CN106477809A - A kind of method that caprolactam wastewater is processed - Google Patents
A kind of method that caprolactam wastewater is processed Download PDFInfo
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- CN106477809A CN106477809A CN201610927362.4A CN201610927362A CN106477809A CN 106477809 A CN106477809 A CN 106477809A CN 201610927362 A CN201610927362 A CN 201610927362A CN 106477809 A CN106477809 A CN 106477809A
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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
- C02F1/24—Treatment of water, waste water, or sewage by flotation
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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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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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
- C02F2103/34—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
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
Abstract
The invention provides a kind of method that caprolactam wastewater is processed, comprise the following steps：(1) oximate device, hydrogen peroxide refined wastewater initially enter oil interceptor, oil recovery, and waste water enters pH regulator pond, then pre-oxidizes through ferrum carbon pond, enters back into Fenton oxidation pond and aoxidize further, water outlet is through coagulating kinetics；(2) other process section waste water of the water after processing step 1 and on-site, sanitary sewage and device flushing water enter the comprehensive adjustment pond regulating water quality water yield after mixing, composite waste enters hydrolysis acidification system after the process of one-level flotation tank, and water outlet enters back into A/O biochemical system and processes；(3) bio-chemical effluent in step 2 enters ozone oxidation pond after the process of secondary air-floatation pond, processes discharge through MBR pond again after the degassed process of waste water.The present invention is good to pollutant removal, system run all right, builds simultaneously and is all significantly lower than handling process of the same trade with operating cost.
Description
Technical field
The invention belongs to field of waste water treatment and in particular to a kind of caprolactam wastewater process method.
Background technology
Caprolactam is a kind of important Organic Chemicals, is mainly used to manufacture polyamide -6 fiber, caprolactam work
Engineering plastics etc., the product of manufacture is widely used in the fields such as automobile, ship, medical article, electronics, article of everyday use.Caprolactam is given birth to
Product need to be through the chemical process of series of complex, in oxime method production process, including the condensation reaction of Ketohexamethylene and oxyammonia sulfate
Obtain Ketohexamethylene, the latter, under oleum catalytic condition, occurs Beckmann rearrangement to obtain crude caprolactam under high temperature,
Obtain caprolactam after multiple tracks concentrating and purifying again.Need in caprolactam production process to consume a large amount of water, simultaneously each production
Link can give off the waste water of a large amount of different qualities again, and wherein main sewage source includes hydrogen peroxide refined wastewater, oximate device,
Reset waste water, pimelinketone device, hydrogen peroxide plant, desalted water acid-base waste fluid, device flushing water；Additionally, also including on-site
Sanitary sewage.Wherein hydrogen peroxide refined wastewater CODCrIn more than 15000mg/L, oximate device waste discharge CODCrIn 7000mg/
More than L, both waste water belongs to high-concentration hardly-degradable waste water, has very strong bio-toxicity, the biological treatment side of routine
Method cannot realize effective removal of pollutant.And the concentration of organic wastewater of other operations discharge is less than above two waste water, such as
The completely independent decentralized processing of fruit, can greatly increase the input cost of equipment；And direct mixed processing, reagent cost can be increased simultaneously again
And affect the stability of processing system.
At present, the commonly used biochemical process of domestic existing caprolactam wastewater is processed, but carries with discharge of wastewater water quality requirement
Height, merely biochemical mode be unable to reach emission request.Then occur in that the preprocessing means such as Fenton oxidation, ozone oxidation combine life
The processing mode of change method, obtains reasonable treatment effect, but the water yield processing is relatively fewer, is often directed to acyl in oneself
Amine produces the concentrated water part of waste water, and to on-site, other most of waste water do not provide clearly rational processing mode.Membrane processing method
It is also study hotspot in recent years, but the membrane pollution problem that simple film process mode causes can't solve well.State
Inside and outside have also appeared the processing modes such as salting out method, wet oxidation process, high temperature incineration method, these modes can more thoroughly remove
Pollutant, but still suffer from processing high energy consumption, the big problem of cost.
In sum, to the object of wastewater of caprolactam production research be often at this stage a certain section of high concentration waste water
Process, or after biochemical treatment waste discharge advanced treating scheme, lack systematic process, can be efficiently steady
Determine, reach emission request at low cost.
Content of the invention
It is an object of the invention to provide the method processing caprolactam wastewater, caprolactam factory can be arranged by the method
The all waste water put all effectively processed it is ensured that water outlet safe and reliable, and greatly reduce investment and operating cost.
For reaching above-mentioned purpose, the present invention adopts following technical proposals：
A kind of method that caprolactam wastewater is processed, comprises the following steps：
1) oximate device waste water, hydrogen peroxide refined wastewater initially enter oil interceptor, and wherein oils is reclaimed by oil sump, give up
Water enters pH regulator pond, then pre-oxidizes through ferrum carbon pond, enters back into Fenton oxidation pond and aoxidize further, and water outlet precipitates through preliminary sedimentation tank
Process；
2) after other process section waste water of the water after processing step 1 and on-site, sanitary sewage and device flushing water mix
After entering the comprehensive adjustment pond regulating water quality water yield, composite waste enters hydrolytic tank after the process of one-level flotation tank, and water outlet enters back into
A/O biochemical system is processed；
3) bio-chemical effluent in step 2 enters ozone pond, waste water warp after passing sequentially through second pond and the process of secondary air-floatation pond
Stripping pond processes discharge through MBR pond after processing again.
As preferred technical scheme：
The method that a kind of caprolactam wastewater of the present invention is processed, described step 1) in pH regulator pond adjusting water outlet pH
In 2-4.
The method that a kind of caprolactam wastewater of the present invention is processed, described step 1) in ferrum carbon pond adopt ferrum material with carbon element
For hollow cylinder build, iron-holder is more than 90%.
The method that a kind of caprolactam wastewater of the present invention is processed, described step 1) Fenton oxidation adds dioxygen in pond
Water concentration is 30%w/w, is 1 with Organic substance mass ratio:1-3:1；The ferrous mol ratio that adds with hydrogen peroxide is 2:1-3:1.
The method that a kind of caprolactam wastewater of the present invention is processed, described step 1) in preliminary sedimentation tank flocculant using sun
Polyacrylamide.
The method that a kind of caprolactam wastewater of the present invention is processed, described step 2) in be mounted with ester inside hydrolytic tank
Change fiberfill, described filler diameter 80-150mm, long 1.5m；Waste water time of staying in described hydrolytic tank is 20-30h.
The method that a kind of caprolactam wastewater of the present invention is processed, described step 2) in A/O biochemical system include according to
The anaerobic pond of secondary connection and Aerobic Pond, take the mode of internal reflux, and described reflux ratio is 100-300%；The anaerobic pond time of staying
For 20-30h, the Aerobic Pond time of staying is 65-75h.
The method that a kind of caprolactam wastewater of the present invention is processed, ozone dosage in ozone pond in described step 3
For 30-50mg/L；The time of staying in ozone pond for the waste water is 50-70min.
The method that a kind of caprolactam wastewater of the present invention is processed, described step 3) in MBR system adopt PVDF to put down
Plate film, described membrane aperture is less than 0.1 μm.
The method that a kind of caprolactam wastewater of the present invention is processed, described step 3) sludge concentration is in MBR system
4000-6000mg/L, operational mode is to take out 8min, stops 2min.
Compared with prior art, its advantage is mainly reflected in the following aspects to the present invention：
1st, high treating effect of the present invention, system run all right, effluent quality being capable of stably reaching standard.
2nd, the present invention greatly reduces project cost, and wherein project investment cost can reduce 50%, and operating cost can
Reduce 30%.
3rd, the present invention is truly realized the dual treatment of waste water, and each processing unit has given full play to respective advantage.
Brief description
Fig. 1 is the process route view of the present invention.
In figure：1 oil interceptor；2 oil sumps；3 pH regulator ponds；4 ferrum carbon ponds；5 Fenton oxidation ponds；6 is just heavy
Pond；7 comprehensive adjustment ponds；8 one-level flotation tanks；9 hydrolytic tanks；10 anaerobic ponds；11 Aerobic Ponds；12 second ponds；
13 secondary air-floatation ponds；14 ozone ponds；15 stripping ponds；16 MBR ponds.
Specific embodiment
The present invention is further described with reference to the accompanying drawings and examples.
The method that a kind of caprolactam wastewater of the present invention is processed, comprises the following steps：
1) oximate device waste water, hydrogen peroxide refined wastewater initially enter oil interceptor 1, and wherein oils is reclaimed by oil sump 2,
Waste water enters pH regulator pond 3, then pre-oxidizes through ferrum carbon pond 4, enters back into Fenton oxidation pond 5 and aoxidize further, water outlet is through just sinking
Pond 6 precipitation process；
2) after other process section waste water of the water after processing step 1 and on-site, sanitary sewage and device flushing water mix
After entering the comprehensive adjustment pond 7 regulating water quality water yield, composite waste enters hydrolytic tank 9 after one-level flotation tank 8 process, and water outlet is entered again
Enter A/O biochemical system to process；
3) bio-chemical effluent in step 2 enters ozone pond 14 after passing sequentially through second pond 12 and secondary air-floatation pond 13 process,
Waste water processes discharge through MBR pond after the process of stripping pond again.
Embodiment one：
Referring to Fig. 1, hydrogen peroxide refined wastewater and oximate device waste discharge enter oil interceptor 1 first, are gone using action of gravity
Except most of heavy oil, light oil etc.；Oils is reclaimed by oil sump 2, oil interceptor 1 water outlet enters to pH regulator pond 3, wastewater pH is adjusted
Save as 2-4, be conducive to follow-up pre-oxidation treatment；Water outlet flow to ferrum carbon pond 4, is polluted in waste water using iron salt and hydroxy compounds
Thing carries out preliminary decomposition；Water outlet flows into Fenton oxidation pond 5 again, enters one using Fenton oxidation system to hard-degraded substance in waste water
Step oxidation, improves the biodegradability of waste water；Water outlet adds PAMC and carries out at conventional precipitation in preliminary sedimentation tank 6
Reason；Substantially increase the biodegradability of waste water after above-mentioned pretreatment, B/C will be greater than 0.4, organic removal rate about 30%.
Oximate device, hydrogen peroxide refined wastewater flow into comprehensive adjustment pond 7 after pretreatment, and remaining several strands of waste water includes resetting
Waste water, pimelinketone device waste discharge, hydrogen peroxide plant waste discharge, desalted water acid-base waste fluid, device rinse water and life are dirty
Water, also into comprehensive adjustment pond 7, carries out water quality and quantity equilibrium using diving mixer in regulating reservoir；Water outlet is promoted to one-level air supporting
Pond 8, removes oil emulsion, float etc.；One-level flotation tank water outlet flows into hydrolytic tank 9, is mounted with to be esterified fiberfill, is micro- in pond
Biological enrichment provides condition, and hydrolytic tank is greatly improved giving birth to of waste water to hardly degraded organic substance in waste water by hydrolysis
The property changed；Hydrolysis water flows into A/O biochemical system, and anaerobic pond 10 plays the effect of degradation of organic substances and denitrogenation, and Aerobic Pond 11 plays
The effect of degradation of organic substances and nitrification further, the part effluent recycling after anaerobic pond 10 nitrification carries out denitrification to Aerobic Pond
Denitrogenation processing；Aerobic Pond water outlet flows into second pond 12 and carries out mud-water separation；Second pond 12 waste discharge ammonia nitrogen is less than 10m/L, COD
Less than 150mg/L.
Process through biochemical system, waste water flows into secondary air-floatation pond 13 from second pond 12, remove the activity of residual in waste water
Mud, float, colloidal impurity etc., can remove most of colourity simultaneously；Secondary air-floatation pond 13 water outlet enters ozone pond 14, utilizes
Ozone strong oxidizing technique, the hard-degraded substance in thorough Decomposition Wastewater；Waste water flows into MBR pond 16 after the stripping of stripping pond 15, profit
With the mud biochemical action in MBR pond and the filtration of Flat Membrane, further organics removal and float etc., final waste water row
Put ammonia nitrogen and be less than 5m/L, COD is less than 40mg/L, concentration of suspension is less than 10mg/L.
Embodiment two：
200,000 tons of caprolactam wastewater discharge engineerings, wherein hydrogen peroxide refining plant and pimelinketone device row is produced in Shanxi per year
Put waste water 550t/d, other devices waste discharge 3000t/d.Hydrogen peroxide refining plant and pimelinketone device waste discharge are through oil removal
Pond processes float and can reach 50% by clearance, and oils clearance reaches 90%, COD clearance and reaches 5%, through ferrum carbon and sweet smell
Oxidation pre-treatment, waste water COD clearance reaches 50%, and removal efficiency reaches 50%, B/C and is more than 0.4.
After air supporting-hydrolysis acidification-A/O- second pond is processed, COD clearance reaches 95%, BOD to comprehensive wastewater5Remove
Rate is 98%, and ammonia nitrogen removal frank reaches 99%.
After biochemical treatment, waste water is through ozone oxidation, after the biological advanced treating further of MBR film, final waste discharge COD
For 30mg/L, BOD5For 15mg/L, ammonia nitrogen concentration is less than 5mg/L.
Embodiment three：
200,000 tons of caprolactam wastewater discharge engineerings, wherein hydrogen peroxide refining plant and pimelinketone device row is produced in Shandong per year
Put waste water 550t/d, other devices waste discharge 3000t/d.Hydrogen peroxide refining plant and pimelinketone device waste discharge are through oil removal
Pond processes float and can reach 50% by clearance, and oils clearance reaches 90%, COD clearance and reaches 5%, through ferrum carbon and sweet smell
Oxidation pre-treatment, waste water COD clearance reaches 50%, and removal efficiency reaches 50%, B/C and is more than 0.4.
After air supporting-hydrolysis acidification-A/O- second pond is processed, COD clearance reaches 95%, BOD to comprehensive wastewater5Remove
Rate is 98%, and ammonia nitrogen removal frank reaches 99%.
After biochemical treatment, waste water is through ozone oxidation, after the biological advanced treating further of MBR film, final waste discharge COD
For 30mg/L, BOD5For 15mg/L, ammonia nitrogen concentration is less than 5mg/L.
Example IV：
Certain 200,000 tons of caprolactam wastewater discharge engineering of annual output of Shandong (eastern dimerization work), wherein hydrogen peroxide refining plant and ring
Hexanone device waste discharge 550t/d, other devices waste discharge 3000t/d.Hydrogen peroxide refining plant and pimelinketone device discharge
Waste water processes float through oil interceptor and can reach 50% by clearance, and oils clearance reaches 90%, COD clearance and reaches 5%,
Through ferrum carbon and Fenton oxidation pretreatment, waste water COD clearance reaches 55%, and removal efficiency reaches 55%, B/C and is more than 0.4.
After air supporting-hydrolysis acidification-A/O- second pond is processed, COD clearance reaches 96%, BOD to comprehensive wastewater5Remove
Rate is 99%, and ammonia nitrogen removal frank reaches 99%.
After biochemical treatment, waste water is through ozone oxidation, after the biological advanced treating further of MBR film, final waste discharge COD
For 35mg/L, BOD5For 18mg/L, ammonia nitrogen concentration is 4mg/L.
Claims (10)
1. a kind of method that caprolactam wastewater is processed is it is characterised in that comprise the following steps：
1) oximate device waste water, hydrogen peroxide refined wastewater initially enter oil interceptor, and wherein oils is reclaimed by oil sump, and waste water enters
Enter pH regulator pond, then pre-oxidize through ferrum carbon pond, enter back into Fenton oxidation pond and aoxidize further, water outlet is through preliminary sedimentation tank place of settling
Reason；
2) other process section waste water of the water after processing step 1 and on-site, sanitary sewage and device flushing water enter after mixing
After the regulating water quality water yield of comprehensive adjustment pond, composite waste enters hydrolytic tank after the process of one-level flotation tank, and water outlet enters back into A/O life
Change system is processed；
3) bio-chemical effluent in step 2 enters ozone pond after passing sequentially through second pond and the process of secondary air-floatation pond, and waste water is through stripping
Pond processes discharge through MBR pond after processing again.
2. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 1) in pH
Regulating reservoir adjusting water outlet pH is in 2-4.
3. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 1) in ferrum
It is hollow cylinder build that carbon pond adopts ferrum material with carbon element, and iron-holder is more than 90%.
4. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 1) Fenton
Adding hydrogen peroxide concentration in oxidation pond is 30%w/w, is 1 with Organic substance mass ratio:1-3:1；Ferrous iron is rubbed with adding of hydrogen peroxide
That ratio is 2:1-3:1.
5. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 1) just sink
In pond, flocculant adopts cationic-type polyacrylamide.
6. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 2) in water
It is mounted with inside Xie Chi to be esterified fiberfill, described filler diameter 80-150mm, long 1.5m；Waste water stops in described hydrolytic tank
Time is 20-30h.
7. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 2) in A/
O biochemical system includes the anaerobic pond being sequentially connected and Aerobic Pond, takes the mode of internal reflux, and described reflux ratio is 100-300%；
The anaerobic pond time of staying is 20-30h, and the Aerobic Pond time of staying is 65-75h.
8. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 3) ozone
In pond, ozone dosage is 30-50mg/L；The time of staying in ozone pond for the waste water is 50-70min.
9. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 3) in
MBR system adopts PVDF Flat Membrane, and described membrane aperture is less than 0.1 μm.
10. a kind of caprolactam wastewater according to claim 1 is processed method is it is characterised in that described step 3) MBR
In system, sludge concentration is 4000-6000mg/L, and operational mode is to take out 8min, stops 2min.
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Cited By (14)
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| CN108311071A (en) * | 2018-04-13 | 2018-07-24 | 中国平煤神马能源化工集团有限责任公司 | A kind of the photocatalysis microchannel processing unit and its processing method of caprolactam rearrangement reaction waste liquid |
| CN110563282A (en) * | 2019-10-10 | 2019-12-13 | 上海玉畔环保设备有限公司 | Treatment system and treatment method for amino resin production wastewater |
| CN110655272A (en) * | 2019-09-12 | 2020-01-07 | 聊城煤泗新材料科技有限公司 | Caprolactam wastewater treatment device and treatment method and application |
| CN110776193A (en) * | 2019-09-26 | 2020-02-11 | 浙江环森环境科技有限公司 | Nylon 6 wastewater treatment method |
| CN110818184A (en) * | 2019-11-15 | 2020-02-21 | 聊城市鲁西化工工程设计有限责任公司 | Biochemical treatment process for sewage of hydrogen peroxide production device |
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| CN110655272A (en) * | 2019-09-12 | 2020-01-07 | 聊城煤泗新材料科技有限公司 | Caprolactam wastewater treatment device and treatment method and application |
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