CN111573942A - Method for recycling copper-nickel electroplating waste liquid - Google Patents
Method for recycling copper-nickel electroplating waste liquid Download PDFInfo
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- CN111573942A CN111573942A CN202010361291.2A CN202010361291A CN111573942A CN 111573942 A CN111573942 A CN 111573942A CN 202010361291 A CN202010361291 A CN 202010361291A CN 111573942 A CN111573942 A CN 111573942A
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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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
Abstract
The invention relates to the technical field of electroplating waste liquid treatment, in particular to a method for recycling copper-nickel electroplating waste liquid, which comprises the following steps: solid-liquid separation; neutralizing and filtering; adsorption and desorption; evaporating and concentrating; electrolytic treatment; evaporating for crystallization and recovering the moist heat, discharging the saturated moist heat discharged from the crystallization kettle into an interlayer of the semi-open heat exchanger, discharging the saturated moist heat from a condensed water overflow port of the semi-open heat exchanger, and collecting the overflow liquid for recycling. The heated air flows out from the bottom of the semi-open type heat exchanger and is blown into the crystallization kettle again by the fan, so that the air can be recycled. According to the method for recycling the copper-nickel electroplating waste liquid, through the arrangement of neutralization and filtration, the low-concentration metal nickel waste water can be well recycled; through the arrangement of electrolytic treatment, the quantity and the efficiency of metal recovery in the electroplating waste liquid can be effectively improved, and the recovered metal can be directly made into granular, even spherical and other electroplating anode supplementary materials with larger surface areas.
Description
Technical Field
The invention relates to the technical field of electroplating waste liquid treatment, in particular to a method for recycling copper-nickel electroplating waste liquid.
Background
Because electroplating universality is strong and application is wide, along with rapid development of industry, more and more electroplating wastewater is generated. The quality of the electroplating wastewater is complex, and the electroplating wastewater contains heavy metal ions such as chromium, copper, zinc, nickel and the like. The electroplating wastewater is toxic and harmful. Therefore, the electroplating wastewater must be properly treated and fully recycled, so as to reduce or even eliminate the adverse effect on the environment.
At present, the recovery products of single heavy metal chemical plating waste liquid are more, and the methods for recovering metals mainly comprise a chemical method, a neutralization precipitation method, an electrolysis method and a membrane separation method. Among them, the chemical precipitation method is a method in which a chemical agent is added to water to cause metal ions to form insoluble compounds from soluble compounds, followed by precipitation separation; the reverse osmosis is a membrane separation technique, which can separate the dissolved substances from water, and is a method for purifying waste water and enriching dissolved metals. In reverse osmosis, the wastewater is passed under mechanical pressure through a specific ion resin semipermeable membrane which allows only water molecules to pass through (or selectively passes through) and blocks the passage of dissolved metals and impurities, and can be recycled, while the blocked metal compounds can be directly recycled. However, these methods generally have disadvantages such as long time consumption, poor operability, and low adsorption efficiency. The method has high recovery rate of copper, but the recovery quantity, the recovery efficiency and the recovery rate of the electroplating waste liquid containing recoverable nickel and recoverable metal are low, so that the electroplating waste liquid cannot be recycled, and the waste of resources is caused.
Disclosure of Invention
The invention aims to solve the defect that nickel and metal in electroplating waste liquid cannot be effectively recycled in the prior art, and provides a method for recycling copper-nickel electroplating waste liquid.
In order to achieve the purpose, the invention adopts the following technical scheme:
a designed method for recycling copper-nickel electroplating waste liquid comprises the following steps:
s1), solid-liquid separation: conveying the electroplating waste liquid to a filtering device through a water pump for solid-liquid separation, then collecting separated solid particles, and then conveying the separated clear liquid to a treatment reaction tank A through the water pump;
s2), neutralization filtration:
a. adding a certain amount of sodium hydroxide solution into the treatment reaction tank A, stirring the mixed solution in the treatment reaction tank A by a stirring device to fully mix the mixed solution, adjusting the pH value of the mixed solution, and layering the mixed solution in the treatment reaction tank A after a certain period of time, wherein the supernatant of the upper layer is waste liquid I, and the precipitate of the lower layer is copper hydroxide;
b. firstly, separating out copper hydroxide precipitate in the treatment reaction tank A in the step a, conveying the waste liquid I into a treatment reaction tank B through a water pump, then adding a certain amount of a binding reagent of hydrogen peroxide and ferrous ions into the treatment reaction tank B so as to break a nickel complex, and then adjusting the pH value of liquid in the treatment reaction tank B until the liquid is neutral to obtain a waste liquid II;
c. then adding a certain amount of polymer PAM flocculant into the treatment reaction tank B, fully stirring the mixed solution in the treatment reaction tank B by a stirring device, layering the mixed solution after a certain time, and discharging the precipitate at the lower layer to obtain waste liquid III;
s3), adsorption and desorption: c, conveying the waste liquid III obtained in the step c into an activated carbon adsorption tank through a water pump, continuously adsorbing the water until the COD of the water in the activated carbon adsorption tank reaches 105-145mg/l, stopping adsorption, and discharging the residual wastewater in the adsorption tank after the adsorption is finished;
s4), evaporation concentration: conveying the wastewater obtained in the step S3) to a fractionating tower through a water pump, heating the wastewater by using hot humid air or recovered hot water in the fractionating tower, and conveying the concentrated wastewater to an evaporator to evaporate water when the wastewater is heated to a certain temperature until the wastewater is evaporated and concentrated to a saturated concentration;
s5), electrolytic treatment: carrying out electrolysis treatment on the saturated concentration solution obtained in the step S4), and obtaining an electrolysis waste liquid after the electrolysis is finished;
s6), evaporative crystallization: conveying the electrolytic waste liquid obtained in the step S5) to a crystallization kettle for crystallization treatment;
s7), recovering damp heat: saturated wet and hot air discharged from the crystallization kettle is discharged into an interlayer of the semi-open heat exchanger, the saturated wet and hot air heats cold ambient air outside the pipe, the temperature of the saturated wet and hot air is reduced, water vapor in the saturated wet and hot air is condensed into water and is discharged from a condensed water overflow port of the semi-open heat exchanger, overflow liquid is collected and can be recycled, and the cooled gas is emptied from the top of a pipe pass of the semi-open heat exchanger. The heated air flows out from the bottom of the semi-open type heat exchanger and is blown into the crystallization kettle again by the fan, so that the air can be recycled.
Preferably, in step S1), the filter device is provided with a diagonal flow device to accelerate solid-liquid separation of the waste liquid.
Preferably, in step S4), the heating temperature for heating the wastewater is 45 ℃ to 85 ℃, which can make full use of heat resources, and can avoid the emission of small amount of acid gas or organic substances without heating to too high temperature.
Preferably, in step S5), the specific steps of the electrolytic treatment are: a roller containing the electrolytic content is arranged, then the solution with the saturated concentration obtained in the step S4) is added into the roller, the electrolysis is started by electrifying, and the metal ions of the waste liquid with high metal concentration are electroplated on the granular or spherical cathode, thereby the metal is easy to recover and can be directly used as the soluble granular or spherical anode required by the electroplating bath. The stirring particles can uniformly stir the electrolytic inclusion in the roller when the roller is turned over, so as to accelerate and improve the electrolytic efficiency and facilitate the recovery of metal in the waste liquid.
Preferably, the electrolytic contents are granular metal or alloy balls as a cathode for electrolysis and non-metallic stirring particles as an anode for electrolysis.
Preferably, in step S6), the crystallization treatment specifically comprises: blowing hot air with the wind pressure of 1.5-4.5KPa and the temperature of 55-85 ℃ into a crystallization kettle, heating the saturated waste liquid to a certain temperature, volatilizing water in the waste liquid into the air to form saturated hot and humid air to be discharged, continuously concentrating the saturated waste liquid, when the saturated concentration is exceeded, beginning to crystallize metal salt, and then carrying out fractional crystallization and separation.
Preferably, the saturated waste liquid is heated to a temperature of 45-65 ℃ to facilitate the gradual crystallization and separation of various salts.
The method for recycling the copper-nickel electroplating waste liquid has the beneficial effects that: according to the method for recycling the copper-nickel electroplating waste liquid, firstly, through the arrangement of neutralization and filtration, the low-concentration metal nickel wastewater can be well recycled; secondly, through the arrangement of electrolytic treatment, the quantity and the efficiency of metal recovery in the electroplating waste liquid can be effectively improved, and the recovered metal can be directly made into granular, even spherical electroplating anode supplementary materials with larger surface areas; in addition, through the arrangement of crystallization treatment, different salts can be conveniently separated out through crystallization step by step.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
A method for recycling copper-nickel electroplating waste liquid comprises the following steps:
s1), solid-liquid separation: conveying the electroplating waste liquid to a filtering device through a water pump for solid-liquid separation, then collecting separated solid particles, and then conveying the separated clear liquid to a treatment reaction tank A through the water pump;
in step S1), the filter device is provided with a diagonal flow device to accelerate solid-liquid separation of the waste liquid.
S2), neutralization filtration:
a. adding a certain amount of sodium hydroxide solution into the treatment reaction tank A, stirring the mixed solution in the treatment reaction tank A by a stirring device to fully mix the mixed solution, adjusting the pH value of the mixed solution, and layering the mixed solution in the treatment reaction tank A after a certain period of time, wherein the supernatant of the upper layer is waste liquid I, and the precipitate of the lower layer is copper hydroxide;
b. firstly, separating out copper hydroxide precipitate in the treatment reaction tank A in the step a, conveying the waste liquid I into a treatment reaction tank B through a water pump, then adding a certain amount of a binding reagent of hydrogen peroxide and ferrous ions into the treatment reaction tank B so as to break a nickel complex, and then adjusting the pH value of liquid in the treatment reaction tank B until the liquid is neutral to obtain a waste liquid II;
c. then adding a certain amount of polymer PAM flocculant into the treatment reaction tank B, fully stirring the mixed solution in the treatment reaction tank B by a stirring device, layering the mixed solution after a certain time, and discharging the precipitate at the lower layer to obtain waste liquid III;
s3), adsorption and desorption: c, conveying the waste liquid III obtained in the step c into an activated carbon adsorption tank through a water pump, continuously adsorbing the water until the COD of the water in the activated carbon adsorption tank reaches 105-145mg/l, stopping adsorption, and discharging the residual wastewater in the adsorption tank after the adsorption is finished;
s4), evaporation concentration: conveying the wastewater obtained in the step S3) to a fractionating tower through a water pump, heating the wastewater by using hot humid air or recovered hot water in the fractionating tower, and conveying the concentrated wastewater to an evaporator to evaporate water when the wastewater is heated to a certain temperature until the wastewater is evaporated and concentrated to a saturated concentration;
in step S4), the heating temperature for heating the wastewater is 45-85 ℃, which can make full use of heat resources, and can avoid the emission of a small amount of acid gas or organic substances without heating to an excessive temperature.
S5), electrolytic treatment: carrying out electrolysis treatment on the saturated concentration solution obtained in the step S4), and obtaining an electrolysis waste liquid after the electrolysis is finished;
in step S5), the specific steps of the electrolytic treatment are: a roller containing electrolysis content is arranged, the electrolysis content is granular metal or alloy balls as a cathode of electrolysis and non-metal stirring particles as an anode of electrolysis, then the saturated concentration solution obtained in the step S4) is added into the roller, the roller is electrified to start the electrolysis, and metal ions of waste liquid with high metal concentration are electroplated on the granular or spherical cathode, thereby the metal is easy to recover and can be directly used as a soluble granular or spherical anode required by a plating bath. The stirring particles can uniformly stir the electrolytic inclusion in the roller when the roller is turned over, so as to accelerate and improve the electrolytic efficiency and facilitate the recovery of metal in the waste liquid.
S6), evaporative crystallization: conveying the electrolytic waste liquid obtained in the step S5) to a crystallization kettle for crystallization treatment;
in step S6), the specific steps of the crystallization process are: blowing hot air with the wind pressure of 1.5-4.5KPa and the temperature of 55-85 ℃ into a crystallization kettle, heating the saturated waste liquid to a certain temperature, volatilizing water in the waste liquid into the air to form saturated hot and humid air to be discharged, continuously concentrating the saturated waste liquid, when the saturated concentration is exceeded, beginning to crystallize metal salt, and then carrying out fractional crystallization and separation. The saturated waste liquid is heated to 45-65 ℃ so as to be crystallized and separated into various salts step by step.
S7), recovering damp heat: and (3) discharging saturated wet and hot air discharged from the crystallization kettle into an interlayer of the semi-open heat exchanger, heating cold ambient air outside the pipe by the saturated wet and hot air, reducing the temperature of the saturated wet and hot air, condensing water vapor in the saturated wet and hot air into water, discharging the water vapor from a condensed water overflow port of the semi-open heat exchanger, and collecting overflow liquid to recycle. And the cooled gas is exhausted from the top of the tube side of the semi-open heat exchanger. The heated air flows out from the bottom of the semi-open type heat exchanger and is blown into the crystallization kettle again by the fan, so that the air can be recycled.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The method for recycling the copper-nickel electroplating waste liquid is characterized by comprising the following steps:
s1), solid-liquid separation: conveying the electroplating waste liquid to a filtering device through a water pump for solid-liquid separation, then collecting separated solid particles, and then conveying the separated clear liquid to a treatment reaction tank A through the water pump;
s2), neutralization filtration:
a. adding a certain amount of sodium hydroxide solution into the treatment reaction tank A, stirring the mixed solution in the treatment reaction tank A by a stirring device to fully mix the mixed solution, adjusting the pH value of the mixed solution, and layering the mixed solution in the treatment reaction tank A after a certain period of time, wherein the supernatant of the upper layer is waste liquid I, and the precipitate of the lower layer is copper hydroxide;
b. firstly, separating out copper hydroxide precipitate in the treatment reaction tank A in the step a, conveying the waste liquid I into a treatment reaction tank B through a water pump, then adding a certain amount of a binding reagent of hydrogen peroxide and ferrous ions into the treatment reaction tank B so as to break a nickel complex, and then adjusting the pH value of liquid in the treatment reaction tank B until the liquid is neutral to obtain a waste liquid II;
c. then adding a certain amount of polymer PAM flocculant into the treatment reaction tank B, fully stirring the mixed solution in the treatment reaction tank B by a stirring device, layering the mixed solution after a certain time, and discharging the precipitate at the lower layer to obtain waste liquid III;
s3), adsorption and desorption: c, conveying the waste liquid III obtained in the step c into an activated carbon adsorption tank through a water pump, continuously adsorbing the water until the COD of the water in the activated carbon adsorption tank reaches 105-145mg/l, stopping adsorption, and discharging the residual wastewater in the adsorption tank after the adsorption is finished;
s4), evaporation concentration: conveying the wastewater obtained in the step S3) to a fractionating tower through a water pump, heating the wastewater by using hot humid air or recovered hot water in the fractionating tower, and conveying the concentrated wastewater to an evaporator to evaporate water when the wastewater is heated to a certain temperature until the wastewater is evaporated and concentrated to a saturated concentration;
s5), electrolytic treatment: carrying out electrolysis treatment on the saturated concentration solution obtained in the step S4), and obtaining an electrolysis waste liquid after the electrolysis is finished;
s6), evaporative crystallization: conveying the electrolytic waste liquid obtained in the step S5) to a crystallization kettle for crystallization treatment;
s7), recovering damp heat: saturated wet and hot air discharged from the crystallization kettle is discharged into an interlayer of the semi-open heat exchanger, the saturated wet and hot air heats cold ambient air outside the pipe, the temperature of the saturated wet and hot air is reduced, water vapor in the saturated wet and hot air is condensed into water and is discharged from a condensed water overflow port of the semi-open heat exchanger, overflow liquid is collected and can be recycled, and the cooled gas is emptied from the top of a pipe pass of the semi-open heat exchanger. The heated air flows out from the bottom of the semi-open type heat exchanger and is blown into the crystallization kettle again by the fan, so that the air can be recycled.
2. The method as claimed in claim 1, wherein in step S1), the filter device is provided with a diagonal flow device to accelerate the solid-liquid separation of the waste liquid.
3. The method for recycling copper-nickel electroplating waste liquid according to claim 1, wherein in step S4), the waste water is heated at a temperature of 45-85 ℃, so that heat resources can be fully utilized, excessive heating is avoided, and a small amount of acid gas or organic substances can be prevented from being released.
4. The method for recycling the copper-nickel electroplating waste liquid according to claim 1, wherein in the step S5), the specific steps of the electrolytic treatment are as follows: a roller containing the electrolytic content is arranged, then the solution with the saturated concentration obtained in the step S4) is added into the roller, the electrolysis is started by electrifying, and the metal ions of the waste liquid with high metal concentration are electroplated on the granular or spherical cathode, thereby the metal is easy to recover and can be directly used as the soluble granular or spherical anode required by the electroplating bath. The stirring particles can uniformly stir the electrolytic inclusion in the roller when the roller is turned over, so as to accelerate and improve the electrolytic efficiency and facilitate the recovery of metal in the waste liquid.
5. The method for recycling copper-nickel electroplating waste liquid according to claim 4, wherein the electrolysis content comprises granular metal or alloy balls as a cathode of electrolysis and non-metal stirring particles as an anode of electrolysis.
6. The method for recycling the copper-nickel electroplating waste liquid according to claim 1, wherein in the step S6), the crystallization treatment comprises the following specific steps: blowing hot air with the wind pressure of 1.5-4.5KPa and the temperature of 55-85 ℃ into a crystallization kettle, heating the saturated waste liquid to a certain temperature, volatilizing water in the waste liquid into the air to form saturated hot and humid air to be discharged, continuously concentrating the saturated waste liquid, when the saturated concentration is exceeded, beginning to crystallize metal salt, and then carrying out fractional crystallization and separation.
7. The method for recycling the copper-nickel electroplating waste liquid according to claim 6, wherein the saturated waste liquid is heated to 45-65 ℃ so as to separate various salts by gradual crystallization.
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Cited By (3)
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| CN112875960A (en) * | 2021-01-25 | 2021-06-01 | 吕梁学院 | Industrial waste water heavy metal extraction element |
| CN112939165A (en) * | 2021-01-27 | 2021-06-11 | 厦门澄志精密科技有限公司 | Purification device for metal heat treatment wastewater |
| TWI756118B (en) * | 2021-04-26 | 2022-02-21 | 玉蓮企業股份有限公司 | Electroplating waste liquid recycling system and recycling method |
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Application publication date: 20200825 |