A (en) * | 2015-01-27 | 2015-05-06 | 绍兴奇彩化工有限公司 | Method for removing bromine from disperse dye wastewater |
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| CN108439569A (en) * | 2018-05-17 | 2018-08-24 | 山东大学 | A kind of method of low-temperature heat enhancing class Fenton processing highly acid disperse dyestuff waste water |
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| CN110156236B (en) * | 2019-06-27 | 2021-05-14 | 南京大学盐城环保技术与工程研究院 | Method for recycling high-salt-content organic wastewater |
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| CN110734172A (en) * | 2019-11-14 | 2020-01-31 | 广东石油化工学院 | preprocessing method for petroleum refining and petrochemical alkaline residue |
| CN112010486B (en) * | 2020-09-07 | 2023-01-20 | 巫协森 | Method and system for treating and recycling cotton dyeing waste dye liquor |
| CN114394709A (en) * | 2021-12-30 | 2022-04-26 | 盐城市国投环境技术股份有限公司 | Bromine removal and purification process for high-salt bromine-containing wastewater |
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Address after: 312000 Zhejiang province Shaoxing Shunjiang Road No. 683 building 903 room 9 Patentee after: ZHEJIANG QICAI ENVIRONMENT TECHNOLOGY CO., LTD. Address before: 312000 Zhejiang city of Shaoxing province Di Dang new building 1709 smartfortune Patentee before: Shaoxing Qicai Chemical Co., Ltd. |