CN106630345A - Electrolytic oxidation treatment process of intermediate 2-chloronicotinic acid production wastewater - Google Patents
Electrolytic oxidation treatment process of intermediate 2-chloronicotinic acid production wastewater Download PDFInfo
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- CN106630345A CN106630345A CN201611015546.XA CN201611015546A CN106630345A CN 106630345 A CN106630345 A CN 106630345A CN 201611015546 A CN201611015546 A CN 201611015546A CN 106630345 A CN106630345 A CN 106630345A
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- Prior art keywords
- electrolytic oxidation
- regulating reservoirs
- waste water
- nicotinic acid
- oxidation process
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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
-
- 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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
-
- 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
- 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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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses an electrolytic oxidation treatment process of intermediate 2-chloronicotinic acid production wastewater. The electrolytic oxidation treatment process comprises the specific steps of wastewater pretreatment operation, electrolytic oxidation treatment operation and ultimate treatment product disposal operation. Free radicals having strong oxidizing property are produced in an electrolysis mode, oxidation water is polluted by organic matter, the biodegradability of the wastewater is further improved through a series of treatment processes, part of COD and ammonia nitrogen in the production wastewater are degraded, and the treatment cost is reduced and the environment pollution is reduced on the premise that the sewage is effectively treated; sulfonated polystyrene resin is used as a carrier, metal ions Fe<2+>, Mn<2+> Cr<3+> and the like are used as active components, the active components metal ions are respectively supported on the sulfonated polystyrene resin carrier by adopting an ion exchange method, the active components can be prevented from producing clusters, it is ensured that the active sites of the active components are fully exposed, the dispersity and the liquidity of the active components are improved, the COD treatment efficiency is improved, and the construction cost of a catalyst is low.
Description
Technical field
The present invention relates to treat the technical field of pharmaceuticals of human body blood-head, specially a kind of intermediate dichloro-nicotinic acid produces waste water
Electrolytic oxidation process technique.
Background technology
2- chlorine apellagrins are a kind of important medical and pesticide intermediates, of many uses, can be used to manufacture VP-74, cigarette fluorine
Fenamic acid, nicosulfuron, Diflufenican etc..Electrolytic oxidation Industrial Wastewater Treatment catalyst of traditional handicraft and preparation method thereof is deposited
Catalyst cost is high, equipment investment is high, the shortcomings of active low service life is short.Therefore invest within 2014 and newly-built day process 800
The sewage disposal system of ton production waste water.The high COD features of waste water are produced according to plant area, the project is devoted to electrolytic oxidation in dichloro
Application study in cigarette acid producing waste water, improves the biodegradability of waste water, and degrade part COD and ammonia nitrogen in production waste water,
To reduce environmental pollution.
The content of the invention
Based on the technical problem that this background technology is present, the present invention proposes a kind of intermediate dichloro-nicotinic acid production waste water
Electrolytic oxidation process technique.
A kind of intermediate dichloro-nicotinic acid proposed by the present invention produces the electrolytic oxidation process technique of waste water, concretely comprises the following steps：
A) Wastewater Pretreatment operation
The first step, by the dichloro-nicotinic acid production discharge of wastewater of collection feed liquor bucket is entered；
Second step, the outlet end of feed liquor bucket is filtered through filter grid coral；
3rd step, by the filtrate of filter grid coral rectifying column is passed through, and output object is passed through into condenser after abundant rectifying；
4th step, by the product of condenser outlet end by reboiler, fully Jing tapping buckets flow out after reaction.
B) electrolytic oxidation process operation
The first step, the water body that tapping bucket flows out is carried out sufficiently cool, and is passed through a PH regulating reservoirs；
Second step, by acidic materials are added in a PH regulating reservoirs PH is adjusted, and adds hydrogen peroxide fully oxidized；
3rd step, is passed through the final reacting product of a PH regulating reservoirs the first electrolysis reactor and is sufficiently electrolysed；
4th step, by the final product of the first electrolysis reactor just subplate press filtration is carried out；
5th step, by the water body after first subplate press filtration the 2nd PH regulating reservoirs are passed through；
6th step, by the inside of the 2nd PH regulating reservoirs alkali lye is added into, and adjusts PH；
7th step, by the outlet end of the 2nd PH regulating reservoirs the second electrolysis reactor is also associated with；
8th step, after water body is fully reacted in the second electrolysis reactor, being passed through carries out two subplate press filtrations；
9th step, by the product of two subplate press filtrations final process operation is carried out.
C) operation of product final process is processed
The product withdraw of two subplate press filtrations is catalyzed to outside purifying and catalyzing container, and purifying and catalyzing container goes out
Liquid end is discharged in water body after process, and after collection bucket is collected outward transport process is carried out.
Preferably, the filter residue discharge section of the filter grid coral is connected with residue collection pond, the discharging in the residue collection pond
End is also communicated with drying machinery and outward transport machinery.
Preferably, a PH regulating reservoirs are externally connected to sulfuric acid addition bucket and hydrogen peroxide addition bucket, and protect after modulating
The pH value for holding a PH regulating reservoirs is 3.
Preferably, a PH regulating reservoirs, the inside of the 2nd PH regulating reservoirs are equiped with stirring, mixed structure part, and
Liquid level bottom is also equiped with pH sensor.
Preferably, the ft connection of the 2nd PH regulating reservoirs has alkali lye addition bucket, and the pH value dimension of the 2nd PH regulating reservoirs
Hold as 9.
Preferably, the outlet end of the purifying and catalyzing container is also equiped with COD analyzers.
Preferably, the outlet end of the purifying and catalyzing container also interlinks and is connected to return duct, the inside dress of the return duct
Drawing liquid pump is provided with, and the end of return duct is connected with a PH regulating reservoirs.
Preferably, the purifying and catalyzing container is with sulfonated polystyrene ion exchange resin as carrier, with metal cations Fe 2+, Mn2+,
Cr3+ etc. is active component, using ion-exchange, activity component metal ion is carried on respectively into the sulfonated polystyrene
On resin carrier.
Beneficial effects of the present invention are as follows：
1st, the free radical of strong oxidizing property, Organic Pollutants in oxidation water, by series of processes are produced by way of electrolysis
Technique, further improves the biodegradability of waste water, part COD and ammonia nitrogen in degraded production waste water, it is ensured that sewage is effectively controlled
On the premise of reason, processing cost is reduced, reduce environmental pollution；
2nd, with sulfonated polystyrene ion exchange resin as carrier, with metal cations Fe 2+, Mn2+, Cr3+ etc. as active component, adopt
Ion-exchange, activity component metal ion is carried on respectively on the sulfonated polystyrene ion exchange resin carrier, can effectively be prevented
Only there is cluster in active component, it is ensured that the active sites exposure of active component is abundant, improve the dispersiveness and circulation of active component,
COD treatment effeciencies, and catalyst low cost are improve, the requirement for using is met；
3rd, by carrying out the regulation and control of pH value, the treatment effeciency in dichloro-nicotinic acid production waste water is further increased, is reduced
Environmental pollution.
Description of the drawings
Fig. 1 is present configuration block diagram；
Fig. 2 is that Wastewater Pretreatment of the present invention operates structured flowchart；
Fig. 3 is purifying and catalyzing container inner structure block diagram of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
A kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, concretely comprises the following steps：
A) Wastewater Pretreatment operation
The first step, by the dichloro-nicotinic acid production discharge of wastewater of collection feed liquor bucket is entered；
Second step, the outlet end of feed liquor bucket is filtered through filter grid coral, and the filter residue discharge section of filter grid coral is connected with filter residue
Collecting pit, the discharge end in the residue collection pond is also communicated with drying machinery and outward transport machinery；
3rd step, by the filtrate of filter grid coral rectifying column is passed through, and output object is passed through into condenser after abundant rectifying；
4th step, by the product of condenser outlet end by reboiler, fully Jing tapping buckets flow out after reaction.
B) electrolytic oxidation process operation
The first step, the water body that tapping bucket flows out is carried out sufficiently cool, and is passed through a PH regulating reservoirs；
Second step, by acidic materials are added in a PH regulating reservoirs PH is adjusted, and adds hydrogen peroxide fully oxidized, a PH
Regulating reservoir is externally connected to sulfuric acid addition and struggles against and hydrogen peroxide addition bucket, and the pH value of the first PH regulating reservoirs of holding is 3 after modulating；
3rd step, is passed through the final reacting product of a PH regulating reservoirs the first electrolysis reactor and is sufficiently electrolysed；
4th step, by the final product of the first electrolysis reactor just subplate press filtration is carried out；
5th step, by the water body after first subplate press filtration the 2nd PH regulating reservoirs are passed through；
6th step, by the inside of the 2nd PH regulating reservoirs alkali lye is added into, and adjusts PH, and a PH regulating reservoirs, the 2nd PH are adjusted
The inside in pond is equiped with stirring, mixed structure part, and liquid level bottom and is also equiped with pH sensor, outside the 2nd PH regulating reservoirs
Portion is communicated with alkali lye addition bucket, and the pH value of the 2nd PH regulating reservoirs is maintained 9；
7th step, by the outlet end of the 2nd PH regulating reservoirs the second electrolysis reactor is also associated with；
8th step, after water body is fully reacted in the second electrolysis reactor, being passed through carries out two subplate press filtrations；
9th step, by the product of two subplate press filtrations final process operation is carried out.
C) operation of product final process is processed
The product withdraw of two subplate press filtrations is catalyzed to outside purifying and catalyzing container, and purifying and catalyzing container goes out
Liquid end is discharged in water body after process, and after collection bucket is collected outward transport process is carried out, and the outlet end of purifying and catalyzing container is also
COD analyzers are equiped with, the outlet end of purifying and catalyzing container also interlinks and is connected to return duct, and the inside of the return duct is equiped with
Drawing liquid pump, and the end of return duct is connected with a PH regulating reservoirs, purifying and catalyzing container with sulfonated polystyrene ion exchange resin as carrier,
With metal cations Fe 2+, Mn2+, Cr3+ etc. as active component, using ion-exchange, activity component metal ion is born respectively
It is loaded on the sulfonated polystyrene ion exchange resin carrier.
This project meets《The high-technology field that state key is supported》2nd, it is biological to research and develop skill with new medicine (three) chemical drugs
" production technology of important intermediate, is greatly reduced environment to the technology of art 5, national essential drugs bulk drug and important intermediate
Pollution, medicine that is energy-saving and significantly reducing production cost and medicine intermediate technology ".
Core technology：1. the electrolytic oxidation wastewater processing technology of environmental pollution is reduced；2. the height for improving COD treatment effeciencies is living
Property component ion exchange technique.
Electrolytic oxidation produces the application study in waste water in dichloro-nicotinic acid, mainly using electrolytic oxidation method, by series
Handling process produces part COD and ammonia nitrogen in waste water to improve the biodegradability of waste water, and degrade, it is ensured that sewage is effectively controlled
On the premise of reason, processing cost is reduced, reduce environmental pollution.
The main research of this project include it is following some：(1) analysis of main component in waste water is produced；(2) it is electrolysed
The design of oxidation technology scheme；(3) lab scale of electrolysis oxidation process, amplification；
Innovative point：(1) technique of the project research is COD and NH_3-N treating technique in dichloro-nicotinic acid production waste water, is adopted
Electrolytic oxidation, with the characteristic of low voltage and high current waste water is processed, and processes economy and the feature of environmental protection is projected；(2) electrolytic oxidation side
Case design and optimization, the regulation and control of pH value in processing procedure.
Test method and technology path
Test method：The test method of the project is to adopt electrolytic oxidation method, production waste water first after the pre-treatment
In plus sulfuric acid adjust PH to 3, and add hydrogen peroxide, the laggard andante block press filtration of process of Jing electrolysis reactors, the portion in degraded production waste water
Divide COD, it is that 9, Jing electrolysis reactors process laggard andante block press filtration then to add liquid caustic soda to adjust PH again, the part produced in waste water of degrading
Ammonia nitrogen.Production waste water Jing after electrolytic oxidation is again Jing after the handling process of other schemes is processed, and it is comprehensive that waste water can reach national sewage
The one-level for closing discharge standard requires that i.e. CODcr≤100mg/L is discharged.
Technology path：(1) the optimal PH environment of degraded COD and ammonia nitrogen is studied first；(2) by experiment, design electrolysis oxygen
Change handling process scheme；(3) control of the temperature of electrolytic acid cleaning oxydation process and speed and optimization.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each
Embodiment only includes an independent technical scheme, and this narrating mode of specification is only this area for clarity
Technical staff should using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form this
Art personnel may be appreciated other embodiment.
Claims (8)
1. a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that：Concretely comprise the following steps：
A) Wastewater Pretreatment operation
The first step, by the dichloro-nicotinic acid production discharge of wastewater of collection feed liquor bucket is entered；
Second step, the outlet end of feed liquor bucket is filtered through filter grid coral；
3rd step, by the filtrate of filter grid coral rectifying column is passed through, and output object is passed through into condenser after abundant rectifying；
4th step, by the product of condenser outlet end by reboiler, fully Jing tapping buckets flow out after reaction.
B) electrolytic oxidation process operation
The first step, the water body that tapping bucket flows out is carried out sufficiently cool, and is passed through a PH regulating reservoirs；
Second step, by acidic materials are added in a PH regulating reservoirs PH is adjusted, and adds hydrogen peroxide fully oxidized；
3rd step, is passed through the final reacting product of a PH regulating reservoirs the first electrolysis reactor and is sufficiently electrolysed；
4th step, by the final product of the first electrolysis reactor just subplate press filtration is carried out；
5th step, by the water body after first subplate press filtration the 2nd PH regulating reservoirs are passed through；
6th step, by the inside of the 2nd PH regulating reservoirs alkali lye is added into, and adjusts PH；
7th step, by the outlet end of the 2nd PH regulating reservoirs the second electrolysis reactor is also associated with；
8th step, after water body is fully reacted in the second electrolysis reactor, being passed through carries out two subplate press filtrations；
9th step, by the product of two subplate press filtrations final process operation is carried out.
C) operation of product final process is processed
The product withdraw of two subplate press filtrations is catalyzed to outside purifying and catalyzing container, the outlet end of purifying and catalyzing container
Water body after process is discharged, after collection bucket is collected outward transport process is carried out.
2. as claimed in claim 1 a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that
The filter residue discharge section of the filter grid coral is connected with residue collection pond, and the discharge end in the residue collection pond is also communicated with dryer
Tool and outward transport machinery.
3. as claimed in claim 1 a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that
The first PH regulating reservoirs are externally connected to sulfuric acid addition bucket and hydrogen peroxide addition bucket, and a PH regulating reservoirs are kept after modulating
PH value is 3.
4. as claimed in claim 1 a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that
The first PH regulating reservoirs, the inside of the 2nd PH regulating reservoirs are equiped with stirring, mixed structure part, and liquid level bottom is also equiped with
PH sensor.
5. as claimed in claim 1 a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that
The ft connection of the 2nd PH regulating reservoirs has alkali lye addition bucket, and the pH value of the 2nd PH regulating reservoirs is maintained 9.
6. as claimed in claim 1 a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that
The outlet end of the purifying and catalyzing container is also equiped with COD analyzers.
7. as claimed in claim 1 a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that
The outlet end of the purifying and catalyzing container also interlinks and is connected to return duct, and the inside of the return duct is equiped with drawing liquid pump, and returns
The end of flow tube is connected with a PH regulating reservoirs.
8. as claimed in claim 1 a kind of intermediate dichloro-nicotinic acid produces the electrolytic oxidation process technique of waste water, it is characterised in that
The purifying and catalyzing container with sulfonated polystyrene ion exchange resin as carrier, with metal cations Fe 2+, Mn2+, Cr3+ etc. as activearm
Point, using ion-exchange, activity component metal ion is carried on respectively on the sulfonated polystyrene ion exchange resin carrier.
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| CN201611015546.XA CN106630345A (en) | 2016-11-18 | 2016-11-18 | Electrolytic oxidation treatment process of intermediate 2-chloronicotinic acid production wastewater |
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| CN201611015546.XA CN106630345A (en) | 2016-11-18 | 2016-11-18 | Electrolytic oxidation treatment process of intermediate 2-chloronicotinic acid production wastewater |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395035A (en) * | 2018-04-24 | 2018-08-14 | 浙江荣凯科技发展有限公司 | A kind of dichloro-nicotinic acid electrolytic oxidation process device |
| CN108529804A (en) * | 2018-04-24 | 2018-09-14 | 浙江荣凯科技发展有限公司 | A kind of dichloro-nicotinic acid production sewage treatment device |
| CN108635947A (en) * | 2018-04-24 | 2018-10-12 | 浙江荣凯科技发展有限公司 | A kind of dichloro-nicotinic acid production filter |
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| CN1792825A (en) * | 2005-11-22 | 2006-06-28 | 宜宾天原股份有限公司 | Process for treating hydrazine hydrate waste salt water by ketone linking nitrogen method |
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Application publication date: 20170510 |