CN112125449B - Method for treating brownification waste liquid - Google Patents
Method for treating brownification waste liquid Download PDFInfo
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- CN112125449B CN112125449B CN202011000520.4A CN202011000520A CN112125449B CN 112125449 B CN112125449 B CN 112125449B CN 202011000520 A CN202011000520 A CN 202011000520A CN 112125449 B CN112125449 B CN 112125449B
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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
- C02F1/46—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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a method for treating brownification waste liquid. The method for treating the browning waste liquid comprises the following steps: adding a catalyst into the brownification waste liquid to react with organic matters in the brownification liquid to generate insoluble substances, wherein the catalyst is a solution containing hypochlorite ions; separating and removing the insoluble substances to obtain brownification filtrate; and carrying out electrolysis operation on the brownification filtrate, and depositing at a cathode to obtain the metal copper. The technical scheme of the invention can solve the problems of high energy consumption and material cost and high safety risk of the processing method in the related technology.
Description
Technical Field
The invention relates to the technical field of waste liquid treatment, in particular to a method for treating brownification waste liquid.
Background
In the PCB industry, in order to prevent the copper surface of the inner layer of the circuit board from being oxidized and enhance the bonding force between plates in the pressing process, a browning liquid is needed to be adopted to brown the copper plate, and when copper ions in the browning liquid are accumulated to a certain concentration, the browning liquid is invalid, so that browning waste liquid is generated. The main components in the brown oxidation waste liquid comprise sulfuric acid, oxazole, pyrrole compounds, copper ions, hydrogen peroxide, polyethylene glycol and the like, the COD concentration is generally more than 20000mg/L, and the contained organic matters have stable properties and are difficult to degrade. When brown oxide waste liquid is treated, organic matters need to be removed firstly to electrolyze and recover metallic copper, and if the removal is not complete, the organic matters can form an insulating film or a hydrophobic film on the surface of a cathode, so that electrolysis is difficult to perform, or the organic matters and the copper are co-deposited, so that cathode electrodeposited copper is blackened and crisp.
In the related technology, the brown oxidation waste liquid treatment method is that the brown oxidation waste liquid is treated by Fenton oxidation (hydrogen peroxide and ferrous ions) at high temperature, namely the waste liquid is filtered, heated to 60-90 ℃, and fed in sequence according to 70-100kg of hydrogen peroxide and 50-80kg of iron powder (or ferrous salt) which are 50 percent of waste water per ton under the action of continuous stirring, and the metal copper is recycled through electrolysis after full reaction. The method needs heating and a large amount of chemical raw materials, and has extremely high energy consumption and material cost; and, the security risk is higher in the course of handling.
Disclosure of Invention
The invention mainly aims to provide a method for treating brown oxidation waste liquid, and aims to solve the problems of high energy consumption, high material cost and high safety risk of a treatment method in the related technology.
In order to realize the purpose, the invention provides a method for treating brownification waste liquid, which comprises the following steps:
adding a catalyst into the brownification waste liquid to react with organic matters in the brownification liquid to generate insoluble substances, wherein the catalyst is a solution containing hypochlorite ions;
separating and removing the insoluble substances to obtain brownification filtrate;
and carrying out electrolysis operation on the brownification filtrate, and depositing at a cathode to obtain the metal copper.
In one embodiment, the catalyst is bleach water having an available chlorine content in the range of 4% to 15%.
In one embodiment, the bleaching water is added in an amount ranging from 80kg to 110kg per ton of the spent browning liquor.
In one embodiment, the step of separating and removing the insolubles to obtain a browned filtrate comprises:
adding a coagulant and/or flocculant to the browned waste liquid to promote flocculation and sedimentation of solid insoluble matter;
and separating and removing the solid insoluble substances by adopting a filtering or settling operation to obtain brownification filtrate.
In one embodiment, the coagulant is calcium carbonate, and the addition amount of the coagulant in each ton of the brownification waste liquid is 5kg-20 kg;
and/or the addition amount of the flocculating agent in each ton of the brownification waste liquid ranges from 0.1kg to 0.5 kg.
In one embodiment, the step of separating and removing the insolubles to provide a browned filtrate comprises:
removing the liquid insoluble substances by adopting an air floatation method to obtain browned filtrate.
In one embodiment, the step of removing the liquid insolubles by air flotation to obtain browned filtrate comprises:
conveying the browned waste liquid containing the liquid insoluble substances into an air flotation tank by adopting a jet pump to form stable foam, and removing the stable foam by an air flotation method.
In one embodiment, the brownification filtrate is subjected to an electrolysis operation, and the step of obtaining the metal copper by cathode deposition comprises the following steps:
and adding an oxidant and a surfactant into the brownification filtrate, carrying out electrolysis operation, and depositing at a cathode to obtain the metal copper, wherein the oxidant is a substance containing chloride ions.
In one embodiment, the oxidant is sodium chloride, and the concentration of the sodium chloride ranges from 15g/L to 20 g/L; and/or the surfactant is sodium dodecyl sulfate, and the concentration range of the sodium dodecyl sulfate is 0.1g/L-0.5 g/L.
In an embodiment, before the step of adding a catalyst to the brownification waste liquid to react with the organic matters in the brownification liquid to generate insoluble matters, the method further comprises the following steps:
and filtering the browned waste liquid to remove solid impurities in the browned waste liquid.
According to the technical scheme, firstly, a catalyst is added into the brownification waste liquid, the catalyst is a solution containing hypochlorite ions and can react with organic matters in the brownification waste liquid to generate insoluble substances, then the insoluble substances are separated and removed by adopting a physical method to obtain brownification filtrate, and finally the brownification filtrate is subjected to electrolysis operation, so that metal copper with high purity can be deposited at a cathode. The operation can effectively remove organic matters in the brownification waste liquid, the treatment process can be carried out at normal temperature, heating and temperature rise are not needed, the addition amount of chemical raw materials is small, and the energy consumption and the material cost can be effectively reduced; meanwhile, the safety risk in the processing process is low.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The main components in the brown oxidation waste liquid comprise sulfuric acid, oxazole, pyrrole compounds, copper ions, hydrogen peroxide, polyethylene glycol and the like, the COD concentration is generally more than 20000mg/L, and the contained organic matters have stable properties and are difficult to degrade. When the brown oxide waste liquid is treated, organic matters need to be removed firstly to electrolyze and recover the metallic copper, and if the removal is not complete, the organic matters can form an insulating film or a hydrophobic film on the surface of a cathode to cause difficulty in electrolysis, or can be co-deposited with the copper to cause the electrodeposited copper on the cathode to be black and brittle.
The invention provides a treatment method of browning waste liquid, aiming at effectively removing organic matters and recovering metal copper in the browning waste liquid.
In an embodiment of the method for treating brown oxidation waste liquid of the present invention, the method comprises the following steps:
adding a catalyst into the brownification waste liquid to react with organic matters in the brownification liquid to generate insoluble substances, wherein the catalyst is a solution containing hypochlorite ions;
separating and removing the insoluble substances to obtain brownification filtrate;
and carrying out electrolysis operation on the brownification filtrate, and depositing at a cathode to obtain the metal copper.
Specifically, the brown oxidation waste liquid is introduced into a catalytic settling tank, continuously stirred, and added with a catalyst, wherein the catalyst is a solution containing hypochlorite ions, such as hypochlorite, and the hypochlorite ions have good oxidability and can react with organic matters such as azole and pyrrole compounds in the solution to form insoluble substances. The insoluble matter may be solid insoluble matter or liquid insoluble matter, and the organic matter in the browned waste liquid is reacted sufficiently for 4 hours or more after the catalyst is added to remove the organic matter sufficiently and efficiently. The formed insoluble matter forms a delamination phenomenon with the browned waste liquid, wherein the solid is not easy to settle at the bottom of the browned waste liquid, and the liquid insoluble matter such as foam floats on the surface of the browned waste liquid. And then, separating the insoluble substances from the brownification waste liquid by adopting a physical method, thus effectively removing the organic substances in the brownification waste liquid, obtaining brownification filtrate after separating and removing the insoluble substances, and effectively reducing the COD value of the brownification filtrate at the moment because most of the organic substances are removed. Finally, the brownification filtrate without insoluble substances is electrolyzed, and metal copper can be obtained by deposition at the cathode, thereby realizing the recycling of resources. The treatment process can be operated at normal temperature, heating and temperature rise are not needed, the addition amount of chemical raw materials is small, and the energy consumption and the material cost can be effectively reduced; meanwhile, the safety risk in the processing process is low.
Therefore, it can be understood that the technical scheme of the invention is that firstly, the catalyst is added into the browning waste liquid, the catalyst is a solution containing hypochlorite ions and can react with organic matters in the browning waste liquid to generate insoluble substances, then the insoluble substances are separated and removed by adopting a physical method to obtain browning filtrate, and finally the browning filtrate is electrolyzed to deposit metal copper with higher purity at a cathode. The operation can effectively remove organic matters in the brownification waste liquid, the treatment process can be carried out at normal temperature, heating and temperature rise are not needed, the addition amount of chemical raw materials is small, and the energy consumption and the material cost can be effectively reduced; meanwhile, the safety risk in the processing process is low.
In one embodiment of the invention, the catalyst is bleach water, and the bleach water has an available chlorine content in the range of 4% to 15%.
The bleaching water mainly contains sodium hypochlorite, has strong oxidizability, and can react with organic matters such as oxazole and pyrrole compounds in the bleaching water to form insoluble substances so as to be effectively removed. To fully develop the oxidizing properties of the bleaching water, the available chlorine content of the bleaching water is controlled in the range of 4% to 15%, e.g. the available chlorine content of the bleaching water is 4%, 6%, 10%, 12%, 14% or 15%.
It should be noted that the bleaching water can be a by-product of the electrolysis recovery system of the acidic etching solution, that is, the by-product bleaching water can be obtained by absorbing the tail gas generated in the copper extraction system of the acidic etching electrolysis with the alkali solution, so that local materials can be obtained, the full utilization of resources can be realized, the price is low, and the treatment cost of the brown oxidation waste liquid is effectively reduced.
In order to convert the organic substances in the browned waste liquid into insoluble substances more sufficiently and effectively, the amount of the bleaching water is controlled, and in alternative embodiments, the amount of the bleaching water added per ton of the browned waste liquid is in the range of 80kg to 110kg, such as 80kg, 90kg, 100kg or 110kg per ton of the browned waste liquid.
In one embodiment of the present invention, the step of separating and removing insoluble matter, including solid insoluble matter, to obtain browned filtrate comprises:
adding a coagulant and/or flocculant to the browned waste liquid to promote flocculation and sedimentation of solid insoluble matter;
and separating and removing the solid insoluble substances by adopting a filtering or settling operation to obtain brownification filtrate.
Specifically, a coagulant and a flocculant are added to promote the solid insoluble substances to flocculate and settle relatively quickly, and then the solid insoluble substances are effectively separated and removed by a filtering device or an old inclined plate settling tank, so that the brownification filtrate can be obtained. The physical method can effectively and fully remove the solid insoluble substances, and the treatment operation is simpler and the treatment cost is lower. It should be noted that coagulants and flocculants may be purchased directly from commercial sources and are not limited thereto and are within the scope of the present invention.
In one embodiment of the present invention, the coagulant is calcium carbonate, and the addition amount of the coagulant is 5kg to 20kg per ton of the brownification waste liquid.
The calcium carbonate is used as a coagulant and can react with sulfuric acid in the brownification waste liquid to generate calcium sulfate precipitate to promote the precipitation of the calcium sulfate precipitate so as to facilitate the subsequent filtering or precipitation separation operation.
In order to promote the solid insoluble substances to be settled more sufficiently and effectively, the addition amount of the coagulant is suitably controlled, and in alternative embodiments, the addition amount of the coagulant per ton of the browned waste liquid is in a range of 5kg to 20kg, such as 5kg, 10kg, 15kg or 20kg per ton of the browned waste liquid.
Similarly, the amount of flocculant added is controlled to be suitable for more sufficiently and effectively promoting flocculation of the solid insoluble matter, and in alternative embodiments, the amount of flocculant added per ton of the browned waste liquid is in the range of 0.1kg to 0.5kg, such as 0.1kg, 0.2kg, 0.3kg, 0.4kg or 0.5kg per ton of the browned waste liquid.
In one embodiment of the present invention, the step of separating and removing insolubles to obtain browned filtrate comprises:
removing the liquid insoluble substances by adopting an air floatation method to obtain browned filtrate.
The liquid insoluble substance is foam and floats on the surface of the brown oxide waste liquid, the liquid insoluble substance can be effectively removed by adopting an air floatation method, and the operation is simpler.
In an embodiment of the present invention, the step of removing the insoluble matter in the liquid by the air flotation method to obtain browned filtrate comprises:
conveying the browned waste liquid containing the liquid insoluble substances into an air flotation tank by adopting a jet pump to form stable foam, and removing the stable foam by an air flotation method.
When adopting jet pump to carry the brown oxide waste liquid that contains the insoluble substance of liquid, jet pump can sneak into the brown oxide waste liquid with the air, and air mixes the foam that forms comparatively temperature with the insoluble substance of liquid in the air supporting groove finally, directly adopts the air supporting method alright effectively get rid of stable foam, and the operation is comparatively simple effective.
In an embodiment of the present invention, the brownification filtrate is subjected to an electrolysis operation, and the step of obtaining metal copper by cathode deposition comprises:
and adding an oxidant and a surfactant into the brownification filtrate, carrying out electrolysis operation, and depositing at a cathode to obtain the metal copper, wherein the oxidant is a substance containing chloride ions.
When the brownification filtrate is electrolyzed, an oxidant is added, wherein the oxidant is a substance containing chloride ions, the chloride ions are discharged at the anode to generate chlorine gas, the chlorine gas has strong oxidizability, and residual organic matters in the brownification filtrate can be oxidized and removed at the anode, namely the residual organic matters can be effectively removed through anodic oxidation. The addition of the surfactant plays a role in wetting, reduces the surface tension of the solution, reduces the deposition of organic matters on the surface of the cathode, and further improves the quality of the metal copper on the surface of the cathode.
In an alternative embodiment, the oxidizing agent is sodium chloride, and the concentration of sodium chloride ranges from 15g/L to 20 g/L.
The oxidant is sodium chloride, so that the cost is low, the sodium chloride can generate chloride ions in the electrolyte, the chloride ions discharge at the anode to generate chlorine, and the chlorine has strong oxidizability and can oxidize and remove residual organic matters in the brownification filtrate at the anode. The concentration of the controller is controlled so that it is sufficiently functional when sodium chloride is added, and in alternative embodiments the concentration of sodium chloride is in the range of 15g/L to 20g/L, such as 15g/L, 16g/L, 17g/L, 18g/L, 19g/L or 20 g/L.
In alternative embodiments, the surfactant is sodium lauryl sulfate, which is present in a concentration range of 0.1g/L to 0.5 g/L.
The sodium dodecyl sulfate is a hydrophilic surface active agent, plays a good role in wetting, and can effectively reduce the deposition of organic matters on the surface of the cathode, thereby effectively improving the quality of the metal copper on the surface of the cathode. The concentration of sodium lauryl sulfate is chosen to be sufficient, and in alternative embodiments, the concentration of sodium lauryl sulfate ranges from 0.1g/L to 0.5g/L, such as 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, or 0.5 g/L.
Further, in an embodiment of the present invention, before the step of adding a catalyst to the browning waste liquid to react with the organic matter in the browning liquid to generate insoluble matter, the method further includes:
and filtering the browned waste liquid to remove solid impurities in the browned waste liquid.
The brownification waste liquid is firstly filtered, so that solid impurities in the brownification waste liquid are effectively removed, and the influence of the solid impurities on subsequent operation is avoided, so that the quality of the final product, namely the metal copper, is influenced.
After the final electrolysis of the brown oxidation waste liquid, the copper ion content in the waste water is lower than 2g/L, the COD concentration is lower than 1000mg/L, and the brown oxidation waste liquid can be discharged to a waste water station for comprehensive treatment.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (6)
1. A treatment method of brown oxidation waste liquid is characterized by comprising the following steps:
adding a catalyst into the browned waste liquid to react with organic matters in the browned waste liquid to generate insoluble substances, wherein the catalyst is a solution containing hypochlorite ions;
separating and removing the insoluble substances to obtain brownification filtrate;
carrying out electrolysis operation on the brownification filtrate, and depositing at a cathode to obtain metal copper;
the catalyst is bleaching water, and the effective chlorine content of the bleaching water is 4-15%;
the insoluble matter comprises solid insoluble matter, and the step of separating and removing the insoluble matter to obtain browned filtrate comprises the following steps:
adding a coagulant and a flocculant to the browned waste liquid to promote flocculation and sedimentation of solid insoluble substances;
separating and removing solid insoluble substances by adopting filtration or sedimentation operation to obtain brownification filtrate;
the coagulant is calcium carbonate, and the addition amount of the coagulant in each ton of the brownification waste liquid ranges from 5kg to 20 kg;
the addition amount of the flocculating agent in each ton of the browned waste liquid ranges from 0.1kg to 0.5 kg;
the insoluble matter also comprises liquid insoluble matter, and the step of separating and removing the insoluble matter to obtain browned filtrate comprises the following steps:
removing the liquid insoluble substances by adopting an air floatation method to obtain browned filtrate.
2. A method for treating spent browning liquor according to claim 1, wherein the amount of bleaching water added per ton of spent browning liquor is in the range of 80kg to 110 kg.
3. The method for treating brownification waste liquid according to claim 1, wherein the step of removing the liquid-insoluble substances by an air-float method to obtain brownification filtrate comprises:
conveying the browned waste liquid containing the liquid insoluble substances into an air flotation tank by adopting a jet pump to form stable foam, and removing the stable foam by an air flotation method.
4. A method for treating spent browning liquor according to any one of claims 1 to 3, wherein the step of subjecting the brownification filtrate to an electrolysis operation to obtain metallic copper by cathodic deposition comprises:
and adding an oxidant and a surfactant into the brownification filtrate, carrying out electrolysis operation, and depositing at a cathode to obtain the metal copper, wherein the oxidant is a substance containing chloride ions.
5. The method for treating brownification waste liquid as claimed in claim 4, wherein the oxidant is sodium chloride, and the concentration of the sodium chloride is in the range of 15g/L-20 g/L;
and/or the surfactant is sodium dodecyl sulfate, and the concentration range of the sodium dodecyl sulfate is 0.1g/L-0.5 g/L.
6. The method for treating a brownification waste liquid as claimed in any one of claims 1 to 3, wherein before the step of adding a catalyst to the brownification waste liquid to react with the organic matter in the brownification waste liquid to generate insoluble matter, the method further comprises:
and filtering the browned waste liquid to remove solid impurities in the browned waste liquid.
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| CN102560533B (en) * | 2010-12-28 | 2016-07-13 | 深圳市瑞世兴科技有限公司 | A kind of technique of electrolyzing copper from brown oxide waste liquid |
| CN102603102B (en) * | 2012-03-30 | 2014-01-08 | 湖南万容科技股份有限公司 | Processing method of browning liquid |
| JP2013244430A (en) * | 2012-05-24 | 2013-12-09 | Swing Corp | Method and apparatus for treating copper chloride-containing acidic waste liquid |
| CN103233244B (en) * | 2013-05-16 | 2015-08-05 | 广东工业大学 | A kind of method utilizing useless brown liquid to extract copper |
| CN104773794A (en) * | 2015-04-30 | 2015-07-15 | 湖南富莱明节能环保科技有限公司 | Composite additive for electrolysis |
| CN110093627A (en) * | 2019-04-22 | 2019-08-06 | 深圳市泓达环境科技有限公司 | A kind of method and device and additive recycling copper from brownification liquid |
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