CN104193061B - A kind of processing method of paraquat agricultural chemicals waste water - Google Patents
A kind of processing method of paraquat agricultural chemicals waste water Download PDFInfo
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- CN104193061B CN104193061B CN201410441815.3A CN201410441815A CN104193061B CN 104193061 B CN104193061 B CN 104193061B CN 201410441815 A CN201410441815 A CN 201410441815A CN 104193061 B CN104193061 B CN 104193061B
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Abstract
The present invention has announced a kind of processing method of paraquat agricultural chemicals waste water, belongs to technical field of three-waste treatment. Comprise ozone oxidation → condensing crystallizing → desalinization of soil by flooding or leaching, after adding adsorbent, lead to ozone 1-2 hour nitrone compound more thoroughly, add hydrogen peroxide to promote ozone oxidation speed, after adding a small amount of hydrogen peroxide after oxidation finishes, hue preserving is stable, remove by filter waste residue, the waste water obtaining is directly concentrated, and the salt obtaining just can reach industrial salt standard through a small amount of wash water rinsing again. Apply the present invention to the processing of paraquat agricultural chemicals waste water, processing cost is lower, low for equipment requirements, simple to operation, and operating cost is low, reclaims salt value larger, is applicable to medium-sized and small enterprises' wastewater treatment.
Description
Technical field
The present invention relates to a kind of processing method of paraquat agricultural chemicals waste water, belong to disposal of three wastes technical field.
Background technology
Along with agriculture develop rapidly, kind and the consumption of agricultural chemicals also increase rapidly, present stage, the major part that China is usedAgricultural chemicals all belongs to organic agricultural chemicals, and many have features such as large, the difficult decomposition of toxicity, and agricultural chemicals waste water becomes a disaster of water treatment fieldTopic. Conventional method has at present: biochemical treatment, burning method, super oxidation etc.: biochemical treatment generally needs the micro-life of long-term domesticationThing, and effect is unstable, and many agricultural chemicals can not thoroughly decompose, and part microorganism also can be transferred to, and decomposition is more difficult, toxicity is strongerProduct; The required condition harshness of burning method, high cost, also easily reveal toxic and harmful; Super oxidation is high to equipment requirement,So cost is high, and operating risk is larger, is difficult to popularize.
Some Enterprises adopts activated sludge process to process paraquat waste water (Zhang Yongmei, etc.) in conjunction with burning method, and estimated cost approximately2000 yuan/waste water; Also have enterprise to adopt catalytic oxidation (CN1576242A), in waste water, add catalyst, at 100-200DEG C, react 12-24 hour under the condition of 0.9-1.5MPa, COD clearance is higher than 90%, cyanogen root is almost removed completely, the going of colourityExcept rate has also exceeded 90%, biochemistry pool can be directly entered in water outlet, but the required pressure of this technique is large, the reaction time is longer, cost mistakeHeight, is not suitable for medium-sized and small enterprises and compared with the continous way industrial wastewater treatment system of large enterprises; Patent CN101628767A has deliveredReclaim successively a technique for paraquat, cyanogen root, ammonium salt, reclaim paraquat with extraction, absorb cyanogen root with alkaline emulsion, thenWaste water two effect evaporations except after cyanogen are obtained to ammonium salt, and this technique has reclaimed most of harmful substance, but removal process complicated operation,Required medicament kind is many and price is higher, and more difficult automatic management and cost are higher; The people such as Fu Guanglong published an article in 2012,Use TiO2/ flyash is worked in coordination with Fenton agent treatment paraquat waste water, TiO2/ fine coal preparation method of reagent thereof complexity, high cost,Be difficult to promote.
Summary of the invention
In paraquat production process, produce a large amount of high chromas, high COD, high ammonia nitrogen and highly toxic toxic wastewater, now alsoThere is no general, economically viable processing method, it is main technique place that the present invention takes ozone oxidation → condensing crystallizing → washReason paraquat waste water, and process this waste water taking ozone oxidation as main method, flow process is brief, simple to operate, can be with lowerCost recovery obtains purer chlorination ammonium salt and other can reuse product, obtains that product is qualified and to produce solid waste amount little, comparesHave technique, this technique is easy to operate, cost is low, is more suitable for the enterprise in medium-sized and small enterprises and transitional period.
For achieving the above object, the technical scheme that the present invention takes is as follows:
A processing method for paraquat agricultural chemicals waste water, serves as theme with " ozone oxidation → condensing crystallizing → washing ", concreteStep is as follows:
(1) ozone oxidation: add adsorbent and hydrogen peroxide to the waste water of collecting, and the decolouring of logical ozone oxidation; Ozone oxidationIn process, remain on 5-7 with the pH of hydrochloric acid or ammoniacal liquor control reaction.
(2) filter: in step 1) solution after treatment, add a small amount of hydrogen peroxide, slightly mix rear direct filtration.
(3) concentrated: step 2) in the filtrate condensing crystallizing that obtains;
(4) desalinization of soil by flooding or leaching: separating step 3) concentrate obtain slightly colored salt, add saturated salt solution washing 1-5 time, mistakeFilter obtains cleaner salt.
Further improve above-mentioned technique, obtain following:
In step (1), hydrogen peroxide mass concentration is 50%, and the 0.01-10% that dosage is wastewater quality, plays catalytic oxidationEffect, for strengthening the oxidation of ozone; The dosage of adsorbent is the 0.1-5% of wastewater quality. More preferred, logicalThe ozone flow entering is 30-90g/h; Adsorbent is the one in aluminium oxide, active carbon, molecular sieve, diatomite, flyash; TwoThe addition of oxygen water is the 0.5-3% of wastewater quality, and system pH is by hydrochloric acid or ammoniacal liquor regulation and control, and pH is controlled at 6-8.
In step (2), it is 30% hydrogen peroxide that the solution after ozone oxidation need continue to add mass concentration, the adding of hydrogen peroxideDosage is the 0.01-2% of wastewater quality, for stable ozone oxidation effectiveness, prevents that solution colour from deepening. More preferred, dioxygenThe addition of water is the 0.05-0.5% of wastewater quality.
In step (3), concentrated a kind of or its combination adopting in the concentrated or Multi-effect concentration of MVR evaporation and concentration, single-action; DenseContracting gained condensation hot water is as washings, recirculated water, product make-up water or in line and middle reuse, and evaporation gained neatly can be doneFor cyclic steam heating is used.
In step (4), the desalinization of soil by flooding or leaching adopts saturated ammonium chloride solution washing, the 10-50% that washing consumption is wastewater quality, washingNumber of times is 1-5 time, and cycle-index is 1-5 time, and the washes after recycling is back to step (3) evaporation concentration system to carry outSalt manufacturing.
Paraquat agricultural chemicals waste water not only has high COD, high NH3The features such as-N, but also contain a large amount of hypertoxic cyanides, adoptUse technique scheme of the present invention, its processing procedure comprises " ozone oxidation → concentrated → desalinization of soil by flooding or leaching ", can obtain meet cleanReclaim salt ammonium chloride, be back to use in industrial production separating after the ammonium chloride obtaining is dried, distillation water outlet and cooling water are back to useIn production, the heat energy of collection also can be used as produces energy use, and washes can continue salt manufacturing. At above-mentioned wastewater treatment processIn can obtain the multiple energy can be recycled, significantly save processing cost, economic environmental protection, its operation principle and beneficial effect asUnder:
1. reclaim in salt-making process, using hydrogen peroxide as catalyst, there is the advantages such as green, environmental protection, easy recovery, and reactionIn process, can not introduce the difficult ions of removing such as metal ion, not use noble metal catalyst in whole course of reaction, cost is lower;
2. recycling process is processed in normal pressure process, therefore, does not need the complexity such as HTHP in course of reactionCondition, more for convenience, it is more convenient to operate for technology controlling and process.
3. in the above-mentioned processing procedure of the present invention, the catalyst hydrogen peroxide adopting has certain oxidation-reduction quality, inProperty or alkaline waste water system in, be not only conducive to strengthen the oxidation of ozone, promote reaction to carry out, improve effluent quality; AndAnd because mostly waste water is to be exposed in outdoor environment, after ozone Oxidation Treatment, excessive hydrogen peroxide is conducive to oxidation effectivenessKeep and stablize, having guaranteed maintaining for the treatment of effect, water treatment effect is better, and inorganic salts quality improves.
4. in technique provided by the present invention, in course of reaction, can not introduce the difficult ions of removing such as new metal ion,The catalyst hydrogen peroxide adding, after completion of the reaction, can be discharged with the form such as filtrate or distillate, therefore, and whole course of reactionIn, produce hardly solid waste amount, avoided wastewater treatment the generation in the secondary pollution source such as waste residue therefore, processing cost is low.
Brief description of the drawings
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Embodiment 1
(COD=65200mg/L, NH3-N content is 89930mg/L to paraquat agricultural chemicals waste water, CN-Content=1100Mg/L, pH=10-12), the salt acid for adjusting pH that adds mass concentration and be 36-38% is 10, adds wastewater quality 5% active carbon, logicalAfter ozone oxidation reaction 2 hours, add the hydrogen peroxide (mass concentration is 50%) of wastewater quality 10%, continue oxidation 6 hours.On-line control pH in course of reaction, the system pH of making is stabilized in 9 left and right. In the waste water of oxidation after finishing, add at once 2% dioxygenWater (mass concentration is 30%) is also uniformly mixed 0.5 hour. The filtrate that filtration obtains is limpid lightcoral, records filtrateCOD clearance approximately 75%. By filtrate condensing crystallizing, obtain slightly yellowy salt, the saturated washing lotion washing with 20% one time,Obtain qualified Nacl. The concentrated condensate liquid obtaining is as clear as crystal, COD=80mg/L after measured, and ammonia nitrogen is greater than 1000mg/L。
Embodiment 2
In the present embodiment, (COD=65200mg/L, NH3-N content is 89930mg/L to paraquat waste water, CN-Content=1100mg/L, pH=10-12) add hydrochloric acid (36-38%wt) regulate pH be about 5, add the diatomite of wastewater quality 5%, all the other processingMode is identical with embodiment 1. Waste water after oxidation processes obtains limpid rufous filtrate after filtration, and liquor C OD clearance is57%; By filtrate condensing crystallizing, obtain bolarious salt, the saturated solution washing with 30% 2 times, can obtain qualified industrySalt; The concentrated condensate liquid obtaining is limpid slightly red, records COD=340mg/L, and ammonia nitrogen is less than 35mg/L.
Embodiment 3
In the present embodiment, (COD=65200mg/L, NH3-N content is 89930mg/L to paraquat waste water, CN-Content=1100mg/L, pH=10-12) add hydrochloric acid (36-38%wt) regulate pH be about 7, add the active carbon of wastewater quality 0.1%, all the other placesReason mode is identical with embodiment 1. Waste water after oxidation finishes obtains limpid dark red filtrate, liquor C OD clearance after filtrationBe 66%. Filtrate condensing crystallizing, obtains pinkish-grey salt, and the saturated solution washing with 40% 2 times, can obtain qualified industrySalt. The concentrated condensate liquid obtaining is limpid slightly yellow, records COD=80mg/L, the about 100mg/L of ammonia nitrogen.
Embodiment 4
In the present embodiment, (COD=65200mg/L, NH3-N content is 89930mg/L to paraquat waste water, CN-Content=1100mg/L, pH=10-12) add hydrochloric acid (36-38%wt) and regulate pH to be about 7, add the active carbon of wastewater quality 5%, logical ozone oxygenChange reaction after 2 hours, add the hydrogen peroxide (mass concentration 50%) of wastewater quality 2%, continue oxidation 6 hours, all the other processing modesIdentical with embodiment 1. Oxidation processes waste water later obtains red filtrate after filtration, and liquor C OD clearance is 60%; Filtrate is denseSheepshank crystalline substance, obtains ruddy salt, and the saturated solution washing with 25% 2 times, can obtain qualified Nacl; Concentrated obtainingCondensate liquid is limpid slightly yellow, records COD=282mg/L, the about 100mg/L of ammonia nitrogen.
Embodiment 5
Setting in the present embodiment is identical with embodiment 1, and difference is: paraquat waste water (COD=65200mg/L,NH3-N content is 89930mg/L, CN-Content=1100mg/L, pH=10-12) add hydrochloric acid (36-38%wt) regulate pH be about 7,Add the active carbon of wastewater quality 5%, logical ozone oxidation reaction is after 2 hours, and (quality is dense to add the hydrogen peroxide of wastewater quality 2%Degree is 50%), continue oxidation 6 hours. Oxidation processes waste water later directly filters, and obtains limpid light red filtrate, filtrateCOD clearance is 69%; Filtrate is exposed in air after 24 hours, filtrate color becomes dark red, and COD slightly raises, and will filterLiquid condensing crystallizing, obtains pinkish-grey salt, and the saturated solution washing with 35% 2 times, can obtain qualified Nacl; ConcentrateThe condensate liquid arriving is limpid slightly yellow, records COD=62mg/L, the about 100mg/L of ammonia nitrogen.
Embodiment 6
(COD=65200mg/L, NH3-N content is 89930mg/L to paraquat agricultural chemicals waste water, CN-Content=1100mg/L, pH=11) to add mass concentration be that the salt acid for adjusting pH of 36-38% is 7, adds paraquat agricultural chemicals waste water gross mass 0.5% activityCharcoal, logical ozone oxidation reaction is after 1 hour, and (mass concentration is 50 to add the hydrogen peroxide of paraquat agricultural chemicals waste water gross mass 2.5%%), continue oxidation 3 hours, on-line control pH in course of reaction, the system pH of making is stabilized in 7 left and right; In waste water after oxidation finishesAdd at once 0.5% hydrogen peroxide (mass concentration is 30%) and be uniformly mixed 0.2 hour; The filtrate that filtration obtains is limpidRedness, record liquor C OD clearance approximately 65%; By filtrate condensing crystallizing, obtain slightly yellowy salt, by 20% saturated saltSolution washing 2 times, obtains qualified Nacl; The concentrated condensate liquid obtaining is as clear as crystal, COD=75mg/L after measured, ammonia nitrogen83mg/L。
Embodiment 7
(COD=17200mg/L, NH3-N content is 18700mg/L to paraquat agricultural chemicals waste water, CN-Content=540mg/L, pH=10) to add mass concentration be that the salt acid for adjusting pH of 36-38% is 7, adds paraquat agricultural chemicals waste water gross mass 0.2% activityCharcoal, logical ozone oxidation reaction is after 1 hour, and (mass concentration is 50 to add the hydrogen peroxide of paraquat agricultural chemicals waste water gross mass 1%%), continue oxidation 2 hours, on-line control pH in course of reaction, the system pH of making is stabilized in 7 left and right; In waste water after oxidation finishesAdd at once 0.1% hydrogen peroxide (mass concentration is 30%) and be uniformly mixed 0.1 hour; The filtrate that filtration obtains is limpidRedness, record liquor C OD clearance approximately 85%; By filtrate condensing crystallizing, obtain slightly yellowy salt, by 10% saturated saltSolution washing 1 time, obtains qualified Nacl; The concentrated condensate liquid obtaining is as clear as crystal, COD=25mg/L after measured, ammonia nitrogen46mg/L。
Comparative example 8
(COD=65200mg/L, NH3-N content is 89930mg/L to paraquat waste water, CN-Content=1100mg/L,PH=10-12) add after the ferrous sulfate of wastewater quality 2% and the hydrogen peroxide of wastewater quality 3% (mass concentration is 50%), addEnter hydrochloric acid (mass concentration 36-38%) and regulate pH to 5, be heated to 50 DEG C of left and right insulated and stirred reactions after 1 hour, at this solutionIn add 0.5% active carbon, continue stirring reaction 1 hour, filter. Record COD clearance approximately 45%, color removal approximately 50%，CN-Clearance approximately 85%. Filtrate condensing crystallizing, separates and obtains chlorination ammonium salt, and color is darker, with washing of mother liquor waste water 20%After the washing of water-soluble solution, then add mother liquor waste water 20% Water dissolve salt recrystallization, separate and obtain cleaner chlorination ammonium salt. DenseThe condensate liquid that contracting obtains is light yellow, and COD=850mg/L must further process after measured.
In table 1, provide and in embodiment, reclaim the quality of ammonium chloride and the contrast situation of industrial ammonium chloride quality standard, standardWith reference to GB/T2946-2008.
The treatment effect table of comparisons that the different embodiment of table 1 obtains
Remarks: in table, "-" represents not detect.
In above-mentioned seven embodiment, the detailed description of the invention that embodiment 1-6 is technical solution of the present invention, comparative example7 is conventional process mode.
Can find out from embodiment 1-6, after pH, catalyst amount, adsorbent consumption, reaction, the consumption of hydrogen peroxide is all to uselessWater treatment effect has obvious impact: alkali condition oxidation efficiency is high, and the loss of acid condition ammonium salt is little; Increasing adsorbent consumption canTo reduce inorganic salts slurry amount; Increase catalyst amount, can improve waste water COD clearance, reduce condensed water COD; OxygenAfter changing, add hydrogen peroxide, can reduce inorganic salts washings consumption. Specifically,
Can find out by embodiment 1 and 2,3: hydrogen peroxide under weak basic condition to the catalytic action of ozone oxidationBy force, under alkali condition, ammonia volatilizees in a large number, produces salt amount and declines, and in condensed water, ammonia nitrogen exceeds standard; And under acid condition, hydrogen peroxide catalysis effectRate obviously declines, but ammonium salt loss is little, and in condensation, ammonia-nitrogen content is low.
Can find out by embodiment 2 and 3: in the time not adding or add adsorbent less, the chroma removal rate of waste water obviously declines,Cause condensed water band color, inorganic salts washings consumption increases.
Can find out by embodiment 2 and 4: in the time not adding or add less catalyst hydrogen peroxide, ozone oxidation efficiency is obviously fallenLow.
Can find out by embodiment 2 and 5: after oxidation, do not add or a small amount of 30% hydrogen peroxide, chroma in waste water can become graduallyCause inorganic salts washings consumption to increase greatly.
Comprehensive embodiment 1-6, can find out, hydrogen peroxide after pH, catalyst amount, adsorbent consumption, reaction in embodiment 6Consumption reach optimization, not only keep waste water treatment efficiency high in this condition, condensate liquid is colourless, ammonia nitrogen is low, inorganic saltsSlurry amount is few, also reduces various dosings, reduces medicament waste, reduces process costs.
Comparative example 6 and embodiment 7, can find out, ozone oxidation is more obvious to low concentration wastewater effect.
Compare the conventional process mode described in embodiment 8, technical scheme provided by the present invention has excellent in following several respectsGesture:
First, scheme operation provided by the present invention is terse, and traditional approach treatment process is many, and the pharmaceutical agent of consumptionMany. In traditional approach, except the operations such as deoxidation, also need to carry out insulation reaction, recrystallization reaction just can complete paraquat agricultureThe processing of medicine waste water, and it processes condensed waste water and also needs to carry out advanced treating and just can reach discharge standard, and the applicationIn the scheme providing, by ozone oxidation, filtration, concentrated, the desalinization of soil by flooding or leaching, operation is terse, a large amount of without consuming in processing procedureHeat carries out insulation reaction, also need not adopt the operations such as recrystallization and advanced treating, can reach in line standard, and treatment effeciency is non-Chang Gao, the electric energy consuming in processing procedure, heat energy, resource etc. all less, be also highly beneficial for energy-saving and emission-reduction.
Secondly, from treatment effect, the present invention's chroma in waste water after treatment reduces obviously, and COD reduced rate is high far awayIn the effect of comparative example. The present invention's waste water after treatment, its colourity is less, and COD reduced rate can reach more than 65%, and comparative exampleIn, waste water color and luster after treatment is still darker, and COD clearance only can reach 50% left and right, and waste water after treatment also needs to carry out weightThe operation such as crystallization, advanced treating, waste water after treatment cannot carry out in line.
Finally, from reclaiming product quality aspect, in the product that scheme provided by the present invention reclaims, can not introduce new impurity,And content of beary metal is low. Because each parameter in embodiment 6 reaches optimization, based on this, table 1 is only to embodiment 6 and contrastThe recovery product that embodiment 7 obtains contrasts, as can be seen from Table 1: the quality of embodiment 6 gained ammonium chlorides reaches industryStandard high-class product rank, and the quality of comparative example's 7 gained ammonium chlorides only can reach industrial standard primes rank; The present inventionMedicine containing other metal ions is not provided in the process conditions that provide, therefore reclaims in product chlorination ammonium salt and do not detectIron, and in traditional handicraft, adopt iron content medicament, in its output ammonium chloride, can contain a certain amount of iron that cannot reclaim or remove; ConventionalParaquat agricultural chemicals waste water to be processed in containing sulfate hardly, in technique of the present invention, do not use sulfate, therefore output yetAmmonium chloride in containing sulfate not, and containing sulfate in the Fenton reagent that conventional method is used, in product after treatment, noOnly cannot remove metallic iron ion, also additionally bring newly-increased sulfur impurity hydrochlorate into; In the technique that embodiment 6 adopts, do not addAdd or produce any higher boiling slightly solubility impurity, so its ignition residue amount is little, the product solid waste after subsequent treatment is less, andIn embodiment 7, introduced this type of more impurity, its ignition residue amount is relatively high, has also increased accordingly post-processing difficulty.
The comprehensive the various embodiments described above of analyzing, are ensureing under the good prerequisite of output inorganic salt product quality conventional pretreatmentMethod not only can be introduced a large amount of impurity, also needs heating and thermal insulation reaction, and obvious to the removal effect of chroma in waste water and CODLower than technique of the present invention, cause the salt after concentrating by simply washing is up to standard, still to need recrystallization; Meanwhile, condensing crystallizingNot only COD is high for the condensed water producing, and colourity is higher, cannot directly utilize, and needs advanced treating. With technique phase of the present inventionRatio, not only weak effect, and also treatment conditions are more complicated, and cost is high, especially recrystallization, and its cost seriously limits conventional methodApplication in middle-size and small-size factory. And in the technical solution used in the present invention, by ozone oxidation, filtration, concentrated, the desalinization of soil by flooding or leachingCan realize the efficient processing of waste water, and the preparation cost of the ozone using decreases, by ozone Oxidation Treatment and its other partyFormula combination, while being applied to paraquat wastewater treatment, not only can reach efficient treatment effect, waste water COD is obviously reduced, waste waterColor and luster is down to can discharge standard, and cost is lower, and technique is more succinct, better effects if.
Claims (3)
1. a processing method for paraquat agricultural chemicals waste water, is characterized in that comprising the steps: (1) ozone oxidation: to collectionWaste water in add the adsorbent of wastewater quality 0.1-5%, system pH regulates and controls to 6-8 by hydrochloric acid or ammoniacal liquor, passes into ozone oxygenChange and process 1-4 hour, ozone flow is 30-90g/h; Add the hydrogen peroxide of wastewater quality 0.5-3%, hydrogen peroxide concentration is 50-70%, continue oxidation 1-10 hour; (2) filter: in the waste water after step (1) oxidation processes, again add wastewater quality 0.05-0.5%, the hydrogen peroxide of mass concentration 30%, stirs after 0.1-1 hour and filters; (3) condensing crystallizing: the filter after step (2) is filteredLiquid carries out after condensing crystallizing, separates and obtains crystal salt; (4) desalinization of soil by flooding or leaching: adopt the crystal salt washing 1-of saturated salt solution to step (3)5 times, cycle-index is 1-5 time, saturated salt solution consumption by the 10-50% of processing waste water gross mass, filter and obtain finished product, washWash waste water again reuse to condensing crystallizing carry out recovery and the purifying of finished product salt.
2. the processing method of a kind of paraquat agricultural chemicals waste water as claimed in claim 1, is characterized in that: described adsorbent isA kind of or its mixture in aluminium oxide, active carbon, molecular sieve, diatomite, flyash.
3. the processing method of a kind of paraquat agricultural chemicals waste water as claimed in claim 1, is characterized in that: in step (3), concentratedCrystallization refers to one or more the combination in the concentrated or Multi-effect concentration of MVR evaporation and concentration, single-action, and saturated salt solution is saturatedAmmonium chloride solution.
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| CN105884105A (en) * | 2016-03-08 | 2016-08-24 | 南京红太阳生物化学有限责任公司 | Waste water treatment method for paraquat synthesized through ammonia cyanidation process |
| CN105692867B (en) * | 2016-03-25 | 2019-05-24 | 南昌大学 | A kind of O3 contacted oxidation device for landfill leachate depth efficient process |
| CN109848185B (en) * | 2019-03-11 | 2020-10-27 | 安徽华星化工有限公司 | Monosultap waste salt harmless treatment method |
| CN110981013A (en) * | 2019-12-16 | 2020-04-10 | 江苏兄弟维生素有限公司 | Method for treating waste liquid after extraction of thiamine |
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