CN106698791A - Crystallization treatment process for ammonium salt in paraquat wastewater - Google Patents
Crystallization treatment process for ammonium salt in paraquat wastewater Download PDFInfo
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- CN106698791A CN106698791A CN201710004706.9A CN201710004706A CN106698791A CN 106698791 A CN106698791 A CN 106698791A CN 201710004706 A CN201710004706 A CN 201710004706A CN 106698791 A CN106698791 A CN 106698791A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/041—Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/18—Cyanides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/306—Pesticides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/026—Treating water for medical or cosmetic purposes
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Abstract
The invention provides a crystallization treatment process for an ammonium salt in paraquat wastewater. The crystallization treatment process comprises the following steps: recycling amino from washing wastewater of a paraquat synthesis filter pressing section by using a stripping tower, breaking cyanogens by using a cyanogens breaking tower, transferring into an acid dropping kettle, adjusting the pH value, introducing into a mechanical steam re-compression evaporator for evaporation concentration, finally transferring into a cooling kettle, and adding a separation acceleration reagent to accelerate separation of the ammonium salt, thereby reducing the yield ratio of a centrifugal mother liquid. The amount of the centrifugal mother liquid can be reduced to 2-3% from 7-10% of that of conventional process wastewater, the ammonium salt separation amount is increased by 4-7%, and the cost of centrifugal mother liquid combustion can be lowered.
Description
Technical field
The present invention relates to herbicide wastewater processing technology field, and in particular in a kind of paraquat waste water at the crystallization of ammonium salt
Science and engineering skill.
Background technology
Paraquat, chemical name is 1-1- dimethyl -4-4- bipyridine cation salt, is a kind of quick total weed control
Agent, with good interior suction, conductive performance, can be absorbed by plant green tissues rapidly makes its withered.Country's ammonia cyanogen method life at present
Production. art obtains important breakthrough, and its technique has many good qualities, and the market competitiveness is also very strong, but the waste water produced in its building-up process
Process problem fails to be solved.For the recovery of ammonium salt in paraquat waste water, most domestic enterprise is steamed using multiple-effect
Hair method or MVR enter centrifuge under cooling reactor crystallization, continuous operation are transferred to after being concentrated by evaporation, and solid is used to be combined after collecting
Fertilizer production, through cell and field experiment, without poisoning and other harmful effects.The centrifuge mother liquor after ammonium salt is separated out to enter at incinerator
Reason.But during cooling reactor crystallization, ammonium salt reclamation amount is on the low side, the centrifuge mother liquor of generation reaches the 7-10% of wastewater flow rate, burns cost
It is too high.Increasingly serious with Environmental Protection Situation, paraquat waste water reclaiming problem is outstanding day by day, progressively synthesizes as paraquat and looks forward to
One key of industry existence.In this context, while paraquat production new technique is accelerated, utilization of wastewater resource with
And minimum discharge Processing Technology Research is also very crucial.Therefore, to the yield of ammonium salt in raising paraquat waste water, centrifugation is reduced
It is significant that the process of mother liquor content carries out Improvement.
The content of the invention
In view of the shortcomings of the prior art, the invention provides ammonium in a kind of crystallization efficiency high, easy-operating paraquat waste water
The crystallization treatment technique of salt.
To realize object above, the present invention is achieved by the following technical programs：
The crystallization treatment technique of ammonium salt, comprises the following steps in a kind of paraquat waste water：
1) washes of paraquat synthesis press filtration workshop section is reclaimed into ammonia through stripper；
2) waste water reclaimed after ammonia is passed into broken cyanide tower carries out broken cyanide treatment；
3) waste water after broken cyanide is transferred in the sour kettle of drop and adjusts pH；
4) waste water adjusted after pH is passed through and concentration is evaporated in mechanical steam recompression evaporator；
5) waste water after evaporation and concentration is transferred to cooling reactor, is added thereto to promote the precipitation that analysis reagent promotes ammonium salt, subtracted
Few centrifuge mother liquor amount；The analysis reagent that promotees is selected from NH4Any one in Cl crystal seeds, the concentrated sulfuric acid, anti-solvent, or the concentrated sulfuric acid and
NH4Cl crystal seeds.
Preferably, the step 1) mass fraction of ammonia is 22% in washes, after reclaiming ammonia through stripper, in discharging
The mass fraction of ammonia is 4%, and cyanogen root concentration is 18.3g/L.
Preferably, the step 2) broken cyanide treatment is that waste water is passed through into broken cyanide tower, and to adding 37% formaldehyde in tower,
30% soda bath is added after 0.5h, is discharged after 2h, cyanogen root content is 65mg/L.
Preferably, the step 3) pH to 6-7 is adjusted using 93% concentrated sulfuric acid in the sour kettle of drop.
Preferably, the step 4) in be concentrated by evaporation remove 50%-60%.
Preferably, the step 5) promote ammonium salt to separate out to adjust pH to 4-5 using toward dripping 93% concentrated sulfuric acid in cooling reactor.
Preferably, the step 5) promote ammonium salt to separate out to adjust pH to 4-5 using toward dripping 93% concentrated sulfuric acid in cooling reactor, then
Crystal seed NH is delivered toward cooling reactor4Cl, Seed charge is the 0.3%-0.5% of ammonium salt output.
Preferably, the step 5) promote ammonium salt precipitation to use the dispensing crystal seed NH toward cooling reactor4Cl, Seed charge is
The 0.3%-0.5% of ammonium salt output.
Preferably, the step 5) promote ammonium salt to separate out using toward adding anti-solvent, anti-solvent adding rate in cooling reactor
It is 10-20kgmin-1(10m3Kettle), anti-solvent addition is the 1/5-1/3 of feed liquid.
Preferably, the anti-solvent is methyl alcohol or ethanol.
Beneficial effect of the present invention：The present invention increased and promote analysis reagent work to addition in cooling reactor on the basis of existing process
Sequence, using toward drop acid in cooling reactor or input crystal seed or addition anti-solvent, increases ammonium salt crystallization amount, so as to reduce centrifuge mother liquor
Yield ratio, it is and reusable after anti-solvent ethanol steams again.Using process of the invention, ammonium salt amount of precipitation increases 4-
7%, centrifuge mother liquor reduces 5% or so, and last centrifuge mother liquor burning amount only has the 2-3% of initial waste water, reduces centrifuge mother liquor
The cost of burning, and process is easy to realization of industrialization.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Embodiment 1：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 590Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and after centrifuge, ammonium salt output 2.9t, centrifuge mother liquor 750Kg burns into incinerator
Burn.
Embodiment 2：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, into broken cyanide
The formaldehyde of 464Kg 37% is added in tower, broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, cyanogen root content 65mg/ after 2h
L；Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 590Kg 93% are added dropwise, and adjusts pH to 6-7.From the sour kettle outflow of drop
Waste water concentrated into mechanical steam recompression evaporator, concentration removal 50%-60%.It is concentrated by evaporation Mother liquor transfer
To cooling reactor, 93% concentrated sulfuric acid is dripped toward cooling reactor, control pH to 4 or so, it is brilliant then toward dispensing crystal seed NH4Cl in cooling reactor
Plant and require NH4Cl contents more than 99.9%, Seed charge is 0.4% (about 14Kg) of ammonium salt output.After through centrifuge,
Ammonium salt output 3.4t, centrifuge mother liquor 270Kg are burned into incinerator.
Embodiment 3：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 600Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and anti-solvent ethanol is added toward cooling reactor, and anti-solvent adding rate is 15kgmin-1
(10m3 kettles), adds anti-solvent ethanol 0.8t (about the 1/4 of feed liquid) altogether.After centrifuge, ammonium salt output 3.5t, centrifugation is female
Liquid steams residue 200Kg after ethanol, is directly entered incinerator burning.
Embodiment 4：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 590Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and 93% concentrated sulfuric acid is dripped toward cooling reactor, controls pH to 4 or so, after centrifuge, ammonium
Salt yield 3.2t, centrifuge mother liquor 480Kg are burned into incinerator.
Embodiment 5：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 590Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and crystal seed NH4Cl is delivered toward cooling reactor, and crystal seed requirement NH4Cl contents are more than 99.9%, crystalline substance
It is 0.4% (about 13Kg) of ammonium salt output to plant addition.After centrifuge, ammonium salt output 3.3t, centrifuge mother liquor 390Kg enters
Enter incinerator burning.
Embodiment 6：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 590Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and 93% concentrated sulfuric acid is dripped toward cooling reactor, controls pH to 4 or so, then toward throwing in cooling reactor
Crystal seed NH4Cl is put, crystal seed requirement NH4Cl contents are more than 99.9%, and Seed charge is 0.3% (about 10Kg) of ammonium salt output.
After centrifuge, ammonium salt output 3.35t, centrifuge mother liquor 340Kg are burned into incinerator.
Embodiment 7：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 590Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and 93% concentrated sulfuric acid is dripped toward cooling reactor, controls pH to 4 or so, then toward throwing in cooling reactor
Put crystal seed NH4Cl, crystal seed requirement NH4Cl contents are more than 99.9%, Seed charge for ammonium salt output 0.5% (about
16.5Kg).After centrifuge, ammonium salt output 3.33t, centrifuge mother liquor 370Kg are burned into incinerator.
Embodiment 8：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 600Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and anti-solvent ethanol is added toward cooling reactor.Anti-solvent adding rate is 10kgmin-1
(10m3 kettles), adds anti-solvent ethanol 0.8t (about the 1/4 of feed liquid) altogether.After centrifuge, ammonium salt output 3.46t, centrifugation
Mother liquor steams residue 290Kg after ethanol, is directly entered incinerator burning.
Embodiment 9：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 600Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and anti-solvent ethanol is added toward cooling reactor.Anti-solvent adding rate is 20kgmin-1
(10m3 kettles), adds anti-solvent ethanol 0.8t (about the 1/4 of feed liquid) altogether.After centrifuge, ammonium salt output 3.45t, centrifugation
Mother liquor steams residue 300Kg after ethanol, is directly entered incinerator burning.
Embodiment 10：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 600Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and anti-solvent ethanol is added toward cooling reactor.Anti-solvent adding rate is 15kgmin-1
(10m3 kettles), adds anti-solvent ethanol about 0.6t (the 1/5 of feed liquid) altogether.After centrifuge, ammonium salt output 3.35t, centrifugation
Mother liquor steams residue 360Kg after ethanol, is directly entered incinerator burning.
Embodiment 11：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 600Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and anti-solvent ethanol is added toward cooling reactor.Anti-solvent adding rate is 15kgmin-1
(10m3 kettles), adds anti-solvent ethanol about 1.0t (the 1/3 of feed liquid) altogether.After centrifuge, ammonium salt output 3.48t, centrifugation
Mother liquor steams residue 260Kg after ethanol, is directly entered incinerator burning.
Embodiment 12：
The once washing water 9t of paraquat synthesis press filtration workshop section washing, the mass fraction 22% of ammonia in washings, through stripping
Tower reclaims ammonia, and the mass fraction of the ammonia that discharges is reduced to 4%, and stripper reclaims the waste water cyanogen root concentration 18.3g/L after ammonia, is heated to
90 DEG C, into broken cyanide tower, the formaldehyde of 464Kg 37% is added in broken cyanide tower, 30% soda bath 1.6t is added after 0.5h, after 2h
Cyanogen root content 65mg/L.Waste water after broken cyanide flows into the sour kettle regulation pH of drop, and the concentrated sulfuric acids of 600Kg 93% are added dropwise, and adjusts pH to 6-7.
Concentrated into mechanical steam recompression evaporator from the waste water of the sour kettle outflow of drop, concentration amount reaches 50%-60%.Evaporation
Concentration Mother liquor is transferred to cooling reactor, and anti-solvent methyl alcohol is added toward cooling reactor.Anti-solvent adding rate is 15kgmin-1
(10m3 kettles), adds anti-solvent ethanol about 0.8t (the 1/4 of feed liquid) altogether.After centrifuge, ammonium salt output 3.3t, centrifugation is female
Liquid steams residue 410Kg after ethanol, is directly entered incinerator burning.
To sum up, embodiment of the present invention 2-12 compared with Example 1, increases to rush analysis reagent operation is added in cooling reactor, can
Obtaining ammonium salt output to find out, embodiment 2-12 will substantially reduce more apparently higher than embodiment 1, and centrifuge mother liquor amount, so as to reduce
Cost is burned, environmental pollution is reduced.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation make a distinction with another entity or operation, and not necessarily require or imply these entities or deposited between operating
In any this actual relation or order.And, term " including ", "comprising" or its any other variant be intended to
Nonexcludability is included, so that process, method, article or equipment including a series of key elements not only will including those
Element, but also other key elements including being not expressly set out, or also include being this process, method, article or equipment
Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that
Also there is other identical element in process, method, article or equipment including the key element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention has been described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic；And these modification or
Replace, do not make the spirit and scope of the essence disengaging various embodiments of the present invention technical scheme of appropriate technical solution.
Claims (10)
1. in a kind of paraquat waste water ammonium salt crystallization treatment technique, it is characterised in that comprise the following steps：
1) washes of paraquat synthesis press filtration workshop section is reclaimed into ammonia through stripper；
2) waste water reclaimed after ammonia is passed into broken cyanide tower carries out broken cyanide treatment；
3) waste water after broken cyanide is transferred in the sour kettle of drop and adjusts pH；
4) waste water adjusted after pH is passed through and concentration is evaporated in mechanical steam recompression evaporator；
5) waste water after evaporation and concentration is transferred to cooling reactor, be added thereto to promote analysis reagent promote ammonium salt precipitation, reduce from
Heart mother liquor amount；The analysis reagent that promotees is selected from NH4Any one in Cl crystal seeds, the concentrated sulfuric acid, anti-solvent, or the concentrated sulfuric acid and NH4Cl is brilliant
Kind.
2. in paraquat waste water as claimed in claim 1 ammonium salt crystallization treatment technique, it is characterised in that the step 1) wash
It is 22% to wash the mass fraction of ammonia in waste water, and after reclaiming ammonia through stripper, the mass fraction of ammonia is 4%, cyanogen root concentration in discharging
It is 18.3g/L.
3. the crystallization treatment technique of ammonium salt in paraquat waste water as claimed in claim 1, it is characterised in that the step 2)
Broken cyanide treatment is that waste water is passed through into broken cyanide tower, and to 37% formaldehyde is added in tower, 30% soda bath is added after 0.5h, after 2h
Discharging, cyanogen root content is 65mg/L.
4. the crystallization treatment technique of ammonium salt in paraquat waste water as claimed in claim 1, it is characterised in that the step 3)
PH to 6-7 is adjusted using 93% concentrated sulfuric acid in the sour kettle of drop.
5. ammonium salt crystallization handling process in paraquat waste water as claimed in claim 1, it is characterised in that the step 4) in
Evaporation and concentration removes 50%-60%.
6. the crystallization treatment technique of ammonium salt in paraquat waste water as claimed in claim 1, it is characterised in that the step 5)
Promote ammonium salt precipitation to use and 93% concentrated sulfuric acid regulation pH to 4-5 is dripped toward cooling reactor.
7. the crystallization treatment technique of ammonium salt in paraquat waste water as claimed in claim 1, it is characterised in that the step 5)
Ammonium salt is promoted to separate out using toward dripping 93% concentrated sulfuric acid regulation pH to 4-5 in cooling reactor, then toward dispensing crystal seed NH in cooling reactor4Cl,
Seed charge is the 0.3%-0.5% of ammonium salt output.
8. the crystallization treatment technique of ammonium salt in paraquat waste water as claimed in claim 1, it is characterised in that the step 5)
Promote ammonium salt to separate out and use the dispensing crystal seed NH toward cooling reactor4Cl, Seed charge is the 0.3%-0.5% of ammonium salt output.
9. the crystallization treatment technique of ammonium salt in paraquat waste water as claimed in claim 1, it is characterised in that the step 5)
Promote ammonium salt precipitation to use and anti-solvent is added toward cooling reactor, anti-solvent adding rate is 10-20kgmin-1, anti-solvent addition
Measure the 1/5-1/3 for feed liquid.
10. the crystallization treatment technique of ammonium salt in paraquat waste water as claimed in claim 9, it is characterised in that described anti-molten
Agent is methyl alcohol or ethanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710004706.9A CN106698791A (en) | 2017-01-04 | 2017-01-04 | Crystallization treatment process for ammonium salt in paraquat wastewater |
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| CN201710004706.9A CN106698791A (en) | 2017-01-04 | 2017-01-04 | Crystallization treatment process for ammonium salt in paraquat wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107500463A (en) * | 2017-09-26 | 2017-12-22 | 安徽国星生物化学有限公司 | A kind of paraquat wastewater treatment and resource utilization process |
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| CN104117280A (en) * | 2014-07-24 | 2014-10-29 | 湖南康盟环保科技有限公司 | Ammonia stripping tail gas treatment method, ammonia-nitrogen wastewater treatment method and equipment |
| CN104230081A (en) * | 2014-07-16 | 2014-12-24 | 湖北仙隆化工股份有限公司 | Paraquat pesticide wastewater treatment process |
| 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 |
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| CN104030508A (en) * | 2014-04-29 | 2014-09-10 | 安徽国星生物化学有限公司 | Cyanide breaking method of cyanogen-containing wastewater |
| CN104230081A (en) * | 2014-07-16 | 2014-12-24 | 湖北仙隆化工股份有限公司 | Paraquat pesticide wastewater treatment process |
| CN104117280A (en) * | 2014-07-24 | 2014-10-29 | 湖南康盟环保科技有限公司 | Ammonia stripping tail gas treatment method, ammonia-nitrogen wastewater treatment method and equipment |
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| CN107500463A (en) * | 2017-09-26 | 2017-12-22 | 安徽国星生物化学有限公司 | A kind of paraquat wastewater treatment and resource utilization process |
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