CN101428935A - Treatment process for wastewater from N-(Phosphonomethyl)iminodiacetic acid production - Google Patents
Treatment process for wastewater from N-(Phosphonomethyl)iminodiacetic acid production Download PDFInfo
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Abstract
The invention discloses a method for treating PMIDA (N-(phosphonomethyl)iminodiacetic acid) production wastewater, which comprises the following steps: 1) the PMIDA production wastewater is sent into equipment with a compound evaporator and a vacuum system, and is separated into a saturated concentrated solution containing sodium chloride and evaporable water at a steam pressure of between 0.1 and 0.4MPa and a vacuum degree of between 0.05 and 0.08MPa; the concentrated solution containing the sodium chloride is cooled to crystallize the sodium chloride; and the solid-liquid separation is performed; 2) separating medium is sent into a curing container, a curing agent is added, and innoxious solid mud and a filtrate are obtained after the washing and filtration; 3) after the evaporable water and the filtrate are mixed, a neutralizing agent is used to adjust the pH value to between 6 and 8; 4) an oxidant is added in neutralized wastewater for oxidation; and 5) a treated oxidized liquid is aerated and then enters the prior biochemical system to obtain treated water. The method can greatly reduce the treatment cost for the PMIDA production wastewater, can also extract partial useful constituents in the PMIDA production wastewater, can be recycled, and is favorable for the environmental protection.
Description
Technical field:
The present invention is relevant with the Chemical Manufacture wastewater treatment method, and is special relevant with the treatment process of pmida98 factory effluent.
Background technology:
Be raw material with iminodiacetonitrile or iminodiethanoic acid, alkaline hydrolysis synthesis of iminodiacetic acid sodium salt, in the synthetic pmida98 explained hereafter of phosphine formylation reaction, the fractionate aqueous solutions after isolating the pmida98 solid phase prod is the pmida98 factory effluent again.Contain 05～5% pmida98 in the pmida98 factory effluent, 1～7%HCl, 0.5～5% phosphorous acid, 0.5～3% formaldehyde, 8～18% sodium-chlor etc.This waste water need carry out wastewater treatment because direct discharging pollutes the environment.
Pmida98 production wastewater treatment method in the past has following three kinds:
1, the technology of Shenyang Chemical Engineering Inst exploitation be with in the alkaline matters such as lime and waste water to neutral, make the pmida98 in the waste water resolve into inorganic phosphorus and make it precipitation, lime adding amount is 3～5% of a Total Water.Treated sodium-chlor in its solution and formaldehyde content enough hour, and just allowed it enter biochemical system and handle.This method needs jumbo container, and the waste residue of generation is many especially, needs filter cleaner at any time, and this method processing costs is higher, the construction investment height, and floor space is big.
2, in the U.S. Pat 6515168, U.S. monsanto company once reported a kind of N-(phosphonomethyl) iminodiacetic acid wastewater treatment technology.In this technology, be that N-(phosphonomethyl) iminodiacetic acid wastewater is placed in the evaporating kettle, heating evaporation after waiting to salt out, filters out salt, and the filtering and concentrating liquid of generation returns in the pmida98 Production Flow Chart.This technology does not provide the wastewater treatment method that evaporates, simultaneously, because the number of times of cyclically utilizing filtering and concentrating liquid is limited, to can also providing the good treatment method by the round-robin waste liquid.
3, the treatment technology of domestic some producer is that the pmida98 factory effluent is sent into incinerator, feeds oil fuel, is burned.The shortcoming of this method is:
1) burn waste water with fuel, burning operation is loaded down with trivial details, and instability, processing cost are very high;
2) burn the later stage, owing in the waste water sodium-chlor is arranged, this salt is easy to crystallization on the wall of incinerator, accumulation, if operate badly, the danger of fryer is arranged;
3) owing in the burning process, have the situation of incomplete combustion, produce and pollute waste gas for the second time, need to build a cover exhaust treatment system, handled the back qualified discharge.
But, after handling by above-mentioned three kinds of methods, N-(phosphonomethyl) iminodiacetic acid wastewater to reach emission standard, need very big processing cost, so just increased the processing cost of pmida98 factory effluent widely.
Summary of the invention:
The objective of the invention is in order to overcome above deficiency, a kind of processing cost that not only can reduce the pmida98 factory effluent greatly is provided, and the part useful component in the pmida98 factory effluent can be extracted again, recycle, be beneficial to the treatment process of the pmida98 factory effluent of environmental protection.
The object of the present invention is achieved like this:
The treatment process of pmida98 factory effluent of the present invention, this method may further comprise the steps:
1) the pmida98 factory effluent being sent into one is with in the equipment of multiple-effect evaporator and the vacuum system that is connected to the multiple-effect evaporator afterbody, at vapor pressure is that 0.1～0.4MPa and vacuum tightness are under the condition of 0.05～0.08MPa, the pmida98 factory effluent is separated into the saturated concentrated solution and the vaporize water of sodium chloride-containing, the saturated concentrated solution of sodium chloride-containing is after cooling, crystallization goes out sodium-chlor, solid-liquid separation is wet sodium-chlor and parting liquid, and the content of sodium-chlor is 80～91% in the wet sodium-chlor; Formaldehyde content is 1.0～6.0% in the vaporize water, and HCl content is 1.0～8.0%, and pH is 0.5～3.0; Pmida98 content is 5.0～13% in the parting liquid, and formaldehyde content is 0.5～2.0%, and phosphorous acid content is 8.0～15.0%;
2) parting liquid is sent in the curing vessel, add solidifying agent, by weight, solid formulation: parting liquid=3～10: 100, pmida98 in the parting liquid, phosphorous acid etc. generate lenticular blended solid mud with its reaction, behind the washing and filtering, obtain phosphorous and harmless solid mud and filtrate nitrogen, harmless solid mud imbed in the soil or burn or sell all can, outstanding Wi-4 solidifying agent of the one-tenth that solidifying agent adopts the Sichuan of outsourcing to become outstanding Environmental Protection Technology Co., Ltd to produce;
3) after the filtrate vaporize water and the step 2 that step (1) is evaporated) is mixed, send into equalizing tank in mixing tank, regulate pH to 6～8 with neutralizing agent;
4) in and add oxygenant in the waste water, carry out oxidation, and then blast air and continue oxidation, the concentration of formaldehyde in the waste water is handled 0.1～0.3%, the chemical oxygen demand cod in the waste water
CrCan drop to 3000～11000PPm;
5) the oxidation liquid that will handle through entering routine biochemistry systems such as anaerobic pond, Aerobic Pond, settling bowl, sand filter, clean water basin successively behind the preaeration tank aeration, obtains treating water, and cod codcr can drop to 80～150PPm in the treating water;
After above-mentioned sodium-chlor is handled through recrystallization, make sodium chloride content and be 〉=99% refining sodium chloride salt.
Above-mentioned neutralizing agent is at least a in sodium hydroxide, calcium hydroxide, potassium hydroxide, ammonia, ammoniacal liquor, calcium oxide, yellow soda ash, lime carbonate, the sodium bicarbonate, and oxygenant is a hydrogen peroxide, and dioxide peroxide is airborne at least a.
Adopt 2nd effect evaporator in the above-mentioned equipment, the thermal source of first single-effect evaporator is supplied with by the water vapor that boiler produces, the heating source of second single-effect evaporator is the evaporation steam that first single-effect evaporator produces, and vacuum system is connected to the second single-effect evaporator afterbody, can save heat energy greatly.
Adopt triple-effect evaporator in the above-mentioned equipment, the thermal source of first single-effect evaporator is supplied with by the water vapor that boiler produces, the heating source of second single-effect evaporator is that the evaporation steam of first single-effect evaporator generation and the heating source of third effect evaporator are the evaporation steam that second single-effect evaporator produces, vacuum system is connected to the third effect evaporator afterbody, can save heat energy greatly.
The treatment process of pmida98 factory effluent of the present invention not only can reduce the processing cost of pmida98 factory effluent greatly, and the part useful component in the pmida98 factory effluent can be extracted, and recycles, and is beneficial to environmental protection.
Embodiment
Below equipment among each embodiment be the equipment that adopts the band triple-effect evaporator of buying on the market and be connected to the vacuum system of third effect evaporator afterbody.
Embodiment 1:
The speed of pmida98 factory effluent with 16 cubic metres/hour is pumped in the triple-effect evaporator of 400 cubic metres/day of cover treatment capacities, (vacuum tightness is 0.05～0.08MPa) and feeds steam (vapor pressure is 0.1～0.4MPa) heating evaporation pmida98 factory effluent to start vacuum system, 9 cubic metres/hour of evaporated waters, vaporize water is put into a reception tank, the concentrated solution of the sodium chloride-containing that triple-effect evaporator pumps enters crystallizer, after treating that the salt crystallization goes out, about 5 cubic metres/hour of 87～91% sodium-chlor wet feed 1830kg/ hour and parting liquid isolated sodium chloride content and is in centrifugation; Parting liquid solidifies in the pond by being pumped into one for about 5 cubic metres/hour, add 200kg/ hour solidifying agent (becoming outstanding Wi-4) make its curing, move into solid-liquid separation in the separator then, obtain 1 ton of/hour harmless solid mud (or landfill, or burn, or sell) and 4.2 tons of/hour filtrates; By 4.2 tons/hour filtrates with send into equalizing tank after 9 cubic metres of/hour vaporize waters mix, hydro-oxidation sodium is neutralized into pH=6-8; Be accumulated to 130 ton hours, add 1.3 tons in oxygenant mass percentage concentration 27% hydrogen peroxide, circulated 2～6 hours, blast atmospheric oxidation 4-8 hours again, treat that concentration of formaldehyde reaches at 0.1～0.3% o'clock, entered the preaeration tank aeration again 6～12 hours, and sent into biochemical treatment system continuously with 20 cubic metres/speed at one hour rating then, the clear water COD after the processing
CrDrop to 80～150PPm.
Embodiment 2:
The speed of pmida98 factory effluent with 8 cubic metres/hour is pumped in the triple-effect evaporator of 400 cubic metres/day of cover treatment capacities, (vacuum tightness is 0.05～0.08MPa) and feeds steam (vapor pressure is 0.1～0.4MPa) heating evaporation pmida98 factory effluent to start vacuum system, 4.5 cubic metres/hour of evaporated waters, vaporize water is put into a reception tank, the concentrated solution of the sodium chloride-containing that triple-effect evaporator pumps enters crystallizer, after treating that the salt crystallization goes out, about 2.6 cubic metres/hour of 87～91% sodium-chlor wet feed 930kg/ hour and parting liquid isolated sodium chloride content and is in centrifugation; Parting liquid solidifies in the pond by being pumped into one for about 2.6 cubic metres/hour, add 100kg/ hour solidifying agent (becoming outstanding Wi-4) make its curing, move into solid-liquid separation in the separator then, obtain 0.5 ton of/hour harmless solid mud (or landfill or burn, or sell) and 2.2 tons of/hour filtrates; With 2.2 tons/hour filtrates with send into equalizing tank after 4.5 cubic metres of/hour vaporize waters mix, hydro-oxidation sodium is neutralized into pH=6～8, be accumulated to 70 ton hours, add the oxygenant mass percentage concentration and be 0.7 ton in 27% hydrogen peroxide, circulated 2～4 hours, blasted atmospheric oxidation again 4～8 hours, when treating that concentration of formaldehyde reaches 0.1-0.3%, enter in the preaeration tank aeration again 6～12 hours, and sent into biochemical treatment system continuously with 20 cubic metres/speed at one hour rating then, the clear water COD after the processing
CrDrop to 80～150PPm.
Embodiment 3:
The speed of pmida98 factory effluent with 12 cubic metres/hour is pumped in the triple-effect evaporator of 400 cubic metres/day of cover treatment capacities, (vacuum tightness is 0.05～0.08MPa) and feeds steam (vapor pressure is 0.1～0.4MPa) heating evaporation pmida98 factory effluent to start vacuum system, 6.7 cubic metres of vaporize waters of evaporated water are put into a reception tank, the concentrated solution of the sodium chloride-containing that triple-effect evaporator pumps enters crystallizer, after treating that the salt crystallization goes out, about 3.7 cubic metres/hour of 87～91% sodium-chlor wet feed 1340kg/ hour and parting liquid isolated sodium chloride content and is in centrifugation; Parting liquid solidifies in the pond by being pumped into one for about 3.7 cubic metres/hour, add 150kg/ hour solidifying agent (becoming outstanding Wi-4) make its curing, move into solid-liquid separation in the separator then, obtain 1 ton of/hour harmless solid mud (or landfill, or burn, or sell) and 6.4 tons of/hour filtrates; With 6.4 tons/hour filtrates with send into equalizing tank after 6.7 cubic metres of/hour vaporize waters mix, hydro-oxidation sodium is neutralized into pH=6～8, be accumulated to 95 ton hours, adding the oxygenant mass percentage concentration is 0.93 ton in 27% hydrogen peroxide, circulates 2～6 hours, blasts atmospheric oxidation again 4～8 hours, treat concentration of formaldehyde processing at least 0.1～0.3% o'clock, entered the preaeration tank aeration again 6～12 hours, and sent into biochemical treatment system continuously with 20 cubic metres/speed at one hour rating then, the clear water COD after the processing
CrDrop to 80～150PPm.
Embodiment 4:
The speed of pmida98 factory effluent with 16 cubic metres/hour is pumped in the triple-effect evaporator of 400 cubic metres/day of cover treatment capacities, (vacuum tightness is 0.05～0.08MPa) and feeds steam (vapor pressure is 0.1～0.4MPa) heating evaporation pmida98 factory effluent to start vacuum system, 9 cubic metres of/hour vaporize waters of evaporated water are put into a reception tank, the concentrated solution of the sodium chloride-containing that triple-effect evaporator pumps enters crystallizer, after treating that the salt crystallization goes out, centrifugation: isolate sodium chloride content and be about 5 cubic metres/hour of 87～91% sodium-chlor wet feed 1800kg/ hour and parting liquid; Parting liquid solidifies in the pond by being pumped into one for about 5 cubic metres/hour, add 200kg/ hour solidifying agent (becoming outstanding Wi-4) make its curing, move into solid-liquid separation in the separator then, obtain 1 ton of/hour harmless solid mud (or landfill, or burn, or sell) and 4.4 tons of/hour filtrates; With 4.4 tons/hour filtrates with send into equalizing tank after 9 cubic metres of/hour vaporize waters mix, hydro-oxidation sodium is neutralized into neutrality, be accumulated to 130 ton hours, adding the oxygenant mass percentage concentration is 1.3 tons in 27% hydrogen peroxide, circulates 2～6 hours, blasted atmospheric oxidation again 4～8 hours, treat that concentration of formaldehyde handled at 0.1～0.3% o'clock, enter preaeration tank again, aeration 6～12 hours, send into biochemical treatment system continuously with 20 cubic metres/speed at one hour rating then, the clear water COD after the processing
CrDrop to 80～150PPm.
Embodiment 5:
The speed of pmida98 factory effluent with 16 cubic metres/hour is pumped in the triple-effect evaporator of 400 cubic metres/day of cover treatment capacities, (vacuum tightness is 0.05～0.08MPa) and feeds steam (vapor pressure is 0.1～0.4MPa) heating evaporation pmida98 factory effluent to start vacuum system, 9 cubic metres/hour of evaporated waters, vaporize water is put into a reception tank, the concentrated solution of the sodium chloride-containing that triple-effect evaporator pumps enters crystallizer, after treating that the salt crystallization goes out, 5 cubic metres/hour of 87～91% sodium-chlor wet feed 1800kg/ hour and parting liquids are isolated sodium chloride content and are in centrifugation; Parting liquid solidifies in the pond by being pumped into one for about 5 cubic metres/hour, add 200kg/ hour solidifying agent (becoming outstanding Wi-4) make its curing, move into solid-liquid separation in the separator then, obtain 1 ton of/hour harmless solid mud (or landfill, or burn, or sell) and 4.2 tons/hour filtrate; With 4.2 tons/hour filtrates with send into equalizing tank after 9 cubic metres of/hour vaporize waters mix, hydro-oxidation sodium is neutralized into neutrality, be accumulated to 130 ton hours, adding the oxygenant mass percentage concentration is 2.6 tons in 27% hydrogen peroxide, circulates 2～6 hours, blast atmospheric oxidation 4-8 hours again, treat that concentration of formaldehyde reaches at 0.1～0.3% o'clock, enter the pre-exposure pond again, aeration 6～12 hours, send into biochemical treatment system continuously with 20 cubic metres/speed at one hour rating then, the clear water COD after the processing
CrDrop to 80～120PPm.
Embodiment 6:
The speed of pmida98 factory effluent with 16 cubic metres/hour is pumped in the triple-effect evaporator of 400 cubic metres/day of cover treatment capacities, (vacuum tightness is 0.05～0.08MPa) and feeds steam (vapor pressure is 0.1～0.4MPa) heating evaporation pmida98 factory effluent to start vacuum system, 9 cubic metres/hour of evaporated waters, vaporize water is put into a reception tank, the concentrated solution of the sodium chloride-containing that triple-effect evaporator pumps enters crystallizer, after treating that the salt crystallization goes out, about 5 cubic metres/hour of 87～91% sodium-chlor wet feed 1800kg/ hour and parting liquid isolated sodium chloride content and is in centrifugation; Parting liquid solidifies in the pond by being pumped into one for about 5 cubic metres/hour.Add 200kg/ hour solidifying agent and make its curing, move into solid-liquid separation in the separator then, obtain 1 ton of/hour harmless solid mud (or landfill, or burn, or sell) and 4.2 tons of/hour filtrates; By 4.2 tons/hour filtrates with send into equalizing tank after 9 cubic metres of/hour vaporize waters mix, hydro-oxidation sodium is neutralized into neutrality, be accumulated to 130 ton hours, adding the oxygenant mass percentage concentration is 5.0 tons in 27% hydrogen peroxide, circulates 4～6 hours, blasts atmospheric oxidation 4-8 hours again, treat that concentration of formaldehyde reaches at 0.1～0.3% o'clock, enter in the preaeration tank aeration again 6～12 hours, and sent into biochemical treatment system continuously with 20 cubic metres/speed at one hour rating then, the clear water COD after the processing
CrDrop to 80～100PPm.
The various embodiments described above are that foregoing of the present invention is further described, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to the foregoing description.All technology that realizes based on foregoing all belong to scope of the present invention.
Claims (5)
1, the treatment process of pmida98 factory effluent, this method may further comprise the steps:
1) the pmida98 factory effluent is sent into one be with multiple-effect evaporator and be connected to the multiple-effect evaporator afterbody vacuum system equipment in, at vapor pressure is that 0.1～0.4MPa and vacuum tightness are under the condition of 0.05～0.08MPa, the pmida98 factory effluent is separated into the saturated concentrated solution and the vaporize water of sodium chloride-containing, the saturated concentrated solution of sodium chloride-containing is after cooling, crystallization goes out sodium-chlor, and solid-liquid separation is wet sodium-chlor and parting liquid;
2) parting liquid is sent in the curing vessel, added solidifying agent, by weight, solidifying agent: parting liquid=3～10: 100, behind the washing and filtering, obtain phosphorous and harmless solid mud and filtrate nitrogen;
3) after the filtrate vaporize water and the step 2 that step (1) is evaporated) is mixed, send into equalizing tank in mixing tank, regulate pH to 6～8 with neutralizing agent;
4) in and add oxygenant in the waste water and carry out oxidation, and then blast air and continue oxidation the concentration of formaldehyde in the waste water is handled 0.1～0.3%;
5) the oxidation liquid that will handle through entering anaerobic pond, Aerobic Pond, settling bowl, sand filter, clean water basin routine biochemistry system successively behind the preaeration tank aeration, obtains treating water.
2, the treatment process of pmida98 factory effluent as claimed in claim 1 after it is characterized in that sodium-chlor handled through recrystallization, is made sodium chloride content and is 〉=99% refining sodium chloride salt.
3, the treatment process of pmida98 factory effluent as claimed in claim 1 or 2, it is characterized in that neutralizing agent is at least a in sodium hydroxide, calcium hydroxide, potassium hydroxide, ammonia, ammoniacal liquor, calcium oxide, yellow soda ash, lime carbonate, the sodium bicarbonate, oxygenant is hydrogen peroxide, dioxide peroxide, airborne at least a.
4, require the treatment process of 1 or 2 described pmida98 factory effluents as profit, it is characterized in that adopting in the equipment 2nd effect evaporator.
5, require the treatment process of 1 or 2 described pmida98 factory effluents as profit, it is characterized in that adopting in the equipment triple-effect evaporator.
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| CN101974032A (en) * | 2010-10-18 | 2011-02-16 | 浙江拜克开普化工有限公司 | Method for recycling N-(Phosphonomethyl)iminodiaceticacid (PMIDA) in PMIDA production wastewater, application and special device |
| CN102033066A (en) * | 2010-11-22 | 2011-04-27 | 重庆紫光化工股份有限公司 | Method for analyzing components of mother solution of glyphosine |
| CN102115281A (en) * | 2011-01-18 | 2011-07-06 | 中国中化股份有限公司 | Method for pretreating wastewater generated in production of N-(Phosphonomethyl) iminodiaceticacid (PMIDA) |
| CN102198989A (en) * | 2011-04-22 | 2011-09-28 | 安徽国星生物化学有限公司 | Method for treating PMIDA wastewater |
| CN101671076B (en) * | 2009-09-01 | 2012-01-25 | 山东先达化工有限公司 | Oxidative degradation process for imidazolinone herbicide wastewater |
| CN102674638A (en) * | 2010-10-18 | 2012-09-19 | 浙江拜克开普化工有限公司 | Device for recycling N-Phosphonomethyl aminodiacetic acid from waste water in N-Phosphonomethyl aminodiacetic acid production process |
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| CN105440074A (en) * | 2014-09-30 | 2016-03-30 | 北京紫光英力化工技术有限公司 | Recycling method for mother liquor of N-(phosphonomethyl)iminodiacetic acid |
| CN105440074B (en) * | 2014-09-30 | 2018-05-22 | 北京紫光英力化工技术有限公司 | A kind of method that pmida Recycling Mother Solution is applied mechanically |
| CN108946850A (en) * | 2018-08-14 | 2018-12-07 | 河北蓝江生物环保科技有限公司 | Evaporate the Retreatment method of raffinate |
| CN108946850B (en) * | 2018-08-14 | 2021-07-16 | 河北蓝江生物环保科技有限公司 | Method for reprocessing evaporation raffinate |
| CN110937727A (en) * | 2019-12-26 | 2020-03-31 | 河南省科学院化学研究所有限公司 | PROBAN flame-retardant wastewater treatment method |
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