CN101671089B - Pretreatment method for glyphosate industrial waste water - Google Patents
Pretreatment method for glyphosate industrial waste water Download PDFInfo
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- CN101671089B CN101671089B CN200910308213XA CN200910308213A CN101671089B CN 101671089 B CN101671089 B CN 101671089B CN 200910308213X A CN200910308213X A CN 200910308213XA CN 200910308213 A CN200910308213 A CN 200910308213A CN 101671089 B CN101671089 B CN 101671089B
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Abstract
A pretreatment method for glyphosate industrial waste water relates to the technical field of the treatment method for the industrial waste water from pesticides. The invention provides the pretreatment method for the glyphosate industrial waste water, which can remove glyphosate, sodium chloride and reduce COD cr value. The pretreatment method can effectively remove the vast majority of sodium chloride and glyphosate in the glyphosate industrial waste water by adopting steps such as adjusting Ph value, catalytic oxidation, calcification phosphorus removal, triple effect evaporation crystallized sodium chloride removal and the like, and greatly reduces COD cr value; the pretreated waste water can be discharged into a follow-up biochemical treatment system for biochemical treatment, thus causing waste water to be discharged after reaching standards, being beneficial to the protection of the environment and having good social benefits.
Description
Technical field
The present invention relates to the treatment process of pesticide wastewater, more particularly, relate to a kind of pretreatment process of glyphosate production wastewater.
Background technology
The glyphosate chemical name is N-(phosphonomethyl) glycine (PMG); it is the natural disposition organophosphorus herbicide that goes out of a kind of efficient, low toxicity, wide spectrum; have good interior suction, conductive performance; very effective to preventing and kill off of multiple dark root malignant weed; having obtained using widely in current agriculture production, is the kind of present weedicide output maximum.At present, the most of glyphosate production of China enterprise is that to be raw material make content by condensation, hydrolysis, crystallization, filtration is 95% glyphosate products with glycine, Paraformaldehyde 96, dimethylphosphite.And meeting produces a large amount of contaminative waste water in the process of using this method production glyphosate, owing to contain the sodium-chlor of high density in this waste water, and contain a certain amount of glyphosate and byproduct of reaction, the CODcr value is high, if directly the discharging meeting causes severe contamination to environment, this waste water be treated as important subject in the industry.
Because glyphosate production wastewater contains a large amount of sodium-chlor and a certain amount of organophosphorus and byproduct of reaction, on handling, there is following difficult point: 1, remove organophosphorus if directly waste water is carried out calcification, the throw out that produces contains a large amount of organophosphoruss, and environment is still a kind of Hazardous wastes; 2, if adopt membrane treatment process to remove organophosphorus, film easily stops up, and often will change film, and system operation cost is too high, and enterprise is difficult to bear; 3,,, finally do not reach the expection treatment effect because of the too high ecotope that can destroy microorganism existence in the biochemical system of waste water saltiness if directly waste water is carried out biochemical treatment; 4, if adopt common vaporizer to concentrate desalination, its shortcoming is to adopt salt continuously, the salt that must turn off steam out behind the condensing crystal, and discontinuous production causes steam consumption big, and processing efficiency is low.
Present domestic most glyphosate production enterprise is to add a certain amount of glyphosate dry powder and be mixed with 10% gyphosate solution and sell by concentrating the back to this wastewater treatment method, but this method and fail thorough removal of pollutants.Along with the raising that China environmental protection requires, 10% gyphosate solution will be stopped the approval registration, and progressively withdraw from China market, and above-mentioned treatment process has been difficult to continue to use.Because this waste water contains sodium-chlor and a certain amount of glyphosate and the byproduct of reaction of high density, use biochemical processing method and handle and be difficult to produce a desired effect, a difficult problem that causes the domestic many glyphosate production of being treated as of this waste water enterprise to be faced.
Summary of the invention
The object of the present invention is to provide and a kind ofly can remove glyphosate, sodium-chlor, reduce the pretreatment process of the glyphosate production wastewater of CODcr value.
The technical solution adopted in the present invention is: a kind of pretreatment process of glyphosate production wastewater may further comprise the steps composition:
(1) regulates pH value
Glyphosate production wastewater is entered equalizing tank, in equalizing tank, add hydrochloric acid soln, the pH value of waste water in the pond is adjusted to 3～4;
(2) catalyzed oxidation
With regulating the back pH value is that 3～4 waste water enters one-level catalyzed oxidation tower, goes into air from the tower pucking of catalyzed oxidation tower, and adds catalytic oxidant Fenton reagent, fully reacts; Then waste water is entered secondary catalyzed oxidation tower, go into air, and add the catalytic oxidant clorox, fully react from the tower pucking of catalyzed oxidation tower;
(3) calcification dephosphorization
Waste water behind catalyzed oxidation is entered in the dephosphorization reaction tank, add dephosphorization agent calcium chloride, after fully reacting, will contain sedimentary waste water and carry out press filtration, throw out is removed after by press filtration;
(4) the triple effect evaporation crystallization removes sodium-chlor
To enter the triple effect evaporation device through the waste water after the calcification dephosphorization, feeding steam carries out stepped evaporation and concentrates, and I is imitated the evaporated vapor pressure-controlling at 0.50～0.65Mpa, and wastewater temperature is controlled at 130～155 ℃; II is imitated the evaporated vapor pressure-controlling at 0.2～0.35Mpa, and temperature is controlled at 100～130 ℃; III is imitated the control of evaporated vapor pressure at 0.03～0.06Mpa, and temperature is controlled at 80～90 ℃, vacuum degree control-0.09～-0.075Mpa; The waste water that will contain crystallization sodium-chlor after triple effect evaporation carries out solid-liquid separation, isolates crystallization sodium-chlor and waste water, crystallization sodium-chlor is carried out centrifugally again, and the centrifugal liquid that goes out returns the dephosphorization reaction tank and carries out dephosphorization once more.
In described step (2) catalyzed oxidation, the amount of going into air from the tower pucking of one-level catalyzed oxidation tower and secondary catalyzed oxidation tower is respectively: the air that blasts and the volume ratio of waste water are 20: 1～25: 1.
In described step (2) catalyzed oxidation, the moiety and the add-on of the catalytic oxidant Fenton reagent that is added are: Fenton reagent by 30% hydrogen peroxide and ferrous sulfate by weight than be 3: 1～8: 1 formulated, the Fenton reagent of adding and the volume ratio of waste water are 1: 10～1: 20.
In described step (2) catalyzed oxidation, the amount of the catalytic oxidant clorox that is added is: available chlorine content is that 7～10% the chlorine bleach liquor and the volume ratio of waste water are 1: 20～1: 50.
In described step (3) the calcification dephosphorization, the amount of the dephosphorization agent calcium chloride that is added is: the weight part ratio of rolling over hundred calcium chloride and waste water is 1: 12～1: 15.
In described step (3) the calcification dephosphorization, will contain sedimentary waste water and carry out press filtration for to carry out press filtration by plate-and-frame filter press.
Described step (4) triple effect evaporation crystallization removes in the sodium-chlor, and the waste water that will contain crystallization sodium-chlor after triple effect evaporation carries out solid-liquid separation for to carry out solid-liquid separation by wet cyclone.
The glyphosate production wastewater that contains the sodium-chlor of high density and a certain amount of glyphosate and byproduct of reaction among the present invention through the twin-stage catalyzed oxidation after, the organophosphoruss of the overwhelming majority are converted into inorganic phosphorus; Generate the calcium phosphate precipitation thing by adding the reaction of dephosphorization agent and inorganic phosphorus again; Then with plate-and-frame filter press to the sedimentary waste water of phosphorous hydrochlorate is carried out press filtration, throw out is removed after being become filter cake by press filtration; The waste water that contains the sodium-chlor of high density after the press filtration, be discharged into and carry out stepped evaporation in the triple effect evaporation device and concentrate, sodium-chlor in the waste water is separated out by crystallization, carry out solid-liquid separation by wet cyclone then, isolate crystallization sodium-chlor and waste water, crystallization sodium-chlor is carried out centrifugally again, the crystallization sodium-chlor after centrifugal can be recycled, the centrifugal liquid that goes out returns and continues reaction in the dephosphorization reaction tank, forms the circulation dephosphorization.Thereby realize removing the purpose of most organophosphoruss, sodium-chlor and reduction CODcr value by aforesaid method.
The invention has the beneficial effects as follows:
1, the present invention is by after carrying out the twin-stage catalyzed oxidation to glyphosate production wastewater, most of organophosphorus is converted into inorganic phosphorus, by adding methods such as dephosphorization agent and the press filtration of application plate-and-frame filter press inorganic phosphorus is removed again, make the organophosphorus in the glyphosate production wastewater realize being removed after the innoxious conversion, thereby reduced the potential threat of this waste water environment.
2, the present invention adopts the triple effect evaporation art breading to contain the glyphosate waste water of a large amount of sodium-chlor, utilizing steam that waste water is carried out stepped evaporation concentrates, the continuous crystallization of sodium-chlor is separated out, adopt spinning liquid to separate then to adopt continuously the salt technology that the sodium-chlor of condensing crystal is carried out solid-liquid separation, the sodium-chlor quality of extraction is good, impurity is few, can recycling.
3, the technical solution adopted in the present invention can effectively be removed most organophosphoruss, the sodium-chlor in the glyphosate production wastewater, significantly reduces the CODcr value; Pretreated waste water can enter follow-up biochemical treatment system and carry out biochemical treatment, can significantly reduce the treatment capacity of follow-up biochemical system, impels waste water finally to realize qualified discharge, is of value to the protection of environment, has good social benefit.
Description of drawings
Fig. 1 is the process flow diagram of the pretreatment process of a kind of glyphosate production wastewater of the present invention.
Embodiment
Embodiment 1:
A kind of pretreatment process of glyphosate production wastewater, implement according to the following steps:
(1) regulates pH value
The glyphosate production wastewater 1000 liters (proportion 1.28 grams per milliliters) that glyphosate content after testing is 1.532%, sodium chloride content is 20.1%, the CODcr value is 58620 mg/litre is entered equalizing tank, in equalizing tank, add 30% hydrochloric acid soln, the pH value of waste water in the pond is adjusted to 3.5.
(2) catalyzed oxidation
With regulating pH value is that waste water after 3.5 enters one-level catalyzed oxidation tower, go into 22500 litres of air from the tower pucking, and in one-level catalyzed oxidation tower, add by 30% hydrogen peroxide and ferrous sulfate by weight than being 66.7 liters of the Fenton reagent that are mixed with at 6: 1, reaction treatment 1.75 hours; And then waste water entered secondary catalyzed oxidation tower, and go into 22500 litres of air from the tower pucking, in secondary catalyzed oxidation tower, add available chlorine content and be 28.6 liters of 8.5% chlorine bleach liquores, reaction treatment 1.75 hours; Behind catalytic oxidation, most of organophosphorus is converted into inorganic phosphorus in the waste water, and some organism is oxidized to small molecules or CO2 in the reaction, and partial organic substances oxidative coupling then takes place generates hydrophobic macromole.
(3) calcification dephosphorization
Waste water behind the catalyzed oxidation is entered in the dephosphorization reaction tank, add 115.6 kilograms in dephosphorization agent 82% calcium chloride, reaction treatment 1.75 hours; To contain sedimentary waste water then and carry out press filtration by plate-and-frame filter press, throw out is removed after being become filter cake by press filtration.Inorganic phosphorus behind catalyzed oxidation in the waste water and dephosphorization agent calcium chloride react and generate the calcium phosphate precipitation thing, use plate-and-frame filter press the more sedimentary waste water of phosphorous hydrochlorate is carried out press filtration, throw out is removed after being become filter cake by press filtration, can remove most organophosphoruss and suspended substance in the glyphosate production wastewater.
(4) the triple effect evaporation crystallization removes sodium-chlor
To enter the triple effect evaporation device through the waste water after the calcification dephosphorization, feeding steam carries out stepped evaporation and concentrates, and I is imitated the evaporated vapor pressure-controlling at 0.50～0.65Mpa, and wastewater temperature is controlled at 130～155 ℃; II is imitated the evaporated vapor pressure-controlling at 0.2～0.35Mpa, and wastewater temperature is controlled at 100～130 ℃; III is imitated the control of evaporated vapor pressure at 0.03～0.06Mpa, and wastewater temperature is controlled at 80～90 ℃, vacuum degree control-0.09～-0.075Mpa; The total time that waste water carries out triple effect evaporation is 1.5 hours; The waste water that contains crystallization sodium-chlor after the triple effect evaporation is carried out solid-liquid separation by wet cyclone, isolate crystallization sodium-chlor and waste water, then crystallization sodium-chlor is carried out centrifugally, the centrifugal liquid that goes out returns the dephosphorization reaction tank and reacts dephosphorization once more.The continuous desalination of process triple effect evaporation can be removed the most sodium-chlor in the glyphosate waste water, the sodium-chlor quality height of extraction, and impurity is few, can recycle.
After testing, the every index through pretreated glyphosate production wastewater changes as follows:
| Sequence number | Index name | Before the processing | After the processing | Clearance (%) |
| 1 | Glyphosate content (%) | 1.532 | 0.017 | 98.9％ |
| 2 | Sodium chloride content (%) | 20.1 | 0.2 | 99.0％ |
| 3 | CODcr(mg/l) | 58620 | 2054 | 96.5％ |
Embodiment 2:
A kind of pretreatment process of glyphosate production wastewater, implement according to the following steps:
(1) regulates pH value
To contain 1.066% glyphosate, 15.3% sodium-chlor, the CODcr value is that 38912 glyphosate production wastewater 2000 liters (proportion 1.22 grams per milliliters) enters equalizing tank, adds 30% hydrochloric acid soln in equalizing tank, and the pH value of waste water in the pond is adjusted to 3;
(2) catalyzed oxidation
With regulating pH value is that waste water after 3 enters one-level catalyzed oxidation tower, go into 40000 litres of air from the tower pucking, and in one-level catalyzed oxidation tower, add by 30% hydrogen peroxide and ferrous sulfate by weight than being 200 liters of the catalytic oxidant Fenton reagent that are mixed with at 3: 1, reaction treatment 1.5 hours; And then waste water entered secondary catalyzed oxidation tower, and go into 40000 litres of air from the tower pucking, in secondary catalyzed oxidation tower, add available chlorine content and be 100 liters of 7% chlorine bleach liquores, reaction treatment 1.5 hours; Behind catalytic oxidation, most of organophosphorus is converted into inorganic phosphorus in the waste water, and some organism is oxidized to small molecules or CO2 in the reaction, and partial organic substances oxidative coupling then takes place generates hydrophobic macromole.
(3) calcification dephosphorization
Waste water behind the catalyzed oxidation is entered in the dephosphorization reaction tank, add 248 kilograms in dephosphorization agent 82% calcium chloride, reaction treatment 1.5 hours; To contain sedimentary waste water then and carry out press filtration by plate-and-frame filter press, throw out is removed after being become filter cake by press filtration.Inorganic phosphorus behind catalyzed oxidation in the waste water and dephosphorization agent calcium chloride react and generate the calcium phosphate precipitation thing, use plate-and-frame filter press the more sedimentary waste water of phosphorous hydrochlorate is carried out press filtration, throw out is removed after being become filter cake by press filtration, can remove most organophosphoruss and suspended substance in the glyphosate production wastewater.
(4) the triple effect evaporation crystallization removes sodium-chlor
To enter the triple effect evaporation device through the waste water after the calcification dephosphorization, feeding steam carries out stepped evaporation and concentrates, and I is imitated the evaporated vapor pressure-controlling at 0.50～0.65Mpa, and wastewater temperature is controlled at 130～155 ℃; II is imitated the evaporated vapor pressure-controlling at 0.2～0.35Mpa, and wastewater temperature is controlled at 100～130 ℃; III is imitated the control of evaporated vapor pressure at 0.03～0.06Mpa, and wastewater temperature is controlled at 80～90 ℃, vacuum degree control-0.09～-0.075Mpa; The time that waste water carries out triple effect evaporation is 1.5 hours; The waste water that contains crystallization sodium-chlor after the triple effect evaporation is carried out solid-liquid separation by wet cyclone, isolate crystallization sodium-chlor and waste water, then crystallization sodium-chlor is carried out centrifugally, the centrifugal liquid that goes out returns the dephosphorization reaction tank and reacts dephosphorization once more.The continuous desalination of process triple effect evaporation can be removed the most sodium-chlor in the glyphosate waste water, the sodium-chlor quality height of extraction, and impurity is few, can recycle.
After testing, the every index through pretreated glyphosate production wastewater changes as follows:
| Sequence number | Index name | Before the processing | After the processing | Clearance (%) |
| 1 | Glyphosate content (%) | 1.066 | 0.013 | 98.8％ |
| 2 | Sodium chloride content (%) | 15.3 | 0.2 | 98.7％ |
| 3 | CODcr(mg/l) | 38912 | 1826 | 95.3％ |
Embodiment 3:
A kind of pretreatment process of glyphosate production wastewater, implement according to the following steps:
(1) regulates pH value
To contain 1.68% glyphosate, 18.5% sodium-chlor, the CODcr value is that 50112 glyphosate production wastewater 5000 liters (proportion 1.25 grams per milliliters) enters equalizing tank, adds 30% hydrochloric acid soln in equalizing tank, and the pH value of waste water in the pond is adjusted to 4;
(2) catalyzed oxidation
With regulating pH value is that waste water after 4 enters one-level catalyzed oxidation tower, go into 125000 litres of air from the tower pucking, and in one-level catalyzed oxidation tower, add by 30% hydrogen peroxide and ferrous sulfate by weight than being 250 liters of the catalytic oxidant Fenton reagent that are mixed with at 8: 1, reaction treatment 2 hours; And then waste water entered secondary catalyzed oxidation tower, and go into 125000 litres of air from the tower pucking, in secondary catalyzed oxidation tower, add available chlorine content and be 100 liters of 10% chlorine bleach liquores, reaction treatment 2 hours; Behind catalytic oxidation, most of organophosphorus is converted into inorganic phosphorus in the waste water, and some organism is oxidized to small molecules or CO2 in the reaction, and partial organic substances oxidative coupling then takes place generates hydrophobic macromole.
(3) calcification dephosphorization
Waste water behind the catalyzed oxidation is entered in the dephosphorization reaction tank, add 508.1 kilograms in dephosphorization agent 82% calcium chloride, reaction treatment 2 hours; To contain sedimentary waste water then and carry out press filtration by plate-and-frame filter press, throw out is removed after being become filter cake by press filtration.Inorganic phosphorus behind catalyzed oxidation in the waste water and dephosphorization agent calcium chloride react and generate the calcium phosphate precipitation thing, use plate-and-frame filter press the more sedimentary waste water of phosphorous hydrochlorate is carried out press filtration, throw out is removed after being become filter cake by press filtration, can remove most organophosphoruss and suspended substance in the glyphosate production wastewater.
(4) the triple effect evaporation crystallization removes sodium-chlor
To enter the triple effect evaporation device through the waste water after the calcification dephosphorization, feeding steam carries out stepped evaporation and concentrates, and I is imitated the evaporated vapor pressure-controlling at 0.50～0.65Mpa, and wastewater temperature is controlled at 130～155 ℃; II is imitated the evaporated vapor pressure-controlling at 0.2～0.35Mpa, and wastewater temperature is controlled at 100～130 ℃; III is imitated the control of evaporated vapor pressure at 0.03～0.06Mpa, and wastewater temperature is controlled at 80～90 ℃, vacuum degree control-0.09～-0.075Mpa; The time that waste water carries out triple effect evaporation is 1.5 hours; The waste water that contains crystallization sodium-chlor after the triple effect evaporation is carried out solid-liquid separation by wet cyclone, isolate crystallization sodium-chlor and waste water, then crystallization sodium-chlor is carried out centrifugally, the centrifugal liquid that goes out returns the dephosphorization reaction tank and reacts dephosphorization once more.The continuous desalination of process triple effect evaporation can be removed the most sodium-chlor in the glyphosate waste water, the sodium-chlor quality height of extraction, and impurity is few, can recycle.
After testing, the every index through pretreated glyphosate production wastewater changes as follows:
| Sequence number | Index name | Before the processing | After the processing | Clearance (%) |
| 1 | Glyphosate content (%) | 1.68 | 0.033 | 98.0％ |
| 2 | Sodium chloride content (%) | 18.5 | 0.3 | 98.4％ |
| 3 | CODcr(mg/l) | 50112 | 3190 | 93.6％ |
Claims (5)
1. the pretreatment process of a glyphosate production wastewater may further comprise the steps composition:
(1) regulates the pH value
Glyphosate production wastewater is entered equalizing tank, in equalizing tank, add hydrochloric acid soln, the pH value of waste water in the pond is adjusted to 3～4;
(2) catalyzed oxidation
With regulating back pH value is that 3～4 waste water enters one-level catalyzed oxidation tower, go into air from the tower pucking of catalyzed oxidation tower, and add by 30% hydrogen peroxide and ferrous sulfate by weight than being 3: 1～8: 1 formulated Fenton reagent, the Fenton reagent that is added and the volume ratio of waste water are 1: 10～1: 20, fully react; Then waste water is entered secondary catalyzed oxidation tower, go into air from the tower pucking of catalyzed oxidation tower, and to add available chlorine content be 7～10% chlorine bleach liquor, and the chlorine bleach liquor who is added and the volume ratio of waste water are 1: 20～1: 50, fully react;
(3) calcification dephosphorization
Waste water behind catalyzed oxidation is entered in the dephosphorization reaction tank, add dephosphorization agent calcium chloride, after fully reacting, will contain sedimentary waste water and carry out press filtration, throw out is removed after by press filtration;
(4) the triple effect evaporation crystallization removes sodium-chlor
To enter the triple effect evaporation device through the waste water after the calcification dephosphorization, feeding steam carries out stepped evaporation and concentrates, and I is imitated the evaporated vapor pressure-controlling at 0.50～0.65Mpa, and wastewater temperature is controlled at 130～155 ℃; II is imitated the evaporated vapor pressure-controlling at 0.2～0.35Mpa, and temperature is controlled at 100～130 ℃; III is imitated the control of evaporated vapor pressure at 0.03～0.06Mpa, and temperature is controlled at 80～90 ℃, vacuum degree control-0.09～-0.075Mpa; The waste water that will contain crystallization sodium-chlor after triple effect evaporation carries out solid-liquid separation, isolates crystallization sodium-chlor and waste water, crystallization sodium-chlor is carried out centrifugally again, and the centrifugal liquid that goes out returns the dephosphorization reaction tank and carries out dephosphorization once more.
2. the pretreatment process of a kind of glyphosate production wastewater according to claim 1, it is characterized in that, in described step (2) catalyzed oxidation, the amount of going into air from the tower pucking of one-level catalyzed oxidation tower and secondary catalyzed oxidation tower is respectively: the air that blasts and the volume ratio of waste water are 20: 1～25: 1.
3. the pretreatment process of a kind of glyphosate production wastewater according to claim 1 is characterized in that, in described step (3) the calcification dephosphorization, the amount of the dephosphorization agent calcium chloride that is added is: the weight part ratio of rolling over hundred calcium chloride and waste water is 1: 12～1: 15.
4. the pretreatment process of a kind of glyphosate production wastewater according to claim 1 is characterized in that, in described step (3) the calcification dephosphorization, will contain sedimentary waste water and carry out press filtration for to carry out press filtration by plate-and-frame filter press.
5. the pretreatment process of a kind of glyphosate production wastewater according to claim 1, it is characterized in that, described step (4) triple effect evaporation crystallization removes in the sodium-chlor, and the waste water that will contain crystallization sodium-chlor after triple effect evaporation carries out solid-liquid separation for to carry out solid-liquid separation by wet cyclone.
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