CN109020030A - A kind of waste water treatment process in paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process - Google Patents
A kind of waste water treatment process in paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process Download PDFInfo
- Publication number
- CN109020030A CN109020030A CN201810978992.3A CN201810978992A CN109020030A CN 109020030 A CN109020030 A CN 109020030A CN 201810978992 A CN201810978992 A CN 201810978992A CN 109020030 A CN109020030 A CN 109020030A
- Authority
- CN
- China
- Prior art keywords
- waste water
- water
- paranitroanilinum
- kettle
- nitraniline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
-
- 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
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The present invention provides a kind of paranitroanilinum, waste water treatment process in ortho-nitraniline and corresponding phenyl amines chemical production process, including material recycle workshop section, waste water acidification of acidification section, formaldehyde condensation workshop section, light electrolysis workshop section, oxidation section, in night and workshop section, ammonium chloride stoste workshop section, it is mainly characterized by, it is processed by workshop section's step, before wastewater treatment and material air that material recycle workshop section first mixes the water of the fully reacting in ammonolysis kettle admittedly is due to paranitroanilinum, ortho-nitraniline and other phenyl amines are all dissolved in hot water, it to react and could complete under the high temperature by 170 DEG C -180 DEG C in paranitroanilinum and ortho-nitraniline, the filter press for waste water pump being such as equipped with anti-corrosion centrifugal pump the mesh Lyu's cloth of 800 mesh -1500 carries out material in waste water and extracts, extraction material waste water pump is squeezed into 2# waste water Pond.It is filtered the invention has the advantages that product waste water passes through the filter press equipped with the mesh filter cloth of 800 mesh -1500, so that it is known as granular crystals, reach the requirement of commerical grade.
Description
Technical field
The present invention relates to the waste water in a kind of paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process
Treatment process.
Background technique
Paranitroanilinum is a kind of indispensable primary raw material of the intermediate of special production dyestuff, its waste water country
Discharge standard, COD one kind discharge standard are 100mg/L, and two class discharge standards are 300mg/L；BOD one kind discharge standard 100mg/
L, two class discharge standard 200mg/L；Ammonia nitrogen amount one kind discharge standard 15mg/L, two class discharge standard 50mg/L；Nitrobenzene one
Class discharge standard is that bis- class discharge standard of 2mg/L is 3mg/L.
Due to the operational characteristic of the two products, determine that COD and ammonia nitrogen amount are extra-high in waste water, COD is in 10000 mg/
14000 mg/L of L-or so, ammonia nitrogen amount is in 28000mg/L -30000mg/L.The waste water biochemical treatment of such high concentration, the
One, it is necessary to waste water be gone to dilute with a large amount of clear water, the waste water COD after diluting it is in 500 mg/L to 800 mg/L or so
It can enter biochemistry pool to be handled.And every cubic metre can only handle 50-70 kg of water or so, an enterprise for biochemistry pool 24 hours one day
Industry is just reached 50 tons or so, 25 must be used before biochemical treatment by the scale for producing 10 tons of products daily, waste water in production
Water again goes to dilute, and can be only achieved the standard into biochemistry pool, and otherwise the biological bacteria in biochemistry pool will be dead, that is to say, that one
Family produces the producer of daily 10 tons of paranitroanilinum and ortho-nitraniline, into handled in biochemistry pool water to reach 50X25=
1250 cubic metres, biochemical pool area is needed to reach the biochemistry pool of 1785m3 or so, by 4 meters of biochemistry pool deep calculating, needs one
The biochemistry pool of 65X70 meters of super large land occupation areas.And go the production of 10 tons of products of processing useless with so large-scale engineering
Water, although COD, BOD are up to standard, ammonia nitrogen amount is still far beyond national emission standard, because biochemical treatment can only have been handled
Machine object, cannot handle ammonia nitrogen, and biological bacteria does not handle the function of ammonia nitrogen.
National ammonia nitrogen discharge standard is 15-50mg/L, and the ammonia nitrogen of the waste water of paranitroanilinum, ortho-nitraniline exists
28000mg/L -30000mg/L or so, and it goes to dilute with 25 times of water now, its treated ammonia nitrogen in waste water amount is at least also
In 1165mg/L or so, far beyond national emission request.Thus at the waste water biochemistry of paranitroanilinum, ortho-nitraniline
Reason be it is unpractical, first, water processing establishment engineering is too big, various water purification agents and other raw material are added in treatment process, at
Ben Taigao, the waste water for almost handling product per ton will reach 3000-4000 yuan or more, and can only locally reach standard, at all
Do not accomplish completely up to standard.
There are also nitrobenzenes after biochemical treatment, its COD can generally reach 200mg/L -300mg/L or so, and this
In the COD of 200mg/L -300mg/L, most of is all paranitrochlorobenzene and o-nitrochlorobenzene, by national standard, nitrobenzene
Discharge must not exceed 2mg/L -3mg/L, and treated in this approach that waste water nitrobenzene greatly exceeds country's discharge mark for institute
Standard also goes to dilute if really wanting up to standard with 100 times or so of water, that is to say, that in the case where being diluted to 25 times
Dilution ability qualified discharge is removed with 100 times of water again, gets off to produce the enterprise of 10 tons of yield so daily, it is necessary to use
The water of 50X25X100=125000 cubic metre goes to dilute, and can be only achieved national emission standard, in our water shortage big countries, at all
It can not do so.While energy-saving and emission-reduction are not both played, more waste of resource.
In addition the producer having invests a set of polyester absorption wastewater treatment equipment of 25-30 ten thousand custom-mades, polyester adsorbent equipment
The waste water exceeded used in low suspended particulate or low pollution can be used, the high concentration such as being used in paranitroanilinum and ortho-nitraniline
The waste water of pollution is worthless.Such as:
1, the polyester device for customizing a 5000L needs 25-30 ten thousand yuan of expense, and handles waste water daily at 10 tons or so, and
This polyester at most must just remove cleaning polyester grain using one day, cleaning is needed every time when adsorbing high-concentration waste water with methanol
With 1 ton or so of methanol.This method processing waste water cost as one can imagine.
2, due to the characteristic of polyester, the waste water of absorption high concentration is removed with it, although going to clean with methanol daily, it makes
With the time limit, also most the too many by two moon must just replace polyester grain by three months.And every replacement must once need nearly 160,000 or so
Expense, if this expense plus methanol expense calculate to about 5000 yuan or so on product per ton, due to the benefit of the two products
Moisten a disk and holds the wastewater treatment expense for daring not accept so high at all at 1000-2000 yuan or so.
Waste water after polyester adsorbs, the ammonia nitrogen amount although COD, BOD are attained by national emission standard, in waste water
It is adsorbed with originally having no idea, so ammonia nitrogen amount is also in 28000mg/L -30000mg/L or so in treated waste water, not
National emission standard can be reached.
Summary of the invention
The purpose of the present invention is deficiency present in view of the above technology, a kind of paranitroanilinum, ortho-nitraniline are provided
With the waste water treatment process in corresponding phenyl amines chemical production process.
Not only can continuous processing, treating capacity is big, processing thoroughly, processing cost is low, and chemical company's waste water is fully achieved
Zero emission requirement.
The object of the present invention is achieved like this, including before wastewater treatment and material recycle workshop section, waste water acidification of acidification section, first
Aldehyde be condensed workshop section, light electrolysis workshop section, oxidation section, in night and workshop section, ammonium chloride stoste workshop section, characterized in that press following step
Rapid operation, before wastewater treatment and material air pressure that material recycle workshop section first mixes the water of the fully reacting in ammonolysis kettle admittedly
Contracting machine is depressed into washing kettle or crystallization kettle is made to be separated by solid-liquid separation, and the ammonia level liquid containing 11% -8% is separated to ammonia still process tank,
It carries out ammonia and extracts reuse, the 80% of solid aggregation material is washed with clear water, is put into separating tank after washing, is dried and contained
The material of water 9% is packed, storage, since paranitroanilinum, ortho-nitraniline and other phenyl amines are all dissolved in hot water, in
Paranitroanilinum and ortho-nitraniline will be by reacting and could complete under 170 DEG C -180 DEG C of high temperature, so waste water includes one
Quantitative paranitroanilinum and ortho-nitraniline, the COD after ammonia is extracted in mg/L of 10000 mg/L -14000 or so, and
Washes is discharged into 1# wastewater disposal basin together, waste water pump is such as equipped with anti-corrosion centrifugal pump the filter press of the mesh Lyu's cloth of 800 mesh -1500
The material carried out in waste water extracts, and extraction material waste water pump is squeezed into 2# wastewater disposal basin.
Waste water acidification of acidification section: being added dropwise with sulfuric acid into waste water, is opened air stirring, so that waste water pH value is reached 2 ~ 3, give up at this time
Water and sulfuric acid generate exothermic reaction, allow waste water natural cooling 12 hours.
Formaldehyde condensation workshop section: being pumped into the waste water after being acidified in 2# wastewater disposal basin with corrosion protection pump the enamel still of 5000L, and unlatching is stirred
It mixes, 2% formaldehyde that waste water total amount is added carries out condensation stirring, opens enamel still chuck cooling water and carries out cooling processing, after processing
Condensation pond is drained into, air stirring is opened, waste water at this time has a certain amount of organic matter to be precipitated, and the waste water after condensation is with being equipped with
The filter press of the filter cloth of 200 mesh is separated by solid-liquid separation, and the clear liquid isolated is discharged into 3# waste water and clear liquid pond, and the COD of waste water is at this time
2950mg/L or so.
Light electrolysis workshop section: being pumped into the waste water in 3# waste water and clear liquid pond with corrosion protection pump the ceramic stirred tank of 1500L, is added per ton
The iron powder that 2.5 kilograms of water carries out micro-electrolysis reaction, and the waste water that the pH value after reacting is 5 or so is slowly flowed with a certain amount of sulfuric acid
Enter to be electrolysed kettle and carries out electrolysis processing.
Oxidation section: when entering electrolysis kettle from the waste water of light electrolysis, with the flow of waste water/20 kilogram 1t hydrogen peroxide per hour
It is added dropwise, opening point solution device, keeps organic matter in waste water and micro iron ion fully oxidized, the waste water after peroxidating is from electrolysis
The diversion trench of kettle is flowed into the continuation of 4# waste water and is aoxidized 4-6 hours.
In night and workshop section: the waste water pH value after oxidation in 4-6 hours, generally 3 or so, be added at this time liquid alkaline into
Row neutralizes, and a large amount of bubble is had in N-process and is occurred, defoaming agent is added, foam is eliminated, the waste water tune in neutralization pond
It is 7 to pH value, the waste water after neutralization is squeezed into the filter press equipped with 200 mesh filter clothes with pump and is filtered, is obtained after filtering colourless
Ammonium chloride stoste.
Ammonium chloride stoste workshop section: the water after neutralization is colourless, PH7, and the water of neutralization pond is pumped into evaporator, is steamed by being added
Hair, pure white ammonium chloride flow into ammonium chloride crystals pond, spill solid carbon dioxide point with centrifuge, obtain the ammonium chloride agricultural fertilizer of content 93%,
In distillation process, steam passes through the condenser of 20m3 or 40m3, condenses steam sufficiently and becomes condensed water, the COD of condensed water is
Condensed water is discharged into condensation water collection pond by the mg/L of 100 mg/L -160, and condensate pump such as kitchen sink is washed material with pump.
A small amount of organic matter after filters pressing, is ratified by environmental protection administration, is transported at qualified chemical industry waste solids processing unit
Reason is burned.
It is filtered the invention has the advantages that product waste water passes through the filter press equipped with the mesh filter cloth of 800 mesh -1500, makes it
Referred to as granular crystals reach the requirement of commerical grade.
The paranitroanilinum recycling 60% -70% being dissolved in waste water, the paranitroanilinum of recycling is put into ammonolysis kettle, weight
New reaction reduction, the COD of waste water drop to 7000mg/L or so from 14000mg/L, cost for wastewater treatment below are greatly saved.
After the filtered waste water acidification of filter press, so that it is dissolved in the material in waste water and be further precipitated, be then acidified
PH value afterwards is 3-4, and the waste water after this acidification makes it more preferably decolourize in next step.
2% oxymethylene polymerization is added in waste water after acidification, and making it, there are also the micro materials being dissolved in waste water to be all precipitated, and leads to
The filter press filtering equipped with 300 mesh is crossed, filtered waste water enters in light electrolysis slot, it is press-filtered out the material recycle come, this
When waste water COD be down to 2950 mg/L or so from 7000 mg/L.
Specific embodiment
Below with reference to embodiment, the present invention will be further described
The present invention is implemented as follows, and 1, before wastewater treatment and material recycle workshop section, 2, waste water acidification of acidification section, 3 formaldehyde condensations
Workshop section, 4 light electrolysis workshop sections, 5 oxidation sections, in 6 nights and workshop section, 7 ammonium chloride stoste workshop sections, concrete technology is wastewater treatment
Preceding and material recycle workshop section, before wastewater treatment and object that material recycle workshop section first mixes the water of the fully reacting in ammonolysis kettle admittedly
Material is depressed into washing kettle with air compressor or crystallization kettle is made to be separated by solid-liquid separation, the ammonia level liquid containing 11% -8% point
From to ammonia still process tank, carries out ammonia and extract reuse, the 80% of solid aggregation material is washed with clear water, separating tank is put into after washing, is carried out
The material for being dried to obtain water content 9% is packed, storage, since paranitroanilinum, ortho-nitraniline and other phenyl amines are all molten
In hot water, to react and could complete under the high temperature by 170 DEG C -180 DEG C in paranitroanilinum and ortho-nitraniline, so
Waste water includes a certain amount of paranitroanilinum and ortho-nitraniline, and the COD after ammonia is extracted is in 10000 mg/L -14000
Mg/L or so and washes are discharged into 1# wastewater disposal basin together, waste water pump are such as equipped with anti-corrosion centrifugal pump mesh Lyu of 800 mesh -1500
The filter press of cloth carries out the material in waste water and extracts, and extraction material waste water pump is squeezed into 2# wastewater disposal basin.
Waste water acidification of acidification section: being added dropwise with sulfuric acid into waste water, is opened air stirring, so that waste water pH value is reached 2 ~ 3, give up at this time
Water and sulfuric acid generate exothermic reaction, allow waste water natural cooling 12 hours.
Formaldehyde condensation workshop section: being pumped into the waste water after being acidified in 2# wastewater disposal basin with corrosion protection pump the enamel still of 5000L, and unlatching is stirred
It mixes, 2% formaldehyde that waste water total amount is added carries out condensation stirring, opens enamel still chuck cooling water and carries out cooling processing, after processing
Condensation pond is drained into, air stirring is opened, waste water at this time has a certain amount of organic matter to be precipitated, and the waste water after condensation is with being equipped with
The filter press of the filter cloth of 200 mesh is separated by solid-liquid separation, and the clear liquid isolated is discharged into 3# waste water and clear liquid pond, and the COD of waste water is at this time
2950 mg/L or so.
Light electrolysis workshop section: being pumped into the waste water in 3# waste water and clear liquid pond with corrosion protection pump the ceramic stirred tank of 1500L, is added per ton
The iron powder that 2.5 kilograms of water carries out micro-electrolysis reaction, and the waste water that the pH value after reacting is 5 or so is slowly flowed with a certain amount of sulfuric acid
Enter to be electrolysed kettle and carries out electrolysis processing.
Oxidation section: when entering electrolysis kettle from the waste water of light electrolysis, with the flow of waste water/20 kilogram 1t hydrogen peroxide per hour
It is added dropwise, opening point solution device, keeps organic matter in waste water and micro iron ion fully oxidized, the waste water after peroxidating is from electrolysis
The diversion trench of kettle is flowed into the continuation of 4# waste water and is aoxidized 4-6 hours.
In night and workshop section: the waste water pH value after oxidation in 4-6 hours, generally 3 or so, be added at this time liquid alkaline into
Row neutralizes, and a large amount of bubble is had in N-process and is occurred, defoaming agent is added, foam is eliminated, the waste water tune in neutralization pond
It is 7 to pH value, the waste water after neutralization is squeezed into the filter press equipped with 200 mesh filter clothes with pump and is filtered, is obtained after filtering colourless
Ammonium chloride stoste.
Ammonium chloride stoste workshop section: the water after neutralization is colourless, PH7, and the water of neutralization pond is pumped into evaporator, is steamed by being added
Hair, pure white ammonium chloride flow into ammonium chloride crystals pond, spill solid carbon dioxide point with centrifuge, obtain the ammonium chloride agricultural fertilizer of content 93%,
In distillation process, steam passes through the condenser of 20m3 or 40m3, condenses steam sufficiently and becomes condensed water, the COD of condensed water is
Condensed water is discharged into condensation water collection pond by mg/L of 100 mg/L -160 or so, and condensate pump such as kitchen sink is washed material with pump.
A small amount of organic matter after filters pressing, is ratified by environmental protection administration, is transported at qualified chemical industry waste solids processing unit
Reason is burned.
Product waste water passes through the filter press equipped with the mesh filter cloth of 800 mesh -1500 and filters, the p-nitrophenyl being dissolved in waste water
Amine recycling 60% -70%, in the paranitroanilinum of recycling investment ammonolysis kettle, reaction reduction again, the COD of waste water is from 14000 mg/
L drops to 7000 mg/L or so, and cost for wastewater treatment below is greatly saved.
After the filtered waste water acidification of filter press, so that it is dissolved in the material in waste water and be further precipitated, be then acidified
PH value afterwards is 3-4, and the waste water after this acidification makes it more preferably decolourize in next step.
2% oxymethylene polymerization is added in waste water after acidification, and making it, there are also the micro materials being dissolved in waste water to be all precipitated, and leads to
The filter press filtering equipped with 300 mesh is crossed, filtered waste water enters in light electrolysis slot, it is press-filtered out the material recycle come, this
When waste water COD from 7000 mg/L to be down to 2950 left mg/L right.
After waste water enters light electrolysis, 10 kilograms of waste water of iron powder per ton is added and is stirred, stirs or so 1 hour, so
The pump opened in acidification pool afterwards is continuously intake from bottom with 2 tons or so per hour into light electrolysis kettle, and upper water is from top water conservancy diversion
Slot enters electrolysis kettle and carries out solution and an oxidation processes, and the waste water come out in light electrolysis is in black and white, and pH value is 4-5 or so.
The waste water that light electrolysis diversion trench comes out flows into electrolysis kettle, kettle top price hydrogen peroxide drip tank is electrolysed, with per hour
20 kilograms or so of flow, continuous that hydrogen peroxide is added dropwise into electrolysis kettle, the electric current being electrolysed in kettle is adjusted to 135A, and voltage is adjusted to 4-
7V or so continuous use, the waste water after the oxidation of passing point solution flow into alkalization neutralization pond from electrolysis kettle top diversion trench.
Alkalization neutralization pond is flowed into from solution oxidation pond, liquid alkaline is added, waste water pH value is adjusted to 7, make its neutrality, added and subtracted
Since a large amount of foams can occur in journey, so to enter a certain amount of defoaming agent eliminates foam, aoxidized, fill in pond by 12 hours
Divide the iron ion and micro organic matter brought out in exhaustive oxidation light electrolysis.
Waste water after fully oxidized is added 10 grams of water of polymerizer per ton and sufficiently polymerize by it, the waste water pump after polymerization
Enter the filter press equipped with 200 mesh filter clothes to filter, obtains colourless, neutral, ammonium chloride stock solution water of the pH value 7, filter press filters out
The micro waste solids come, ratify through Environmental Protection Agency, send to the treating stations processing for having chemical industry waste solids processing qualification.
Ammonium chloride clear liquid is pumped into the evaporator evaporation of 120m3 with 2 tons per hour of flow, and ammonium chloride is from Shang Zhongkou flow-guiding mouth
Ammonium chloride crystals slot is flowed into, the ammonium chloride after crystallization is dehydrated with centrifuge, and dewatered ammonium chloride pure white, nitrogen content is 17
The agricultural fertilizer of 19 mg/L of mg/L-.
The gas that evaporator comes out makes it sufficiently be known as liquid water by the condenser of 20m3, and liquid water flows into condensed water
Recovery pond recycling, COD100 mg/L -160mg/L of condensed water.The condensed water in condensing hot air furnace pond is pumped into pump and washes truck
Between wash material, reach enterprise's cycling utilization of wastewater in process of production, reach production zero-emission effect.
Claims (5)
1. the waste water treatment process in a kind of paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process, packet
Include following workshop section: it is characterized in that, before wastewater treatment and material recycle workshop section: first mixing the water of the fully reacting in ammonolysis kettle admittedly
Material be depressed into washing kettle with air compressor or crystallization kettle made to be separated by solid-liquid separation, contain 11% -8% ammonia level liquid
Body is separated to ammonia still process tank, is carried out ammonia and is extracted reuse, and the 80% of solid aggregation material is washed with clear water, is put into separating tank after washing,
The material for being dried to obtain water content 9% is packed, storage, due to paranitroanilinum, ortho-nitraniline and other phenyl amines
It is all dissolved in hot water, to react and could complete under the high temperature by 170 DEG C -180 DEG C in paranitroanilinum and ortho-nitraniline,
So waste water includes a certain amount of paranitroanilinum and ortho-nitraniline, the COD after ammonia is extracted is in 10000 mg/L-
14000 mg/L or so and washes are discharged into 1# wastewater disposal basin together, waste water pump are such as equipped with 800 mesh-with anti-corrosion centrifugal pump
The filter press of 1500 mesh Lyu's cloth carries out the material in waste water and extracts, and extraction material waste water pump is squeezed into 2# wastewater disposal basin；
Waste water acidification of acidification section: being added dropwise with sulfuric acid into waste water, open air stirring, so that waste water pH value is reached 2 ~ 3, at this time waste water and
Sulfuric acid generates exothermic reaction, allows waste water natural cooling 12 hours；
Formaldehyde condensation workshop section: being pumped into the waste water after being acidified in 2# wastewater disposal basin with corrosion protection pump the enamel still of 5000L, open stirring,
2% formaldehyde that waste water total amount is added carries out condensation stirring, opens enamel still chuck cooling water and carries out cooling processing, handles heel row
It is put into condensation pond, opens air stirring, waste water at this time has a certain amount of organic matter to be precipitated, and the waste water after condensation, which is used, is equipped with 200
The filter press of purpose filter cloth is separated by solid-liquid separation, and the clear liquid isolated is discharged into 3# waste water and clear liquid pond, and the COD of waste water is 2950 at this time
Mg/L or so；
Light electrolysis workshop section: the waste water in 3# waste water and clear liquid pond is pumped into corrosion protection pump the ceramic stirred tank of 1500L, water per ton is added
2.5 kilograms of iron powder carries out micro-electrolysis reaction, and the waste water that the pH value after reacting is 5 or so is flowed slowly into a certain amount of sulfuric acid
Electrolysis kettle carries out electrolysis processing；
Oxidation section: it when entering electrolysis kettle from the waste water of light electrolysis, is dripped with the flow of waste water/20 kilogram 1t hydrogen peroxide per hour
Add, opening point solution device, keep organic matter in waste water and micro iron ion fully oxidized, the waste water after peroxidating is from electrolysis kettle
Diversion trench flow into 4# waste water continue in aoxidize 4-6 hours；
In night and workshop section: liquid alkaline is added at this time and is neutralized generally in 3-4 for the waste water pH value after oxidation in 4-6 hours,
A large amount of bubble is had in N-process to occur, defoaming agent is added, and eliminates foam, the waste water in neutralization pond, which is adjusted to pH value, is
7, the waste water after neutralization is squeezed into the filter press equipped with 200 mesh filter clothes with pump and is filtered, colourless ammonium chloride is obtained after filtering
Stoste；
Ammonium chloride stoste workshop section: the water after neutralization is colourless, pH value 7, and the water of neutralization pond is pumped into evaporator, is steamed by being added
Hair, pure white ammonium chloride flow into ammonium chloride crystals pond, spill solid carbon dioxide point with centrifuge, obtain the ammonium chloride agricultural fertilizer of content 93%,
In distillation process, steam passes through the condenser of 20m3 or 40m3, condenses steam sufficiently and becomes condensed water, the COD of condensed water is
Condensed water is discharged into condensation water collection pond by mg/L of 100 mg/L -160 or so, and condensate pump such as kitchen sink is washed material with pump.
2. a kind of paranitroanilinum according to claim 1, ortho-nitraniline and corresponding phenyl amines chemical production process
In waste water treatment process, characterized in that product waste water pass through equipped with the mesh filter cloth of 800 mesh -1500 filter press filter, molten
Paranitroanilinum recycling 60% -70% in waste water, the paranitroanilinum of recycling are put into ammonolysis kettle, and reaction reduction, makes again
It is known as granular crystals, reaches the requirement of commerical grade.
3. a kind of paranitroanilinum according to claim 1, ortho-nitraniline and corresponding phenyl amines chemical production process
In waste water treatment process, characterized in that waste water by equipped with the mesh of 800 mesh -1500 Lyu's cloth filter press filtering after, waste water
COD drops to 7000-8000 mg/L from 14000 mg/L, cost for wastewater treatment below is greatly saved, after filter press filters
Waste water acidification after, so that it is dissolved in the material in waste water and be further precipitated, then be acidified after pH value be 3-4, after this acidification
Waste water so that it is more preferably decolourized in next step, 2% oxymethylene polymerization is added in waste water after acidification, it is made to be dissolved in waste water there are also micro
In material all be precipitated.
4. a kind of paranitroanilinum according to claim 1, ortho-nitraniline and corresponding phenyl amines chemical production process
In waste water treatment process, characterized in that filtered by the filter press equipped with 300 mesh, filtered waste water enters light electrolysis slot
In, it is press-filtered out the material recycle come, waste water COD at this time is down to 2950 mg/L from 7000 mg/L, and waste water enters micro- electricity
Xie Hou is added 10 kilograms of waste water of iron powder per ton and is stirred, stirs or so 1 hour, and the pump being then turned in acidification pool connects
Continuous to intake from bottom with 2 tons or so per hour into light electrolysis kettle, upper water enters electrolysis kettle from top diversion trench and carries out a solution
And oxidation processes, the waste water come out in light electrolysis are in black and white, pH value is 4-5, and the waste water that light electrolysis diversion trench comes out flows into electricity
Kettle is solved, kettle top price hydrogen peroxide drip tank is electrolysed, it is continuous that dioxygen is added dropwise into electrolysis kettle with 20 kilograms per hour of flow
Water, the electric current being electrolysed in kettle are adjusted to 135A, and voltage is adjusted to 4-7V continuous use, and the waste water after the oxidation of passing point solution is from electrolysis kettle
Top diversion trench flows into alkalization neutralization pond, flows into alkalization neutralization pond from solution oxidation pond and liquid alkaline is added, waste water pH value tune
To 7, makes its neutrality, use defoaming agent to eliminate foam during plus-minus, aoxidized in pond by 12 hours, abundant exhaustive oxidation
10 grams of water of polymerization per ton is added in the iron ion and micro organic matter brought out in light electrolysis, the waste water after fully oxidized
Agent allows it sufficiently to polymerize, and the waste water after polymerization is pumped into the filtering of the filter press equipped with 200 mesh filter clothes, obtains colourless, neutral, pH value exists
7 ammonium chloride stock solution water, the micro waste solids that filter press filters out, ratifies through Environmental Protection Agency, send to have chemical industry waste solids processing
The treating stations of qualification are handled.
5. a kind of paranitroanilinum according to claim 1, ortho-nitraniline and corresponding phenyl amines chemical production process
In waste water treatment process, characterized in that ammonium chloride clear liquid with 2 tons per hour of flow be pumped into 120m3 evaporator evaporate, chlorine
Change ammonium and flow into ammonium chloride crystals slot from Shang Zhongkou flow-guiding mouth, the ammonium chloride after crystallization is dehydrated with centrifuge, dewatered ammonium chloride
Pure white, agricultural fertilizer of the nitrogen content in the mg/L of 17 mg/L -19；
The gas that evaporator comes out makes it sufficiently be known as liquid water by the condenser of 20m3, and liquid water flows into condensing hot air furnace
Pond recycling, COD100 mg/L -160mg/L of condensed water are pumped into the condensed water in condensing hot air furnace pond with pump between washing truck and wash
Material, reaches enterprise's cycling utilization of wastewater in process of production, reaches production zero-emission effect.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810978992.3A CN109020030A (en) | 2018-08-27 | 2018-08-27 | A kind of waste water treatment process in paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810978992.3A CN109020030A (en) | 2018-08-27 | 2018-08-27 | A kind of waste water treatment process in paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109020030A true CN109020030A (en) | 2018-12-18 |
Family
ID=64624600
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810978992.3A Pending CN109020030A (en) | 2018-08-27 | 2018-08-27 | A kind of waste water treatment process in paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109020030A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117531790A (en) * | 2024-01-05 | 2024-02-09 | 定远县尚时新材料有限公司 | P-phenylenediamine production system with automatic cleaning device of pipeline |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1132347A2 (en) * | 2000-01-27 | 2001-09-12 | Noram Engineering & Constructors Ltd. | Integrated effluent treatment process for nitroaromatic manufacture |
| CN101585620A (en) * | 2009-06-26 | 2009-11-25 | 河北建新化工股份有限公司 | Method for comprehensively treating high salt content organic industrial wastewater |
| WO2013132294A1 (en) * | 2012-03-09 | 2013-09-12 | Biazzi S.A. | Process for treatment of waste water from nitro-aromatic production |
| CN103359862A (en) * | 2012-03-28 | 2013-10-23 | 杜惠红 | Process and system for treating nitrochlorobenzene ammonolysis wastewater |
| CN104445711A (en) * | 2014-10-29 | 2015-03-25 | 绍兴奇彩化工有限公司 | Treatment method for aniline wastewater |
| CN105884098A (en) * | 2016-05-30 | 2016-08-24 | 中北大学 | Method and device for treating nitrobenzene wastewater through ultrasonic wave/iron-carbon micro-electrolysis-Fenton oxidation method |
| CN205917103U (en) * | 2016-07-06 | 2017-02-01 | 姚俊 | Processing apparatus of dinitroaniline class pesticide waste water |
-
2018
- 2018-08-27 CN CN201810978992.3A patent/CN109020030A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1132347A2 (en) * | 2000-01-27 | 2001-09-12 | Noram Engineering & Constructors Ltd. | Integrated effluent treatment process for nitroaromatic manufacture |
| CN101585620A (en) * | 2009-06-26 | 2009-11-25 | 河北建新化工股份有限公司 | Method for comprehensively treating high salt content organic industrial wastewater |
| WO2013132294A1 (en) * | 2012-03-09 | 2013-09-12 | Biazzi S.A. | Process for treatment of waste water from nitro-aromatic production |
| CN103359862A (en) * | 2012-03-28 | 2013-10-23 | 杜惠红 | Process and system for treating nitrochlorobenzene ammonolysis wastewater |
| CN104445711A (en) * | 2014-10-29 | 2015-03-25 | 绍兴奇彩化工有限公司 | Treatment method for aniline wastewater |
| CN105884098A (en) * | 2016-05-30 | 2016-08-24 | 中北大学 | Method and device for treating nitrobenzene wastewater through ultrasonic wave/iron-carbon micro-electrolysis-Fenton oxidation method |
| CN205917103U (en) * | 2016-07-06 | 2017-02-01 | 姚俊 | Processing apparatus of dinitroaniline class pesticide waste water |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117531790A (en) * | 2024-01-05 | 2024-02-09 | 定远县尚时新材料有限公司 | P-phenylenediamine production system with automatic cleaning device of pipeline |
| CN117531790B (en) * | 2024-01-05 | 2024-04-05 | 定远县尚时新材料有限公司 | P-phenylenediamine production system with automatic cleaning device of pipeline |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109455885B (en) | Nitrogen resource heat extraction and recovery method | |
| CN109455884A (en) | A kind of nitrogen resource thermal extraction recovery system | |
| CN105217869B (en) | The method of resource of spent acid a kind of generated in flue gas during smelting Sulphuric acid | |
| CN109019634A (en) | The purification of chemical industry abraum salt and resource utilization system and method | |
| CN1986390A (en) | Process of purifying and recovering waste sulfuric acid containing organic impurity | |
| CN106744721A (en) | The recovery separation method and application of sulfuric acid and dissolubility titanium in titanium white waste acid | |
| CN111635086A (en) | Zero discharge system for producing ammonium salt from ammonia nitrogen-containing wastewater and treatment process thereof | |
| CN109704492A (en) | A kind of abraum salt harmless resource processing system | |
| CN109912096A (en) | A kind of pretreated method of o-methyl formate benzene sulfonamide waste water sub-prime | |
| CN106809836B (en) | The by-product potassium carbonate purification purification recovery method of Herbicide Jing quizalofop-ethyl | |
| CN111620504A (en) | Production method of novel process for treating prewashing wastewater in polynitrotoluene production | |
| CN107129098B (en) | High concentration hard-degraded organic waste water treatment process with high salt | |
| CN102153224A (en) | Treatment technology for industrial sewage from sodium carboxymethylcellulose | |
| CN109020030A (en) | A kind of waste water treatment process in paranitroanilinum, ortho-nitraniline and corresponding phenyl amines chemical production process | |
| CN104528989A (en) | High-ammonia-nitrogen wastewater treatment ammonia recycling system | |
| CN109651052A (en) | The treatment process and processing system of methanol toluene production styrene high-concentration waste water | |
| CN215592846U (en) | Dirty sour effluent disposal system | |
| CN1814546B (en) | Method for producing general superphosphate from waste water of yellow ginger processing by dry method | |
| CN103435226B (en) | Comprehensive treatment technology for formation water in natural gas extraction | |
| CN110790440B (en) | High COD high salt wastewater treatment system | |
| CN115838216A (en) | Coal chemical wastewater treatment method and system | |
| CN109721035B (en) | Purification and concentration process of waste dilute sulfuric acid | |
| CN107686193A (en) | A kind of method for handling high-concentration sulfuric acid ammonium waste water | |
| CN102153223A (en) | Sodium carboxymethylcellulose industrial sewage recycling device | |
| CN113087424A (en) | Phosphogypsum closed internal circulation pretreatment process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181218 |
|
| WD01 | Invention patent application deemed withdrawn after publication |