CN113387469A - Method for treating cobalt-nickel raffinate - Google Patents
Method for treating cobalt-nickel raffinate Download PDFInfo
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- CN113387469A CN113387469A CN202110599541.0A CN202110599541A CN113387469A CN 113387469 A CN113387469 A CN 113387469A CN 202110599541 A CN202110599541 A CN 202110599541A CN 113387469 A CN113387469 A CN 113387469A
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- 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
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention belongs to the field of metallurgical wastewater treatment, and relates to a method for treating cobalt-nickel-containing raffinate. The invention relates to a method for treating cobalt-nickel raffinate, which comprises the following steps: (1) air flotation oil removal; (2) coagulation sedimentation oil removal; (3) removing COD and P by activated carbon adsorption; (4) and (5) regenerating the activated carbon. Through the steps, COD in the cobalt-nickel raffinate is reduced to be below 100mg/L, P content is reduced to be below 3mg/L, and oil content is reduced to be below 20mg/L, so that the three items reach the wastewater discharge standard. Through the activated carbon regeneration technology, the activated carbon can be reused, the use amount of the activated carbon is reduced, the generation of solid waste after the activated carbon is adsorbed is reduced, and the harmonious development with the environment is facilitated.
Description
Technical Field
The invention belongs to the field of metallurgical wastewater treatment, and relates to a treatment method of cobalt-nickel raffinate.
Background
In the process of wet smelting of raw materials such as cobalt concentrate, cobalt intermediate products and the like, kerosene and a P507 extracting agent are usually used for extracting cobalt and nickel in an extraction stage, after the extraction of cobalt and nickel is finished, an organic phase and a water phase are usually separated, P507 raffinate is generated after the separation, the generated P507 raffinate usually contains organic components, the organic components are mainly sulfonated kerosene and the P507 extracting agent, the organic matter and phosphorus content in the raffinate exceeds the standard, and the direct discharge causes huge pollution to the environment.
Chinese patent CN201810408625.X discloses a treatment method for deeply removing COD from nickel cobalt raffinate, which comprises the steps of firstly carrying out coagulation demulsification treatment on the wastewater, converting emulsified oil into suspended oil, then carrying out air floatation oil removal treatment to remove the suspended oil, carrying out adsorption treatment on effluent to deeply remove the suspended oil, reducing the oil content, and then further carrying out ozone catalytic oxidation advanced treatment on the effluent to finally obtain the effluent COD (chemical oxygen demand) of less than 80 mg/L. The method can greatly reduce the oil content of the wastewater by deeply removing oil through resin adsorption, but the resin analysis and analysis agent recovery processes are complex, and the wastewater treatment cost is greatly increased.
Disclosure of Invention
Aiming at the problems, the invention provides a method for treating cobalt-nickel raffinate, which can effectively reduce phosphorus, oil and COD in the cobalt-nickel raffinate, so that the COD in wastewater is less than 100mg/L, P is less than 3mg/L, and the oil content is less than 20 mg/L.
The invention discloses a method for treating cobalt-nickel raffinate, which can be realized by the following technical scheme:
a method for treating cobalt-nickel raffinate comprises the following steps:
(1) air-float oil removing
Carrying out aeration treatment on cobalt-nickel (P204/P507) raffinate for 2-4 h, and fishing out the upper-layer suspended solid after the aeration is finished;
(2) coagulation sedimentation oil removal
Adjusting the pH value of the oil-removed air flotation solution obtained in the step (1) to 7-8, adding a coagulant for coagulation and sedimentation, and performing solid-liquid separation after the reaction is finished;
(3) COD and P are removed by activated carbon adsorption
Putting 1 liter of the filtrate obtained after solid-liquid separation in the step (2) into a beaker, adding activated carbon into the filtrate, and adsorbing by using the activated carbon to remove COD and P;
(4) regeneration of activated carbon
And (3) regenerating the activated carbon used in the step (3) by using a tubular furnace, wherein the regeneration conditions are as follows: and drying at the temperature of 150-200 ℃ in an inert gas atmosphere for 30-120 min, raising the temperature to 700-800 ℃ in the inert gas atmosphere after drying, keeping the temperature for 1-4 h, and reducing the temperature to room temperature after regeneration to obtain the regenerated activated carbon.
The aeration mode in the step (1) adopts a microporous aeration disc, and the aeration time is 4 hours.
The coagulant in the step (2) is one or a mixture of PAC, PFS and PAM.
The activated carbon in the step (3) is one or a mixture of powdered activated carbon and shell activated carbon.
And (3) stirring the filtrate, adding activated carbon, stirring at the stirring speed of 600r/min, and mixing the activated carbon with the cobalt-nickel raffinate to reduce COD in the cobalt-nickel raffinate.
The conditions for regenerating the activated carbon in the step (4) are as follows: drying in inert gas at 180 deg.C for 60min, heating to 750 deg.C in inert gas for 3h, and cooling to room temperature to obtain regenerated activated carbon.
And (4) the inert gas in the step (4) is nitrogen or argon.
Compared with the prior art, the process has the following beneficial effects:
(1) by the process, COD in the cobalt-nickel raffinate with P204/P507 as an extraction system can be reduced to be below 100 mg/L;
(2) the oil content in the cobalt-nickel raffinate taking P204/P507 as an extraction system can be reduced to below 20mg/L by the process;
(3) by the process, the phosphorus content in the cobalt-nickel raffinate taking P204/P507 as an extraction system can be reduced to be below 3 mg/L;
(4) the use efficiency of the activated carbon can be effectively increased through the regeneration of the activated carbon, the treatment cost of the cobalt-nickel raffinate can be reduced, and the process operation efficiency is improved;
(5) the method has the advantages of simple process flow, strong operability and very wide application prospect.
Drawings
FIG. 1 is a schematic diagram of a process for treating a cobalt-nickel raffinate according to the present invention;
FIG. 2 is a graph showing the effect of the amount of added activated carbon on the removal rate of COD and P in the present invention;
FIG. 3 is a graph showing the effect of air flotation time on oil content in cobalt-nickel raffinate.
Detailed Description
Example 1
The COD in the P507 cobalt nickel raffinate is 1425mg/L, P to be 21.04mg/L, and the oil content is 98.677 mg/L. 1000mL of P507 raffinate is put into a 3L beaker and is aerated for 3 hours, solid insoluble substances suspended on the liquid surface are fished out after aeration is finished, and the remaining solution becomes aerated liquid. And then adding PAC and PAM with certain concentration into the aerated liquid under the condition of mechanical stirring, adjusting the pH of the solution to be = 7-8, carrying out solid-liquid separation by suction filtration after reacting for 30min, and reserving the filtrate for later use to obtain the filtrate as the coagulated liquid. Stirring the remained filtrate at the stirring speed of 600r/min, adding 4g of powdered activated carbon into the filtrate, stirring for 1 hour, and performing solid-liquid separation by suction filtration to obtain filtrate which is the liquid after activated carbon adsorption. After the separation is finished, the activated carbon is regenerated, and the regeneration specific process comprises the following steps: firstly, drying in a nitrogen atmosphere at the temperature of 200 ℃ for 60min, raising the temperature to 800 ℃ in the nitrogen atmosphere after drying, keeping the temperature for 3h, reducing the temperature to room temperature after regeneration to obtain regenerated activated carbon, and subsequently removing COD and P from the regenerated activated carbon continuously;
the results of the sample analysis during the experiment were as follows:
| sample name | COD（mg/L） | P（mg/L） | Oil content (mg/L) |
| Liquid after aeration | 1082 | 16.92 | 44.532 |
| Liquid after coagulation | 966 | 16.33 | 22.276 |
| Activated carbon after-adsorption liquid | 197 | 3.52 | 19.44 |
According to the experimental analysis result, through aeration, coagulation and activated carbon adsorption, the COD content in the final solution is 197mg/L, the P content is 3.52mg/L, and the oil content is 19.44 mg/L.
Regenerating the activated carbon after removing COD and P, and treating the coagulated liquid by using the activated carbon with different regeneration times, wherein the treatment steps are as follows: taking 1L of the coagulated liquid, respectively adding 4g of powdered activated carbon with different regeneration times, stirring for 1 hour, and performing solid-liquid separation by suction filtration to obtain filtrate which becomes activated carbon adsorption liquid. After different regeneration times, the cobalt-nickel raffinate is treated by the method with the specific effects as follows:
| number of regeneration of activated carbon | Loss ratio of activated carbon (%) | Sample name | COD（mg/L） | P（mg/L） |
| 1 | 1.32 | Activated carbon after-adsorption liquid | 196 | 3.72 |
| 5 | 2.34 | Activated carbon after-adsorption liquid | 198 | 3.92 |
| 9 | 8.34 | Activated carbon after-adsorption liquid | 198 | 3.94 |
| 10 | 10.32 | Activated carbon after-adsorption liquid | 229 | 6.78 |
| 11 | 12.63 | Activated carbon after-adsorption liquid | 268 | 7.28 |
Experiments show that when the regeneration times of the activated carbon is 10, the COD of the regenerated activated carbon is 229mg/L, the P of the regenerated activated carbon is 6.78mg/L, and the oil content of the regenerated activated carbon is 30.12mg/L, so that the effect of the regenerated activated carbon on treating the cobalt-nickel raffinate is poor. In addition, after 10 regenerations, the loss rate of the activated carbon was 10.32%, and the loss was large.
Example 2
The COD in the P507 cobalt nickel raffinate is 1425mg/L, P to be 21.04mg/L, and the oil content is 98.677 mg/L. 1000mL of P507 raffinate is put into a 3L beaker and is aerated for 4 hours, solid insoluble substances suspended on the liquid surface are fished out after aeration is finished, and the remaining solution becomes aerated liquid. And then adding PAC and PAM with certain concentration into the aerated liquid under the condition of mechanical stirring, adjusting the pH of the solution to be = 7-8, carrying out solid-liquid separation by suction filtration after reacting for 30min, and reserving the filtrate for later use to obtain the filtrate as the coagulated liquid. Stirring the remained filtrate at the stirring speed of 600r/min, adding 5g of powdered activated carbon into the filtrate, stirring for 1 hour, and performing solid-liquid separation by suction filtration to obtain filtrate which is the liquid after activated carbon adsorption. After the separation is finished, the activated carbon is regenerated, and the regeneration specific process comprises the following steps: firstly, drying in a nitrogen atmosphere at the temperature of 180 ℃ for 60min, raising the temperature to 750 ℃ in the nitrogen atmosphere after drying, keeping the temperature for 3h, reducing the temperature to room temperature after regeneration to obtain regenerated activated carbon, and subsequently continuously removing COD and P from the regenerated activated carbon;
the results of the sample analysis during the experiment were as follows:
| sample name | COD（mg/L） | P（mg/L） | Oil content (mg/L) |
| Liquid after aeration | 982 | 16.80 | 34.532 |
| Liquid after coagulation | 876 | 16.28 | 20.399 |
| Activated carbon after-adsorption liquid | 97 | 2.52 | 19.24 |
According to the experimental analysis result, through aeration, coagulation and activated carbon adsorption, the COD content in the final solution is 97mg/L, the P content is 2.52mg/L, and the oil content is 19.24 mg/L.
Regenerating the activated carbon after removing COD and P, and treating the coagulated liquid by using the activated carbon with different regeneration times, wherein the treatment steps are as follows: taking 1L of the coagulated liquid, respectively adding 5g of powdered activated carbon with different regeneration times, stirring for 1 hour, and performing solid-liquid separation by suction filtration to obtain filtrate which becomes activated carbon adsorption liquid. After different regeneration times, the cobalt-nickel raffinate is treated by the method with the specific effects as follows:
| number of regeneration of activated carbon | Loss ratio of activated carbon (%) | Sample name | COD（mg/L） | P（mg/L） |
| 1 | 1.25 | Activated carbon after-adsorption liquid | 107 | 2.72 |
| 5 | 2.24 | Activated carbon after-adsorption liquid | 138 | 2.82 |
| 9 | 8.35 | Activated carbon after-adsorption liquid | 198 | 2.98 |
| 10 | 10.28 | Activated carbon after-adsorption liquid | 211 | 6.34 |
| 11 | 12.47 | Activated carbon after-adsorption liquid | 252 | 7.66 |
Experiments show that when the regeneration times of the activated carbon is 10, the COD of the regenerated activated carbon is 211mg/L, the P of the regenerated activated carbon is 6.34mg/L, and the oil content of the regenerated activated carbon is 29.14mg/L, so that the effect of the regenerated activated carbon on treating the cobalt-nickel raffinate is poor. In addition, after 10 regenerations, the loss rate of the activated carbon was 10.28%, and the loss was large.
Example 3
The COD in the P507 cobalt nickel raffinate is 1425mg/L, P to be 21.04mg/L, and the oil content is 98.677 mg/L. 1000mL of P507 raffinate is put into a 3L beaker and is aerated for 4 hours, solid insoluble substances suspended on the liquid surface are fished out after aeration is finished, and the remaining solution becomes aerated liquid. And then adding PAC and PAM with certain concentration into the aerated liquid under the condition of mechanical stirring, adjusting the pH of the solution to be = 7-8, carrying out solid-liquid separation by suction filtration after reacting for 30min, and reserving the filtrate for later use to obtain the filtrate as the coagulated liquid. Stirring the remained filtrate at the stirring speed of 600r/min, adding 6g of powdered activated carbon into the filtrate, stirring for 1 hour, and performing solid-liquid separation by suction filtration to obtain filtrate which is the liquid after activated carbon adsorption. After the separation is finished, the activated carbon is regenerated, and the regeneration specific process comprises the following steps: firstly, drying in a nitrogen atmosphere at the temperature of 180 ℃ for 60min, raising the temperature to 750 ℃ in the nitrogen atmosphere after drying, keeping the temperature for 3h, reducing the temperature to room temperature after regeneration to obtain regenerated activated carbon, and then continuously removing oil from the regenerated activated carbon;
the results of the sample analysis during the experiment were as follows:
| sample name | COD（mg/L） | P（mg/L） | Oil content (mg/L) |
| Liquid after aeration | 981 | 16.77 | 33.348 |
| Liquid after coagulation | 866 | 16.15 | 20.235 |
| Activated carbon after-adsorption liquid | 95 | 2.43 | 19.09 |
According to the experimental analysis result, through aeration, coagulation and activated carbon adsorption, the COD content in the final solution is 95mg/L, the P content is 2.43mg/L, and the oil content is 19.09 mg/L.
Regenerating the activated carbon after removing COD and P, and treating the coagulated liquid by using the activated carbon with different regeneration times, wherein the treatment steps are as follows: taking 1L of the coagulated liquid, adding 6g of powdered activated carbon with different regeneration times respectively, stirring for 1 hour, and performing solid-liquid separation by suction filtration to obtain filtrate which becomes activated carbon adsorption liquid. After different regeneration times, the cobalt-nickel raffinate is treated by the method with the specific effects as follows:
| number of regeneration of activated carbon | Loss ratio of activated carbon (%) | Sample name | COD（mg/L） | P（mg/L） |
| 1 | 1.27 | Activated carbon after-adsorption liquid | 112 | 2.68 |
| 5 | 2.26 | Activated carbon after-adsorption liquid | 128 | 2.73 |
| 9 | 8.77 | Activated carbon after-adsorption liquid | 188 | 2.93 |
| 10 | 10.37 | Activated carbon after-adsorption liquid | 209 | 6.34 |
| 20 | 12.66 | Activated carbon after-adsorption liquid | 223 | 7.11 |
Experiments show that when the regeneration frequency of the activated carbon is 10, the COD of the regenerated activated carbon is 209mg/L, the P is 6.34mg/L, and the oil content is 28.12mg/L by the adsorption of the regenerated activated carbon, and the effect of the regenerated activated carbon on treating the cobalt-nickel raffinate is poor. In addition, after 10 regenerations, the loss rate of the activated carbon was 10.37%, and the loss was large.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A method for treating cobalt-nickel raffinate is characterized by comprising the following steps:
(1) air-float oil removing
Carrying out aeration treatment on the cobalt-nickel raffinate for 2-4 h, and fishing out the upper-layer suspended solid after the aeration is finished;
(2) coagulation sedimentation oil removal
Adjusting the pH value of the oil-removed air flotation solution obtained in the step (1) to 7-8, adding a coagulant for coagulation and sedimentation, and performing solid-liquid separation after the reaction is finished;
(3) COD and P are removed by activated carbon adsorption
Putting 1 liter of the filtrate obtained after solid-liquid separation in the step (2) into a beaker, adding activated carbon into the filtrate, and adsorbing by using the activated carbon to remove COD and P;
(4) regeneration of activated carbon
And (3) regenerating the activated carbon used in the step (3) by using a tubular furnace, wherein the regeneration conditions are as follows: and drying at the temperature of 150-200 ℃ in an inert gas atmosphere for 30-120 min, raising the temperature to 700-800 ℃ in the inert gas atmosphere after drying, keeping the temperature for 1-4 h, and reducing the temperature to room temperature after regeneration to obtain the regenerated activated carbon.
2. The method of claim 1, wherein the cobalt-nickel raffinate is treated by: the aeration mode in the step (1) adopts a microporous aeration disc, and the aeration time is 4 hours.
3. The method of claim 1, wherein the cobalt-nickel raffinate is treated by: the coagulant in the step (2) is one or a mixture of PAC, PFS and PAM.
4. The method of claim 1, wherein the cobalt-nickel raffinate is treated by: the activated carbon in the step (3) is one or a mixture of powdered activated carbon and shell activated carbon.
5. The method of claim 1, wherein the cobalt-nickel raffinate is treated by: and (3) stirring the filtrate, adding activated carbon, stirring at the stirring speed of 600r/min, and mixing the activated carbon with the cobalt-nickel raffinate to reduce COD in the cobalt-nickel raffinate.
6. The method of claim 1, wherein the cobalt-nickel raffinate is treated by: the conditions for regenerating the activated carbon in the step (4) are as follows: drying in inert gas at 180 deg.C for 60min, heating to 750 deg.C in inert gas for 3h, and cooling to room temperature to obtain regenerated activated carbon.
7. The method of claim 1, wherein the cobalt-nickel raffinate is treated by: and (4) the inert gas in the step (4) is nitrogen or argon.
8. The method of claim 1, wherein the cobalt-nickel raffinate is treated by: the cobalt-nickel raffinate in the step (1) is P507 or P204 cobalt-nickel raffinate.
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Cited By (3)
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| CN114620859A (en) * | 2022-02-25 | 2022-06-14 | 中南大学 | Method for removing dissolved P507 in saponified P507 wastewater |
| CN115672274A (en) * | 2022-11-09 | 2023-02-03 | 浙江工业大学 | Hydrothermal oxidation activated carbon, preparation method thereof and application thereof in cobalt-nickel extraction waste liquor |
| CN117964178A (en) * | 2024-03-25 | 2024-05-03 | 矿冶科技集团有限公司 | Raffinate steam oil removal method |
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| CN117964178A (en) * | 2024-03-25 | 2024-05-03 | 矿冶科技集团有限公司 | Raffinate steam oil removal method |
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