CN102992542A - Method for treating heavy-nitrogen mother solution generated from production of dinitrodiazophenol - Google Patents
Method for treating heavy-nitrogen mother solution generated from production of dinitrodiazophenol Download PDFInfo
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- CN102992542A CN102992542A CN2012104854149A CN201210485414A CN102992542A CN 102992542 A CN102992542 A CN 102992542A CN 2012104854149 A CN2012104854149 A CN 2012104854149A CN 201210485414 A CN201210485414 A CN 201210485414A CN 102992542 A CN102992542 A CN 102992542A
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- mother liquor
- pool
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Abstract
The invention relates to a method for treating the heavy-nitrogen mother solution generated from production of dinitrodiazophenol, comprising the following steps of: collecting the heavy-nitrogen mother solution into a primary acid-base regulation pool, mixing, adjusting the pH value to 3, lifting onto an iron-carbon bed, making the effluent flow into a secondary acid-base regulation pool, adjusting the pH value to 3-4, feeding into a Fenton-like reaction pool for reaction, making the mother solution flow into a neutralization pool, adding carbide slag to adjust the pH to 7-8, filing nitrogen in the mother solution at the same time, making the mother solution flow into a flocculation and sedimentation pool, feeding the supernatant obtained by settling into a subsequent biological treatment unit, treating until the supernatant reaches the standard, discharging or recycling, lifting the sludge obtained by precipitating into a sludge concentration pool, making the supernatant obtained by concentrating reflow into the primary acid-base regulation pool, feeding the concentrated sludge into a horizontal helical centrifuge for centrifugal dehydrating, mixing the dehydrated sludge into steam coal for combustion and utilization, and making a centrifugal separation solution reflow into the primary acid-base regulation pool. The method provided by the invention has the advantages of low investment and stable effect, adopts the carbide slag and waste the scrap iron as the materials for treatment and achieves the purpose of treating the wastes by the wastes.
Description
Technical field
The invention belongs to the technology for treating industrial waste water field, be specifically related to the treatment process of diazonium mother liquor in a kind of priming explosive dinitrodiazophenol production process.
Background technology
Dinitrodiazophenol is as a kind of priming explosive, because of the production process of its good blast performance, safety, and the advantage such as raw material sources are wide, acquisition cost is low, obtain using more widely in the various priming systems at home.The at present domestic dinitrodiazophenol production method that generally adopts is the sodium salt method, and the every production of the method 1kg dinitrodiazophenol approximately produces the mother liquor of 200kg-300kg, and the mother liquor generation is very high.It is complicated that dinitrodiazophenol is produced mother liquor composition, derives from the diazonium mother liquor of picramic acid sodium diazotization flow process in the production process of the second stage, contains the hazardous contaminants such as a large amount of diazoes, nitro, nitroso-group, and COD reaches 1.0 * 10
4-1.5 * 10
4Mg/L, biodegradability is poor, and mother liquor itself is strongly-acid in addition, and colourity can reach 3.0 * 10
4-4.0 * 10
4Doubly, if effectively do not process, its harm to environment is larger.
Mostly adopt dilution method to carry out pre-treatment to the diazonium mother liquor both at home and abroad, namely in the diazonium mother liquor, add a large amount of process waters, with its dilution 10-50 doubly, make the COD of diazonium mother liquor be diluted to about 500-1000mg/L, colourity be diluted to 3000-5000 doubly about, be referred to as diazonium waste water.Then these diazonium waste water are taked mainly to comprise that the technology such as physico-chemical processes, biological process, advanced oxidation processes process.These treatment processs all techniques that exist comparatively complicated more, and treatment effect is not good, is difficult to qualified discharge, and the deficiency such as cost of investment is higher, processing costs is larger, makes manufacturing enterprise be difficult to bear.Simultaneously because of in treating processes, dinitrodiazophenol in the mother liquor usually possesses blast characteristics (even dinitrodiazophenol is also very easily blasted) because of deposition, crystallization in water, cause many enterprises in the process of processing this type of mother liquor, the accidental explosion accident to occur, cause certain loss of life and personal injury and financial loss.Therefore seek efficiently, diazonium mother liquid disposal technical meaning is great economically and reasonably.
Summary of the invention
The objective of the invention is for the deficiency that solves existing diazonium mother liquid disposal technology propose a kind of with iron charcoal micro-electrolysis method as process early stage, in conjunction with the novel combination diazonium mother liquid disposal technology of Fenton oxidation style as follow-up advanced treatment, realize that safe, efficient, the low consumption of diazonium mother liquor processed.
The used process flow sheet of the present invention as shown in Figure 1, concrete technical scheme is as follows:
The treatment process of diazonium mother liquor in a kind of dinitrodiazophenol production process: be the diazonium mother liquor to be collected into through pipeline one-level soda acid equalizing tank mixes, homogeneous, regulating pH is 3, by water pump lifting to iron and carbon bed, the Fe/C mass ratio is 1:1 in the iron and carbon bed, residence time 1h, water outlet is from flowing into secondary acid-alkali accommodation pond, and adjusting pH is 3-4, then enter the Fenton-like reaction tank, adding mass concentration in the reaction tank in the ratio of 5mL/L-10mL/L is 30% H
2O
2Reaction times is 3-4h, mother liquor flows automatically into neutralization tank after the reaction treatment, add carbide slag and regulate pH to 7-8, utilize simultaneously the aerating machine that arranges at the bottom of the pond that mother liquor is carried out oxygenation, rear inflow flocculation sedimentation tank, the precipitation supernatant liquor enters the rear discharging up to standard of follow-up biochemical processing unit processes or reuse, it is concentrated that precipitating sludge is promoted to sludge thickener, supernatant liquor after concentrated is back to one-level soda acid equalizing tank, thickened sludge enters Horizontal helical type centrifuge and carries out centrifuge dehydration, and the mud after the dehydration mixes burning utilization in the steam coal, and centrate is back to one-level soda acid equalizing tank.
The present invention's electrolyte content in considering the diazonium mother liquor is high, conductivity is well on the basis, the waste iron filing that produces take mechanical workout is as the electrolysis raw material, utilize iron charcoal micro-electrolysis method as processing early stage, destroy chromophoric group, nitro compound is reduced into amino benzenes compounds, relies on simultaneously the adsorption function that gac possesses in the iron and carbon bed that the microelectrolysis processing effect is strengthened; Fe via little electrolysis generation
2+, can be directly and the H of follow-up adding
2O
2Reaction forms the Fenton-like reagent with strong oxidizing property, reaches mother liquor is further processed; The present invention has the advantages such as one-time investment is little, working cost is lower, treatment effect is stable, adopts carbide slag, waste iron filing for processing material in pre-treatment, has realized " treatment of wastes with processes of wastes against one another ".
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Among the figure: 1. one-level soda acid equalizing tank; 2. iron and carbon bed; 3. secondary acid-alkali accommodation pond; 4. Fenton-like reaction tank; 5. neutralization tank; 6. flocculation sedimentation tank; 7. sludge thickener; 8. horizontal screw centrifuge; 9. biochemical treatment unit.
Embodiment
The present invention is with the little electrolysis/H of iron charcoal
2O
2Method is processed the diazonium mother liquor, the nascent state [H] that the activity of utilizing electrode reaction to produce is very high, make the organic structural break of ring-type in the mother liquor, the part larger molecular organics is degraded to the small molecules attitude, lower working in coordination with of charcoal absorption effect simultaneously, reduce the COD value of mother liquor, improve the biodegradability of mother liquor; The Fe that the continuous galvanic corrosion of warp produces
2+, in the H of follow-up adding
2O
2Can in conjunction with the Fenton reagent that forms the tool strong oxidizing property, further remove organic pollutant; In neutralization tank, add carbide slag, regulate pH to 7-8, be accompanied by simultaneously aeration, make Fe
2+And Fe
3+Be hydrolyzed into the complex compound that possesses very strong flocculating function, produce precipitation in colloid, suspended substance and the insoluble organic in the absorption mother liquor, water quality is purified; The precipitation supernatant liquor enters the biochemical treatment cell processing and effluxes or reuse after up to standard, and mud is through concentrating, mixing in the steam coal after the centrifuge dehydration and burn, and concentrated solution, parting liquid then are back to one-level soda acid equalizing tank.
Its concrete treatment process is as follows:
As shown in Figure 1, the diazonium mother liquor is collected into through pipeline that one-level soda acid equalizing tank 1 mixes, homogeneous, regulating pH is 3, by water pump lifting to iron and carbon bed 2, in iron and carbon bed 2 interior generation micro-electrolysis reactions, lower working in coordination with of charcoal absorption effect simultaneously, finish pre-treatment, the Fe/C mass ratio is 1:1 in the iron and carbon bed 2, residence time 1h; Water outlet is from flowing into secondary acid-alkali accommodation pond 3, and adjustings pH is 3-4, then enters Fenton-like reaction tank 4, is 30% H in the ratio of 5mL/L-10mL/L adding mass concentration in the reaction tank 4
2O
2, this moment mother liquor in through Fe that galvanic corrosion produces
2+With H
2O
2In conjunction with forming Fenton reagent, make that most organic pollutants obtain degraded in the mother liquor, the reaction times is 3-4h; Mother liquor flows automatically into neutralization tank 5 after the reaction treatment, adds carbide slag and regulates pH to 7-8, utilizes simultaneously the aerating machine that arranges at the bottom of the pond that mother liquor is carried out oxygenation, Fe
2+And Fe
3+Can under the condition of aerobic and alkalescence, form the complex compound of iron, the organism of indissoluble in the absorption waste water; Water outlet flows into flocculation sedimentation tank 6, water quality behind flocculation sediment can reach or near " weapon industry pollution discharge standard Charge of ammunitions " (GB 14470.3-2002) emission request (existing utility), the precipitation supernatant liquor finally enters biochemical treatment unit 9, after processing, biochemical operation can realize standard discharge or reuse, precipitating sludge is promoted to sludge thickener 7, concentrated solution is back to one-level soda acid equalizing tank 1, thickened sludge enters horizontal screw centrifuge 8 centrifuge dehydrations, centrifuge speed is 1500-1800r/min, centrifuge dehydration 8min, moisture percentage in sewage sludge after the dehydration is less than 20%, mix burning utilization in the steam coal, centrate is back to one-level soda acid equalizing tank 1.
The diazonium mother liquor is regulated pH to 3 among the present invention in one-level soda acid equalizing tank, so that waste iron filing and gac in the iron and carbon bed 2 form countless microbatterys under the condition of acidity, [H] activity that produces nascent state through electrolytic reaction is very strong, can with most organism generation redox reactions in the mother liquor, simultaneously by the formed Fe of galvanic corrosion
2+Can with the H of follow-up adding
2O
2Form Fenton reagent, the correlated response equation is for being:
The reduction of Zero-valent Iron: Fe+ larger molecular organics (coloured) → Fe
2++ small organic molecule (colourless)
The reduction of nascent state [H]: [H]+larger molecular organics (coloured) → small organic molecule (colourless)
Little electrolysis electrode reaction formula is:
Anode: Fe-2e → Fe
2+Fe
2++ 2OH
-→ Fe (OH)
2
Negative electrode: larger molecular organics (coloured)+ne-→ small organic molecule (colourless) 2H
2O+2e
-→ H
2+ 2OH
-
Fe
2+With H
2O
2In conjunction with formed Fenton reagent, transferring under the acid condition of pH one-tenth Fe via secondary acid-alkali accommodation pond
2+Become catalyzer and make H
2O
2Decompose generation hydroxyl radical free radical (OH), reaction equation is:
Fe
2++H
2O
2→Fe
3++OH
-+·OH
Fe
3++H
2O
2→Fe
2++·HO
2+H
+
·OH+H
2O
2→H
2O+·HO
2
·HO
2→·O
2 -+H
+
·O
2 -+H
2O
2→O
2+·OH+OH
-
In neutralization tank 5, add carbide slag, at the bottom of the pond, be accompanied by aeration simultaneously, under the condition of oxygenation and alkalescence, make the Fe in the mother liquor
2+And Fe
3+In flocculation sedimentation tank 6, be hydrolyzed into the complex compound with very strong adsorption-flocculation effect, with colloid, the suspended substance in the removal mother liquor, and the organic pollutant of indissoluble, the precipitation water outlet enters follow-up biochemical processing unit 9 and finishes final processing.
The diazonium mother liquor can be realized qualified discharge or reuse after above-mentioned art breading
3 embodiment of the present invention below are provided.
Embodiment 1
The diazonium mother liquor generation that present embodiment is processed is 1.0m
3/ d.
The former pH=1.5-1.7 of diazonium mother liquor, water inlet colourity is 20000 times, COD concentration is 1695.94mg/L.The implementation step is as follows: the diazonium mother liquor is collected into one-level soda acid equalizing tank 1 through pipeline, and regulating pH is 3, and to iron and carbon bed 2, the Fe/C mass ratio is 1:1 in the iron and carbon bed 2, residence time 1h by water pump lifting; Water outlet is from flowing into secondary acid-alkali accommodation pond 3, and regulating pH is 4, then enters Fenton-like reaction tank 4, and adding mass concentration in the reaction tank 4 in the ratio of 5mL/L is 30% H
2O
2, the reaction times is 3h; Mother liquor flows automatically into neutralization tank 5 after the reaction treatment, add carbide slag and regulate pH to 7, utilize simultaneously the aerating machine that arranges at the bottom of the pond that mother liquor is carried out oxygenation, water outlet flows into flocculation sedimentation tank 6, supernatant liquor enters follow-up biochemical processing unit 9 in the pond, COD concentration is down to 11.85mg/L in the supernatant liquor, colourity is down to 40, its COD value and colourity all reach " weapon industry pollution discharge standard Charge of ammunitions " (GB 14470.3-2002) emission request (existing utility), and percent of decolourization and COD clearance are respectively 99.8% and 99.30%; Precipitating sludge is promoted to and is back to one-level soda acid equalizing tank 1 after sludge thickener 7 concentrates, thickened sludge enters horizontal screw centrifuge 8 centrifuge dehydrations, centrifugal rotational speed 1500-1800r/min, centrifuge dehydration 8min, moisture percentage in sewage sludge after the dehydration is less than 20%, mix burning utilization in the steam coal, centrate is back to one-level soda acid equalizing tank 1.
Embodiment 2
The generation of the diazonium mother liquor that present embodiment is processed is 1.2m
3/ d.
The former pH=1.5-1.7 of diazonium mother liquor, water inlet colourity is 20000 times, COD concentration is 1695.94mg/L.The implementation step is as follows: the diazonium mother liquor is collected into one-level soda acid equalizing tank 1 through pipeline, and regulating pH is 3, and to iron and carbon bed 2, the Fe/C mass ratio is 1:1 in the iron and carbon bed 2, residence time 1h by water pump lifting; Water outlet is from flowing into secondary acid-alkali accommodation pond 3, and regulating pH is 3, then enters Fenton-like reaction tank 4, and adding mass concentration in the reaction tank 4 in the ratio of 10mL/L is 30% H
2O
2, the reaction times is 2h; Mother liquor flows automatically into neutralization tank 5 after the reaction treatment, add carbide slag and regulate pH to 8, utilize simultaneously the aerating machine that arranges at the bottom of the pond that mother liquor is carried out oxygenation, water outlet flows into flocculation sedimentation tank 6, supernatant liquor enters follow-up biochemical processing unit 9 in the pond, COD concentration is down to 134.83mg/L in the supernatant liquor, colourity is down to 300, its COD value is near " weapon industry pollution discharge standard Charge of ammunitions " (GB 14470.3-2002) emission request (existing utility), and percent of decolourization and COD clearance are respectively 98.5% and 92.05%; Precipitating sludge is promoted to and is back to one-level soda acid equalizing tank 1 after sludge thickener 7 concentrates, thickened sludge enters horizontal screw centrifuge 8 centrifuge dehydrations, centrifugal rotational speed 1500-1800r/min, centrifuge dehydration 8min, moisture percentage in sewage sludge after the dehydration is less than 20%, mix burning utilization in the steam coal, centrate is back to one-level soda acid equalizing tank 1.
Embodiment 3
The generation of the diazonium mother liquor that present embodiment is processed is 1.8m
3/ d.The former pH=1.5-1.7 of diazonium mother liquor, water inlet colourity is 20000 times, COD concentration is 1695.94mg/L.The implementation step is as follows: the diazonium mother liquor is collected into one-level soda acid equalizing tank 1 through pipeline, and regulating pH is 3, and to iron and carbon bed 2, the Fe/C mass ratio is 1:1 in the iron and carbon bed 2, residence time 1h by water pump lifting; Water outlet is from flowing into secondary acid-alkali accommodation pond 3, and regulating pH is 3, then enters Fenton-like reaction tank 4, and adding mass concentration in the reaction tank 4 in the ratio of 10mL/L is 30% H
2O
2, the reaction times is 3h; Mother liquor flows automatically into neutralization tank 5 after the reaction treatment, add carbide slag and regulate pH to 7-8, utilize simultaneously the aerating machine that arranges at the bottom of the pond that mother liquor is carried out oxygenation, water outlet flows into flocculation sedimentation tank 6, supernatant liquor enters follow-up biochemical processing unit 9 in the pond, COD concentration is down to 86.32mg/L in the supernatant liquor, colourity is down to 220, its COD value is near " weapon industry pollution discharge standard Charge of ammunitions " (GB 14470.3-2002) emission request (existing utility), and percent of decolourization and COD clearance are respectively 98.9% and 94.91%; Precipitating sludge is promoted to and is back to one-level soda acid equalizing tank 1 after sludge thickener 7 concentrates, thickened sludge enters horizontal screw centrifuge 8 centrifuge dehydrations, centrifugal rotational speed 1500-1800r/min, centrifuge dehydration 8min, moisture percentage in sewage sludge after the dehydration is less than 20%, mix burning utilization in the steam coal, centrate is back to one-level soda acid equalizing tank 1.
Claims (1)
1. the treatment process of diazonium mother liquor in the dinitrodiazophenol production process, it is characterized in that, be the diazonium mother liquor to be collected into through pipeline one-level soda acid equalizing tank mixes, homogeneous, regulating pH is 3, by water pump lifting to iron and carbon bed, the Fe/C mass ratio is 1:1 in the iron and carbon bed, residence time 1h, water outlet is from flowing into secondary acid-alkali accommodation pond, and adjusting pH is 3-4, then enter the Fenton-like reaction tank, adding mass concentration in the reaction tank in the ratio of 5mL/L-10mL/L is 30% H
2O
2Reaction times is 3-4h, mother liquor flows automatically into neutralization tank after the reaction treatment, add carbide slag and regulate pH to 7-8, utilize simultaneously the aerating machine that arranges at the bottom of the pond that mother liquor is carried out oxygenation, rear inflow flocculation sedimentation tank, the precipitation supernatant liquor enters the rear discharging up to standard of follow-up biochemical processing unit processes or reuse, it is concentrated that precipitating sludge is promoted to sludge thickener, supernatant liquor after concentrated is back to one-level soda acid equalizing tank, thickened sludge enters Horizontal helical type centrifuge and carries out centrifuge dehydration, and the mud after the dehydration mixes burning utilization in the steam coal, and centrate is back to one-level soda acid equalizing tank.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107144143A (en) * | 2017-04-27 | 2017-09-08 | 福建省民爆化工股份有限公司 | The method that its Heat Treatment DDNP waste water is utilized by technological transformation rotary cement kiln |
| CN107935309A (en) * | 2017-12-01 | 2018-04-20 | 南京理工大学 | Priming produces waste water physicochemical pre-treat biological intensive treatment integrated technique |
| CN108485931A (en) * | 2018-05-04 | 2018-09-04 | 江西洁地环境治理生态科技有限公司 | A kind of continuous processing system handling fermentation biogas slurry based on chlorella |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107144143A (en) * | 2017-04-27 | 2017-09-08 | 福建省民爆化工股份有限公司 | The method that its Heat Treatment DDNP waste water is utilized by technological transformation rotary cement kiln |
| CN107144143B (en) * | 2017-04-27 | 2019-05-10 | 福建省民爆化工股份有限公司 | The method for utilizing its Heat Treatment DDNP waste water by technological transformation rotary cement kiln |
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| CN108485931A (en) * | 2018-05-04 | 2018-09-04 | 江西洁地环境治理生态科技有限公司 | A kind of continuous processing system handling fermentation biogas slurry based on chlorella |
| CN108485931B (en) * | 2018-05-04 | 2023-12-19 | 江西洁地环境治理生态科技有限公司 | Continuous treatment system for treating fermentation biogas slurry based on chlorella |
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Application publication date: 20130327 |