CN113403134B - Copper wire drawing oil waste liquid treatment method - Google Patents
Copper wire drawing oil waste liquid treatment method Download PDFInfo
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- CN113403134B CN113403134B CN202110697598.4A CN202110697598A CN113403134B CN 113403134 B CN113403134 B CN 113403134B CN 202110697598 A CN202110697598 A CN 202110697598A CN 113403134 B CN113403134 B CN 113403134B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0025—Working-up used lubricants to recover useful products ; Cleaning by thermal processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0058—Working-up used lubricants to recover useful products ; Cleaning by filtration and centrifugation processes; apparatus therefor
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/04—Working-up used lubricants to recover useful products ; Cleaning aqueous emulsion based
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/20—Metal working
- C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
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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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Abstract
The invention discloses a method for treating copper wire drawing oil waste liquid, which comprises the following steps: mixing the copper wire drawing oil waste liquid and alkali for hydrothermal reaction, filtering a reaction product to obtain a precipitate and a filtrate, and washing and drying the precipitate to obtain cuprous oxide; the filtrate was centrifuged to give a separate organic and aqueous phase. The treatment method is simple, and the obtained cuprous oxide can be used as a catalyst to be applied to the field of photoelectricity after being recovered, so that the method has good economic benefit; after the organic phase and the water phase are separated, the organic phase can be recycled, and the concentration of copper ions in the water phase can reach the national allowable discharge standard, so that the environmental pollution is less.
Description
Technical Field
The invention belongs to the technical field of industrial waste liquid treatment, and particularly relates to a method for treating copper wire drawing oil waste liquid.
Background
Copper wires are widely applied to the electrical and electronic industry, and with the rapid development of related industries, the usage amount of copper wire drawing oil used as an auxiliary agent for a copper drawing process is gradually increased, and the waste liquid of the copper wire drawing oil contains a large amount of copper ions and organic matters which are complexed together, so that the copper wires are more difficult to treat.
At present, waste copper wire drawing oil is generally treated by heating, changing the pH value, adding an organic demulsifier and then carrying out membrane filtration and biological separation, and Chinese invention patent (application No. CN202010776252.9) discloses a method for harmlessly treating, recycling and reusing waste drawing oil.
Disclosure of Invention
In order to solve the problems in the prior art, the invention discloses a method for treating copper wire drawing oil waste liquid, which provides the following technical scheme:
a method for treating copper wire drawing oil waste liquid comprises the following steps:
mixing copper wire drawing oil waste liquid and alkali for hydrothermal reaction, filtering the reaction product to obtain precipitate and filtrate,
washing and drying the precipitate to obtain cuprous oxide;
the filtrate was centrifuged to obtain a layered organic and aqueous phase.
Further, the ratio of the volume of the copper wire drawing oil waste liquid to the amount of the alkaline substances is 1: 0.1-2.5, wherein the volume unit is L, and the amount unit of the substances is mol.
Further, the alkali is sodium hydroxide and/or potassium hydroxide.
Further, the temperature of the hydrothermal reaction is 100-200 ℃, and the time is 1-12 h.
Further, the washing liquid in the washing process is ethanol and water.
Further, the drying method is vacuum drying.
Furthermore, the temperature in the drying process is 30-60 ℃, and the time is 6-24 h.
Furthermore, the rotating speed of the centrifugal equipment in the centrifugal process is 1000 r/min-10000 r/min, and the centrifugal time is 1 min-30 min.
And further washing and drying the precipitate to obtain the ellipsoidal cuprous oxide.
Through the technical scheme, the invention has the beneficial effects that:
1. the treatment method of the invention is used for treating the copper wire drawing oil waste liquid to obtain products of ellipsoidal cuprous oxide and organic and aqueous phases which are layered with each other, and the ellipsoidal cuprous oxide can be used as a catalyst to be applied to the photoelectric field after being recovered; after the organic phase and the water phase are separated, the organic phase can be recycled, and the concentration of copper ions in the water phase can reach the national allowable discharge standard, so that the environmental pollution is less.
2. The treatment method is very simple, only cheap and easily-obtained alkali reagents are added, and the surfactant and the high-carbon-chain alcohol in the wiredrawing oil waste liquid participate in the reaction for preparing the ellipsoidal cuprous oxide in the treatment process, so that the reutilization is realized, and the method has good economic benefit.
Drawings
FIG. 1 is a FESEM photograph of ellipsoidal cuprous oxide obtained in example 1
FIG. 2 is an XRD pattern of ellipsoidal cuprous oxide obtained in example 1
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 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.
At copper line wire drawing in-process, can produce a large amount of discarded object, mainly include copper mud and copper wire drawing oil waste liquid, copper mud is the solid waste that the copper wire drawing in-process produced, mainly includes copper and greasy dirt, and copper line wire drawing oil waste liquid is the liquid waste that the copper wire drawing in-process produced, mainly includes a large amount of copper ions and organic matter. With the wide application of copper wires, the usage amount of copper wire drawing oil used as an auxiliary agent for a copper drawing process is gradually increased, so that the amount of the generated copper wire drawing oil waste liquid is gradually increased, the existing treatment method of the copper wire drawing oil waste liquid is complex and high in cost, and the treated waste liquid contains high copper ions, so that the copper wire drawing oil waste liquid cannot be utilized and cannot meet the discharge standard. The invention discloses a method for treating copper wire drawing oil waste liquid, which is considered from the aspects of reducing recovery cost, improving recovery value, reducing environmental pollution and the like, and comprises the following steps:
mixing the copper wire drawing oil waste liquid and alkali for hydrothermal reaction, filtering a reaction product to obtain a precipitate and a filtrate, and washing and drying the precipitate to obtain cuprous oxide; the filtrate was centrifuged to give a separate organic and aqueous phase.
The main components of the copper wire drawing oil are organic matters such as a surfactant and various functional additives, copper ions and the organic matters are complexed together in the copper wire drawing oil waste liquid formed after copper wire drawing, the copper ions and the organic matters are difficult to separate, and meanwhile, the organic matters also contain some high-carbon chain alcohols.
According to the invention, copper drawing oil waste liquid and alkali are mixed together for hydrothermal reaction, copper ions in the copper drawing oil waste liquid react with the alkali to generate copper hydroxide, and the copper hydroxide further generates copper oxide at high temperature; the high carbon chain alcohol in the copper wire drawing oil waste liquid can be oxidized into aldehyde during heating and then further oxidized into acid, and the acid formed by oxidizing the high carbon chain alcohol has weak reducibility and can reduce copper oxide into cuprous oxide.
Furthermore, due to the existence of the surfactant in the copper wire drawing oil waste liquid, the finally formed cuprous oxide is in an ellipsoid shape.
The cuprous oxide is a catalyst commonly used in the photoelectric field, and the ellipsoidal cuprous oxide prepared by the method can be recycled in the photoelectric field and has better economic benefit.
Meanwhile, the hydrothermal reaction can be used for demulsification, and the filtrate after demulsification can be separated into a water phase and an organic phase through centrifugation.
In one embodiment, the ratio of the volume of the copper wire drawing oil waste liquid to the amount of alkaline substances is 1: 0.1-2.5, wherein the volume unit is L, and the amount of the alkaline substances is mol.
In one embodiment, the base is sodium hydroxide and/or potassium hydroxide, which may be solid or solution, and is not limited herein.
In one embodiment, the temperature of the hydrothermal reaction is 100 ℃ to 200 ℃ and the time is 1h to 12 h.
In one embodiment, the wash solution in the washing process is ethanol and water.
In one embodiment, the drying method is vacuum drying.
In one embodiment, the temperature in the drying process is 30-60 ℃ and the time is 6-24 h.
In one embodiment, the rotation speed of the centrifugal device in the centrifugal process is 1000 r/min-10000 r/min, and the centrifugal time is 1 min-30 min.
Example 1
Adding 0.4g of sodium hydroxide into 100ml of copper wire drawing waste liquid, stirring to obtain mixed slurry, transferring the mixed slurry into a hydrothermal kettle, carrying out hydrothermal reaction at 100 ℃ for 12 hours to obtain a precipitate and a solution, filtering to obtain a solid and a filtrate, respectively washing the solid with ethanol and water, carrying out vacuum drying at 30 ℃ for 24 hours to obtain ellipsoidal cuprous oxide, carrying out centrifugal separation on the filtrate at a rotating speed of 3000r/min for 5 minutes to obtain an oil-water separation solution, wherein the concentration of copper ions in a water layer is 0.24 g/L.
Example 2
Adding 3.5g of sodium hydroxide into 70ml of copper wire drawing waste liquid, stirring to obtain mixed slurry, transferring the mixed slurry into a hydrothermal kettle, carrying out hydrothermal reaction for 6 hours at 150 ℃ to obtain a precipitate and a solution, filtering to obtain a solid and a filtrate, respectively washing the solid with ethanol and water, carrying out vacuum drying for 12 hours at 45 ℃ to obtain ellipsoidal cuprous oxide, carrying out centrifugal separation on the filtrate at the rotating speed of 1000r/min for 10 minutes to obtain an oil-water separation solution, wherein the concentration of copper ions in a water layer is 0.33 mg/L.
Example 3
Adding 7g of sodium hydroxide into 70ml of copper wire drawing waste liquid, stirring to obtain mixed slurry, transferring the mixed slurry into a hydrothermal kettle, carrying out hydrothermal reaction for 1h at 200 ℃ to obtain a precipitate and a solution, filtering to obtain a solid and a filtrate, washing the solid with ethanol and water respectively, carrying out vacuum drying for 6h at 60 ℃ to obtain ellipsoidal cuprous oxide, carrying out centrifugal separation on the filtrate at the rotating speed of 10000r/min for 20min to obtain an oil-water separation solution, wherein the concentration of copper ions in a water layer is 0.15 mg/L.
Example 4
Adding 0.5g of potassium hydroxide into 70ml of copper wire drawing waste liquid, stirring to obtain mixed slurry, transferring the mixed slurry into a hydrothermal kettle, carrying out hydrothermal reaction at 100 ℃ for 12 hours to obtain a precipitate and a solution, filtering to obtain a solid and a filtrate, respectively washing the solid with ethanol and water, carrying out vacuum drying at 30 ℃ for 24 hours to obtain ellipsoidal cuprous oxide, carrying out centrifugal separation on the filtrate at a rotating speed of 3000r/min for 1min to obtain an oil-water separation solution, wherein the concentration of copper ions in a water layer is 0.26 mg/L.
Example 5
Adding 5g of potassium hydroxide into 70ml of copper wire drawing waste liquid, stirring to obtain mixed slurry, transferring the mixed slurry into a hydrothermal kettle, carrying out hydrothermal reaction for 1h at 200 ℃ to obtain a precipitate and a solution, filtering to obtain a solid and a filtrate, washing the solid with ethanol and water respectively, carrying out vacuum drying for 12h at 45 ℃ to obtain ellipsoidal cuprous oxide, carrying out centrifugal separation on the filtrate at the rotating speed of 5000r/min for 30min to obtain an oil-water separation solution, wherein the concentration of copper ions in a water layer is 0.10 mg/L.
Example 6
Adding 7g of potassium hydroxide into 70ml of copper wire drawing waste liquid, stirring to obtain mixed slurry, transferring the mixed slurry into a hydrothermal kettle, carrying out hydrothermal reaction for 6 hours at 150 ℃ to obtain a precipitate and a solution, filtering to obtain a solid and a filtrate, washing the solid with ethanol and water respectively, carrying out vacuum drying for 6 hours at 60 ℃ to obtain ellipsoidal cuprous oxide, carrying out centrifugal separation on the filtrate at the rotating speed of 10000r/min for 15 minutes to obtain an oil-water separation solution, wherein the concentration of copper ions in a water layer is 0.31 mg/L.
It should be noted that the alkaline reagents such as sodium hydroxide and potassium hydroxide related to the present invention are all common reagents in the market, and can be superior pure, analytically pure, chemically pure, etc., and the purity grade is not particularly limited.
Fig. 1 and 2 are a FESEM (field emission scanning electron microscope) image and an XRD (X-ray diffraction) image of the ellipsoidal cuprous oxide obtained in example 1, and it can be seen from fig. 1 that the cuprous oxide particles are in an ellipsoidal form, and from fig. 2 that the dried product is only cuprous oxide without cupric oxide and copper impurities.
In conclusion, the treatment method is simple, the obtained product is the ellipsoidal cuprous oxide with good economic benefit, the organic matters and water in the waste liquid can be well layered, the recycling of the organic matters is realized, the concentration of copper ions in the water layer is low, and the emission standard is met.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still modify the technical solutions described in the foregoing embodiments, or may equally substitute some or all of the technical features; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (5)
1. A method for treating copper wire drawing oil waste liquid is characterized by comprising the following steps: the method comprises the following steps:
mixing copper wire drawing oil waste liquid and alkali for hydrothermal reaction, and filtering a reaction product to obtain a precipitate and a filtrate;
because copper ions in the copper wire drawing oil waste liquid react with alkali to generate copper oxide, high-carbon-chain alcohol in the copper wire drawing oil waste liquid is oxidized into aldehyde during heating and then further oxidized into acid, the acid formed by the oxidation of the high-carbon-chain alcohol has weak reducibility and reduces the copper oxide into cuprous oxide, and the cuprous oxide is in an ellipsoidal shape due to a surfactant in the copper wire drawing oil waste liquid, the precipitate is washed and dried to obtain ellipsoidal cuprous oxide;
centrifuging the filtrate to obtain a layered organic phase and a layered water phase;
wherein the ratio of the volume of the copper wire drawing oil waste liquid to the amount of the alkaline substances is 1: 0.1-2.5, wherein the volume unit is L, and the amount unit of the substances is mol;
the alkali is sodium hydroxide and/or potassium hydroxide;
the temperature of the hydrothermal reaction is 150-200 ℃, and the time is 1-12 h.
2. The method for treating the copper wire drawing oil waste liquid according to claim 1, characterized in that: the washing liquid in the washing process is ethanol and water.
3. The method for treating the copper wire drawing oil waste liquid according to claim 1, characterized in that: the drying method is vacuum drying.
4. The method for treating the copper wire drawing oil waste liquid according to claim 1, characterized in that: the temperature in the drying process is 30-60 ℃, and the time is 6-24 h.
5. The method for treating the copper wire drawing oil waste liquid according to claim 1, characterized in that: the rotating speed of the centrifugal equipment in the centrifugal process is 1000 r/min-10000 r/min, and the centrifugal time is 1 min-30 min.
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