CN108529791A - The processing method of deep removal COD in a kind of raffinate from nickel cobalt - Google Patents
The processing method of deep removal COD in a kind of raffinate from nickel cobalt Download PDFInfo
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- CN108529791A CN108529791A CN201810408625.XA CN201810408625A CN108529791A CN 108529791 A CN108529791 A CN 108529791A CN 201810408625 A CN201810408625 A CN 201810408625A CN 108529791 A CN108529791 A CN 108529791A
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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
- C02F1/24—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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic 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
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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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)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses the processing methods of deep removal COD in raffinate from nickel cobalt a kind of, the waste water is first carried out coagulation demulsification processing by this method, it converts after suspended oil oil emulsion to and enters oil removal by air bubbling processing removing suspended oil, water outlet enters adsorption treatment depth oil removing, further through catalytic ozonation advanced treating, final outflow water COD ＜ 80mg/L after reduction COD；The technique solves the problems, such as that COD removings are difficult in nickel cobalt raffinate, water outlet COD is reduced to ＜ 100mg/L, technological process is simple, and operating cost is relatively low, has good market prospects.
Description
Technical field
From deep removal COD in sewage advanced treatment field more particularly to a kind of raffinate from nickel cobalt
Reason method.
Background technology
It is well known that the COD removals of nickel cobalt raffinate are always field of environment protection technical problem urgently to be resolved hurrily.Nickel cobalt raffinate
In organic matter there are various, be divided into suspended state, dispersed, emulsification state and solubilised state, suspended state and dispersed by existing forms
Through a long time, which is placed, can remove, it is difficult to predominantly emulsification state and the dissolved organic matter of removing.Extractant（P204/P507）, it is molten
Agent（Such as sulfonated kerosene）It is the key component of organic matter in nickel cobalt raffinate with extracted species etc., these organic matters are aliphatic hydrocarbon
Class, property are highly stable, it is extremely difficult to degrade.Currently, being directed to systems of the P204/P507 as extractant both at home and abroad, there are no can be with
Nickel cobalt raffinate COD is removed to 100mg/L mature technologies below.By repetition test and it is difficult study intensively, researcher is finally
The method for exploring deep removal COD in a kind of raffinate from nickel cobalt, compared to current industrial existing processing method, the party
Method not only COD can be removed to 80mg/L hereinafter, but also operating cost it is relatively low, have boundless application prospect.
Invention content
In view of the above-mentioned problems, the present invention provides the processing methods of deep removal COD in raffinate from cobalt plating a kind of, mainly
It is various for organic matter existing forms in nickel cobalt raffinate, emulsification state and the removal of dissolved organic matter difficulty, extractant, solvent and extraction
It closes the fat hydrocarbons matter properties such as object to stablize, it is extremely difficult to which the problem of degrading, COD in nickel cobalt raffinate can be dropped by providing one kind
To less than the new method of 80mg/L.This method is emulsified by coagulation and first converts oil emulsion to suspended oil to be removed by air supporting
COD is reduced, then by absorption and catalysis oxidation depth degradation, final outflow water COD ＜ 80mg/L meet national integrated wastewater discharge
Standard, whole flow process is simple, and processing cost is relatively low, and suitable process is promoted.
For this purpose, the present invention uses following technical scheme：
The processing method of deep removal COD in a kind of raffinate from nickel cobalt, first carries out coagulation demulsification processing by the waste water, will be newborn
Carburetion enters oil removal by air bubbling processing removing suspended oil after being converted into suspended oil, and water outlet enters adsorption deeply oil removing, it is laggard to reduce COD
One step is through catalytic ozonation advanced treating, final outflow water COD ＜ 80mg/L.
Demulsifier is added into the waste water, is carried out coagulation demulsification processing, is converted oil emulsion to suspended oil；
The demulsifier dosage is 0.2 ~ 2g/L；
The coagulation demulsification time is 10 ~ 60min.
Water outlet enters oil removal by air bubbling and handles after coagulation demulsification processing, is 30 ~ 60min when stop；
Water outlet COD is 400 ~ 600mg/L after oil removal by air bubbling processing.
After water outlet pH is adjusted to 2 ~ 7 after oil removal by air bubbling is handled, adsorption deeply oil removal treatment is entered with 1 ~ 5BV/h flow velocitys, is inhaled
Attached water outlet COD is 100 ~ 200mg/L.
After absorption water outlet pH is adjusted to 7 ~ 9, into the degradation of catalytic ozonation system depth COD, water outlet COD ＜ 80mg/
L。
Hydrogen peroxide, hydrogen peroxide are added to catalytic ozonation system：COD is 1 ~ 2；Reaction time is 15 ~ 60min；Gas-liquid
Than being 1 ~ 5.
Sorbing material after adsorption deeply oil removal treatment is desorbed by strippant, and the strippant is preferably hydrogen-oxygen
Change one kind in sodium solution, ethanol solution, methanol solution or acetone soln；
Preferably, the strippant be sodium hydroxide solution, a concentration of 10% ~ 20%.
The strippant flow velocity is 1 ~ 2BV/h, and desorption time is 4 ~ 6h.
When strippant is sodium hydroxide solution, stripping liquid returns to extractant saponification process reuse.
When strippant is a kind of in ethanol solution, methanol solution or acetone soln, stripping liquid goes to distillation system point
It is more than 99.5% from recycling strippant and oil, the strippant rate of recovery.
Compared with prior art, the invention has the advantages that：
1）The invention discloses the processing method of deep removal COD in raffinate from nickel cobalt a kind of, the method achieve by P204/
Nickel cobalt raffinate removing COD water outlet ＜ 100mg/Ls of the P507 as extraction system;
2）The present invention solves the problems, such as that oil emulsion is intractable by coagulation demulsification, converts oil emulsion to suspended oil removal, inhales
Attached oil removing removal dispersed oil reduces COD, and catalytic ozonation depth degradation hardly degraded organic substance is final to realize that COD is up to standard.
3）Present invention process flow is simple, and operating cost is relatively low, has boundless application prospect.
Description of the drawings
Fig. 1 is the process flow figure that the present invention removes COD deeply from nickel cobalt raffinate.
Specific implementation mode
For the present invention is better described, it is easy to understand technical scheme of the present invention, of the invention is typical but non-limiting
Embodiment is as follows：
As shown in Figure 1, in a kind of raffinate from nickel cobalt deep removal COD processing method, this method first gives up nickel cobalt raffinate
Water carries out coagulation demulsification processing, converts after suspended oil oil emulsion to and enters oil removal by air bubbling processing removing suspended oil, and water outlet enters
Adsorption treatment depth oil removing, reduce COD after further through catalytic ozonation advanced treating, final outflow water COD ＜ 80mg/L.
Demulsifier, and mechanical agitation are added into nickel cobalt raffinate waste water, carry out coagulation demulsification processing, oil emulsion is converted
For suspended oil；Wherein demulsifier dosage be 0.2 ~ 2g/L, 0.2g/L, 0.3 g/L, 0.4 g/L, 0.5 g/L, 0.6 g/L,
0.7 g/L、0.8 g/L、0.9 g/L、1 g/L、1.2 g/L、1.5 g/L、1.6 g/L、1.8 g/L、1.9 g/L、2 g/L；
The coagulation demulsification time be 10 ~ 60min, 10min, 11min, 12 min, 15 min, 18 min, 20 min, 25min, 30min,
35min、40min、45min、50min、55min、60min。
Water outlet enters oil removal by air bubbling and handles after coagulation demulsification processing, is 30 ~ 60min when stop, 30min, 35min,
40min、45min、50min、55min、60min；It is 400 ~ 600mg/L, 400 mg/L, 420 mg/ that COD is discharged after air-flotation process
L、450 mg/L、480 mg/L、500 mg/L、520 mg/L、550 mg/L、580 mg/L、600 mg/L。
It is adjusted to 2 ~ 7,2,3,4,5,6,7 by pH is discharged after air-flotation process（1 is adjusted in figure）, suction is entered with 1 ~ 5BV/h flow velocitys
Attached processing oil removing, absorption water outlet COD is 100 ~ 200m/L, 100m/L, 120 m/L, 150 m/L, 180 m/L, 190 m/L, 200
m/L。
After absorption water outlet pH is adjusted to 7 ~ 9, into catalytic oxidation system depth degradation COD, water outlet COD ＜ 80mg/L.
Hydrogen peroxide, hydrogen peroxide are added to catalytic ozonation system：COD is 1 ~ 2；Reaction time is 15 ~ 60min,
15min、20min、25min、30 min、35 min、40 min、45 min、50 min、55 min、60min；Gas liquid ratio be 1 ~
5,1,2,3,4,5.
Sorbing material after adsorption deeply oil removing reaction is desorbed by strippant, and strippant is preferably sodium hydroxide
One kind in solution or ethanol solution, methanol solution or acetone soln；
Preferably, strippant is sodium hydroxide solution, a concentration of 10% ~ 20%, 10%, 12%, 15%, 18%, 20%.
Strippant flow velocity is 1 ~ 2BV/h, and desorption time is 4 ~ 6h, 4h, 5h, 6h（2 are adjusted in figure）.
When strippant is sodium hydroxide solution, stripping liquid returns to extractant saponification process reuse.
When stripping liquid is a kind of in ethanol solution, methanol solution or acetone soln, stripping liquid goes to distillation system point
It is more than 99.5% from recycling strippant and oil, the strippant rate of recovery.
Embodiment 1：
Certain cobalt manufacturing enterprise cobalt raffinate, main component are sodium sulphate, pH=4.56, COD 1500mg/L.
Step（1）：The above-mentioned waste water of 20L is taken, 0.2g/L demulsifiers are added, are stirred to react 30min；
Step（2）：Step（1）Water outlet enters air supporting Slag Scraping Device, and residence time 30min, water outlet COD are 400mg/L；
Step（3）：Step（2）Sulphur acid for adjusting pH=2 are added in water outlet, subsequently into oil removing adsorption column.Adsorption column water inlet flow velocity be
5BV/h, water outlet COD are 120mg/L.
Step（4）：Step（3）Water outlet is added sodium hydroxide and adjusts pH=7, subsequently into catalyst oxidation reactor.Dioxygen
Water：COD（Mass concentration is）It is 1, gas liquid ratio 1, the residence time is 15min to waste water in the reactor, and water outlet COD is 68mg/
L。
Step（3）In, it after sorbing material penetrates, is desorbed with 10% sodium hydroxide solution, solution intakes flow velocity as 1BV/h, solves
The suction time is 4h.Sodium hydroxide stripping liquid returns to extractant saponification process reuse.
Embodiment 2：
Certain cobalt manufacturing enterprise cobalt raffinate, main component are sodium sulphate, pH=4.6, COD 1800mg/L.
Step（1）：The above-mentioned waste water of 20L is taken, 0.5g/L demulsifiers are added, are stirred to react 40min；
Step（2）：Step（1）Water outlet enters air supporting Slag Scraping Device, and residence time 40min, water outlet COD are 500mg/L；
Step（3）：Step（2）Sulphur acid for adjusting pH=3 are added in water outlet, subsequently into oil removing adsorption column.Adsorption column water inlet flow velocity be
5BV/h, water outlet COD are 130mg/L.
Step（4）：Step（3）Water outlet is added sodium hydroxide and adjusts pH=7, subsequently into catalyst oxidation reactor.Dioxygen
Water：COD（Mass concentration is）It is 1, gas liquid ratio 1, the residence time is 16min to waste water in the reactor, and water outlet COD is 78mg/
L。
Step（3）In, it after sorbing material penetrates, is desorbed with 10% sodium hydroxide solution, solution intakes flow velocity as 2BV/h, solves
The suction time is 5h.Sodium hydroxide stripping liquid returns to extractant saponification process reuse.
Embodiment 3：
Certain cobalt manufacturing enterprise cobalt raffinate, main component are sodium sulphate, pH=6, COD 1800mg/L.
Step（1）：The above-mentioned waste water of 20L is taken, 1.5g/L demulsifiers are added, are stirred to react 50min；
Step（2）：Step（1）Water outlet enters air supporting Slag Scraping Device, and residence time 40min, water outlet COD are 500mg/L；
Step（3）：Step（2）Sulphur acid for adjusting pH=2 are added in water outlet, subsequently into oil removing adsorption column.Adsorption column water inlet flow velocity be
5BV/h, water outlet COD are 140mg/L.
Step（4）：Step（3）Water outlet is added sodium hydroxide and adjusts pH=7, subsequently into catalyst oxidation reactor.Dioxygen
Water：COD（Mass concentration is）It is 1, gas liquid ratio 1, the residence time is 18min to waste water in the reactor, and water outlet COD is 75mg/
L。
Step（3）In, it after sorbing material penetrates, is desorbed with 10% sodium hydroxide solution, solution intakes flow velocity as 2BV/h, solves
The suction time is 6h.Sodium hydroxide stripping liquid returns to extractant saponification process reuse.
Applicant states that the present invention illustrates the method detailed of the present invention, but the present invention not office by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, the selection etc. of concrete mode, all fall within protection scope of the present invention and the open scope.
Claims (10)
1. the processing method of deep removal COD in a kind of raffinate from nickel cobalt, which is characterized in that the waste water is first carried out coagulation
Demulsification is handled, and is converted after suspended oil oil emulsion to and is entered oil removal by air bubbling processing removing suspended oil, and water outlet is removed into adsorption deeply
Oil, reduce COD after further through catalytic ozonation advanced treating, final outflow water COD ＜ 80mg/L.
2. processing method as described in claim 1, which is characterized in that add demulsifier into the waste water, it is broken to carry out coagulation
Breast processing, converts oil emulsion to suspended oil；
The demulsifier dosage is 0.2 ~ 2g/L；
The coagulation demulsification time is 10 ~ 60min.
3. processing method as claimed in claim 2, which is characterized in that water outlet enters at oil removal by air bubbling after coagulation demulsification processing
Reason is 30 ~ 60min when stop；
Water outlet COD is 400 ~ 600mg/L after oil removal by air bubbling processing.
4. processing method as claimed in claim 3, which is characterized in that after water outlet pH is adjusted to 2 ~ 7 after handling oil removal by air bubbling, with
1 ~ 5BV/h flow velocitys enter adsorption deeply oil removal treatment, and absorption water outlet COD is 100 ~ 200m/L.
5. processing method as claimed in claim 4, which is characterized in that after absorption water outlet pH is adjusted to 7 ~ 9, into ozone catalytic
Oxidative system depth degradation COD, water outlet COD ＜ 80mg/L.
6. processing method as claimed in claim 5, which is characterized in that add hydrogen peroxide, dioxygen to catalytic ozonation system
Water：COD is 1 ~ 2；Reaction time is 15 ~ 60min；Gas liquid ratio is 1 ~ 5.
7. the processing method in a kind of 1-6 such as claim as described in any claim, which is characterized in that through adsorbing oil removal treatment
Sorbing material afterwards is desorbed by strippant, and the strippant is preferably sodium hydroxide solution, ethanol solution, methanol solution
Or one kind in acetone soln；
Preferably, the strippant be sodium hydroxide solution, a concentration of 10% ~ 20%.
8. processing method as claimed in claim 7, which is characterized in that the strippant flow velocity is 1 ~ 2BV/h, and desorption time is
4~6h。
9. processing method as claimed in claim 7, which is characterized in that when strippant is sodium hydroxide solution, stripping liquid returns
Return extractant saponification process reuse.
10. processing method as claimed in claim 7, which is characterized in that when strippant is ethanol solution, methanol solution or acetone
When a kind of in solution, it is more than 99.5% that stripping liquid, which goes to distillation system separation and recovery strippant and oil, the strippant rate of recovery,.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194545A (en) * | 2019-06-26 | 2019-09-03 | 浙江中金格派锂电产业股份有限公司 | Nickel, cobalt heavy metal are separated with magnesium, are enriched with and recovery process in a kind of waste water |
| CN111333216A (en) * | 2020-03-06 | 2020-06-26 | 北京中科康仑环境科技研究院有限公司 | Treatment and reuse process of methanol-to-olefin wastewater |
| CN111635051A (en) * | 2020-05-06 | 2020-09-08 | 陕西聚泰新材料科技有限公司 | Waste water treatment method in nickel-cobalt hydrometallurgy |
| CN111777082A (en) * | 2019-04-04 | 2020-10-16 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from raffinate of waste battery recovery liquid |
| CN113307438A (en) * | 2021-06-30 | 2021-08-27 | 赛恩斯环保股份有限公司 | Treatment method of nickel-cobalt smelting heavy metal wastewater |
| CN113387469A (en) * | 2021-05-31 | 2021-09-14 | 浙江中金格派锂电产业股份有限公司 | Method for treating cobalt-nickel raffinate |
| CN113830919A (en) * | 2021-09-18 | 2021-12-24 | 天津市茂联科技有限公司 | Oil removing method for high-salt oily sewage |
| CN113880292A (en) * | 2021-09-14 | 2022-01-04 | 天津市茂联科技有限公司 | Oil removing process for saponified water |
| CN116495864A (en) * | 2023-04-23 | 2023-07-28 | 中国轻工业广州工程有限公司 | Oil removal method for raffinate of ternary lithium battery material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111777082A (en) * | 2019-04-04 | 2020-10-16 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from raffinate of waste battery recovery liquid |
| CN111777082B (en) * | 2019-04-04 | 2021-11-23 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from raffinate of waste battery recovery liquid |
| CN110194545A (en) * | 2019-06-26 | 2019-09-03 | 浙江中金格派锂电产业股份有限公司 | Nickel, cobalt heavy metal are separated with magnesium, are enriched with and recovery process in a kind of waste water |
| CN110194545B (en) * | 2019-06-26 | 2021-04-27 | 浙江中金格派锂电产业股份有限公司 | Process for separating, enriching and recovering nickel, cobalt and heavy metal from magnesium in wastewater |
| CN111333216A (en) * | 2020-03-06 | 2020-06-26 | 北京中科康仑环境科技研究院有限公司 | Treatment and reuse process of methanol-to-olefin wastewater |
| CN111635051A (en) * | 2020-05-06 | 2020-09-08 | 陕西聚泰新材料科技有限公司 | Waste water treatment method in nickel-cobalt hydrometallurgy |
| CN113387469A (en) * | 2021-05-31 | 2021-09-14 | 浙江中金格派锂电产业股份有限公司 | Method for treating cobalt-nickel raffinate |
| CN113307438A (en) * | 2021-06-30 | 2021-08-27 | 赛恩斯环保股份有限公司 | Treatment method of nickel-cobalt smelting heavy metal wastewater |
| CN113880292A (en) * | 2021-09-14 | 2022-01-04 | 天津市茂联科技有限公司 | Oil removing process for saponified water |
| CN113830919A (en) * | 2021-09-18 | 2021-12-24 | 天津市茂联科技有限公司 | Oil removing method for high-salt oily sewage |
| CN116495864A (en) * | 2023-04-23 | 2023-07-28 | 中国轻工业广州工程有限公司 | Oil removal method for raffinate of ternary lithium battery material |
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