CN214681698U - Preparation device of copper oxide powder - Google Patents
Preparation device of copper oxide powder Download PDFInfo
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- CN214681698U CN214681698U CN202023351683.5U CN202023351683U CN214681698U CN 214681698 U CN214681698 U CN 214681698U CN 202023351683 U CN202023351683 U CN 202023351683U CN 214681698 U CN214681698 U CN 214681698U
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Abstract
The application relates to a waste liquid recovery technical field provides a preparation facilities of copper oxide powder, and this preparation facilities includes: the first reaction barrel is used for carrying out first mixing treatment on the acidic etching waste liquid containing cuprous ions and an oxidant so as to oxidize the cuprous ions into copper ions and form a first mixed solution; the second reaction barrel is communicated with the first reaction barrel, is provided with a pH probe and a temperature control element and is used for carrying out second mixing treatment on the first mixed solution and the alkaline solution under the conditions that the pH is more than or equal to 8 and the temperature is more than 50 ℃ so as to form copper oxide; the collecting barrel is used for collecting the suspension liquid with the copper oxide powder dispersed in the second reaction barrel; and the solid-liquid separation element is communicated with the collecting barrel and is used for separating the copper oxide powder in the suspension. The device simple structure, degree of automation is high, is favorable to simplifying technology, reduce cost, moreover, does not produce toxic gas, and no waste water waste liquid produces, and the environment is friendly.
Description
Technical Field
The application belongs to the technical field of waste liquid recovery, especially relates to a preparation facilities of copper oxide powder.
Background
With the rapid development of the electronic industry, the yield of printed circuit boards is increased year by year, and in the etching process for manufacturing the printed circuit boards, a large amount of acidic waste etching solution is required, and is formed after the etching solution is used, and the acidic waste etching solution often contains a large amount of copper in an ion form. Various methods have been attempted to effectively recycle copper contained in acidic etching waste liquid. At present, the method mainly comprises a neutralization method and an electrolysis method, wherein the neutralization method is to add alkali into the acid etching waste liquid for neutralization so as to precipitate copper in the form of hydroxide, the copper is changed into copper sludge after filter pressing and sent to a smelting plant for smelting into elemental copper, the method not only wastes a large amount of alkali, but also generates a large amount of waste water, and the value of the copper sludge after filter pressing is low. The electrolysis method can produce valuable electrolytic copper, but because an electrolysis additive needs to be added in the electrolysis process, the residual additive can influence the recycling effect of subsequent regenerated liquid, and meanwhile, the electrolysis method has high energy consumption and complex operation and even can produce toxic chlorine.
Disclosure of Invention
The application aims to provide a preparation device of copper oxide powder, and aims to solve the problem that the existing method cannot effectively recover and treat copper in acidic etching waste liquid.
In order to solve the technical problem, the technical scheme adopted by the application is as follows:
a preparation device of copper oxide powder comprises the following steps:
the first reaction barrel is used for carrying out first mixing treatment on the acidic etching waste liquid containing cuprous ions and an oxidant so as to oxidize the cuprous ions into copper ions and form a first mixed solution;
the second reaction barrel is communicated with the first reaction barrel, is provided with a pH probe and a temperature control element and is used for carrying out second mixing treatment on the first mixed solution and the alkaline solution under the conditions that the pH is more than or equal to 8 and the temperature is more than 50 ℃ so as to form copper oxide;
the collecting barrel is used for collecting the suspension liquid with the copper oxide powder dispersed in the second reaction barrel;
and the solid-liquid separation element is communicated with the collecting barrel and is used for separating the copper oxide powder in the suspension.
The application provides a preparation facilities of copper oxide powder, including first reaction vessel, second reaction vessel, collecting vessel and solid-liquid separation component, the first reaction vessel of second reaction vessel intercommunication, in first reaction vessel acid etching waste liquid and oxidant mix so that the cuprous ion in the acid etching waste liquid is by oxidant oxidation for copper ion, flow first mixed solution into the second reaction vessel from first reaction vessel and mix with alkaline solution under the condition that pH is no less than 8, the temperature > 50 ℃ for copper ion in the first mixed solution reacts with hydroxyl ion and oxidant and makes copper oxide powder, and the acid composition who derives from in the acid etching waste liquid is neutralized, later collect the suspension that disperses copper oxide powder and separate the copper oxide powder in the suspension through solid-liquid separation component through the collecting vessel, the device simple structure, degree of automation is high, the method is beneficial to simplifying the process and reducing the cost, does not generate toxic gas, does not generate waste water and waste liquid, and is environment-friendly. The copper oxide powder prepared by the preparation device has high purity and small particle size, has higher commercial value, and realizes the purpose of changing acidic etching waste liquid into valuable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural view of an apparatus for preparing copper oxide powder according to an embodiment of the present disclosure;
FIG. 2 is an SEM image of the copper oxide powder prepared in example 1;
FIG. 3 is a particle size distribution of the copper oxide powder prepared in example 1;
FIG. 4 is an XRD pattern of the copper oxide powder prepared in example 1;
FIG. 5 is an XPS plot of the copper oxide powder prepared in example 1.
1-a first reaction barrel, 11-a flow pump, 12-a first stirring element, 13-a third pipeline, 2-a second reaction barrel, 21-a temperature control element, 22-a second stirring element, 23-a pH probe, 24-an overflow port, 3-a collection barrel, 4-a solid-liquid separation element, 5-an acidic etching waste liquid feeding port, 51-a filtering element, 52-a first pipeline, 6-an oxidant feeding port, 62-a second pipeline, 31-a switch valve and 32-a fourth pipeline.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
In the present specification, the terms "first", "second", "third" and "fourth" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another, and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated, and the features defined as "first", "second", "third" and "fourth" may explicitly or implicitly include one or more such features.
The embodiment of the present application provides a preparation apparatus of copper oxide powder, as shown in fig. 1, the preparation apparatus includes:
the first reaction barrel 1 is used for carrying out first mixing treatment on the acidic etching waste liquid containing cuprous ions and an oxidant so as to oxidize the cuprous ions into copper ions and form a first mixed solution;
the second reaction barrel 2 is communicated with the first reaction barrel 1, is provided with a pH probe 23 and a temperature control element 21, and is used for carrying out second mixing treatment on the first mixed solution and the alkaline solution under the conditions that the pH is more than or equal to 8 and the temperature is more than 50 ℃ to form copper oxide;
a collecting barrel 3 for collecting the suspension from the second reaction barrel 2 in which the copper oxide powder is dispersed;
and the solid-liquid separation element 4 is communicated with the collecting barrel 3 and is used for separating the copper oxide powder in the suspension.
The device for preparing the copper oxide powder comprises a first reaction barrel, a second reaction barrel, a collecting barrel and a solid-liquid separation element, wherein the second reaction barrel is communicated with the first reaction barrel, the acidic etching waste liquid and an oxidant are mixed in the first reaction barrel, so that cuprous ions in the acidic etching waste liquid are oxidized into copper ions by the oxidant, a first mixed solution flows into the second reaction barrel from the first reaction barrel and is mixed with an alkaline solution under the conditions that the pH value is more than or equal to 8 and the temperature is more than 50 ℃, so that the copper ions in the first mixed solution react with hydroxide ions and the oxidant to prepare the copper oxide powder, acid components in the acidic etching waste liquid are neutralized, then, a suspension dispersed with the copper oxide powder is collected by the collecting barrel, and the copper oxide powder in the suspension is separated by the solid-liquid separation element, the device is simple in structure and high in automation degree, the method is beneficial to simplifying the process and reducing the cost, does not generate toxic gas, does not generate waste water and waste liquid, and is environment-friendly. The copper oxide powder prepared by the preparation device has high purity and small particle size, has higher commercial value, and realizes the purpose of changing acidic etching waste liquid into valuable.
On the basis of the above embodiment, the above preparation apparatus further includes: the acidic etching waste liquid feeding port 5 and the oxidant feeding port 6 are respectively communicated with the acidic etching waste liquid feeding port 5 and the oxidant feeding port 6 through a first pipeline 52 and a second pipeline 62, and the first pipeline 52 and the second pipeline 62 are respectively provided with a filter element 51 for filtering impurities. Therefore, impurities in the acidic waste etching solution and the oxidant are prevented from being doped into the subsequently formed copper oxide powder, and the purity of the copper oxide powder is ensured.
On the basis of the above embodiment, the second reaction barrel 2 is communicated with the first reaction barrel 1 through the third pipeline 13, and one end of the third pipeline 13 is open and communicated with the bottom of the second reaction barrel 2. Specifically, the third pipeline 13 is provided with two end openings along the solution flowing direction, wherein one end opening is communicated with the bottom of the second reaction barrel 2, and the other end opening is communicated with the first reaction barrel 1, so that the first mixed solution in the first reaction barrel 1 can enter the second reaction barrel 2 from the bottom of the second reaction barrel 2 through the third pipeline 13 to be mixed with the alkaline solution, thereby promoting the first mixed solution to be fully and uniformly mixed with the alkaline solution, and enabling the copper ions in the added first mixed solution to be reacted with the hydroxide ions and the oxidant provided by the alkaline solution immediately, which is favorable for synthesizing the copper oxide powder with small particle size. Meanwhile, the first mixed solution is added from the bottom of the second reaction barrel 2, so that the pH value in the system is kept above 8 all the time, and the purity of the copper oxide powder is ensured. In a further embodiment, a flow pump 11 is disposed on the third pipeline 13 for controlling the flow rate of the first mixed solution into the second reaction barrel 2, so as to further regulate and control the synthesis efficiency of the copper oxide powder.
On the basis of the above embodiment, the first reaction barrel 1 is provided with the first stirring element 12 to promote the acidic waste etching solution to be sufficiently and uniformly mixed with the oxidant, so that the cuprous ions in the acidic waste etching solution are sufficiently oxidized into copper ions. On the basis of the above embodiment, the second reaction barrel 2 is provided with the second stirring element 22 to promote the first mixed solution and the alkaline solution to be fully and uniformly mixed, which is beneficial to improving the yield of the copper oxide to a certain extent.
On the basis of the above embodiment, the second reaction barrel 2 is provided with the overflow port 24 at 1/3-2/3 of the barrel height thereof, and the barrel port of the collecting barrel 3 is located right below the overflow port 24. Because the copper oxide powder synthesized in the second reaction barrel is suspended above the solution, and the overflow port 24 is arranged at the position 1/3-2/3 which is 2 barrels high in the second reaction barrel, the copper oxide powder synthesized by reaction can overflow into the collecting barrel 3 through the overflow port in time, and the production efficiency of the copper oxide powder is improved to a certain extent.
On the basis of the above embodiment, the collecting tub 3 communicates with the solid-liquid separation element 4 through the fourth pipe 32, and the fourth pipe 32 is provided with the on-off valve 31. Separating the copper oxide powder from the solution in the suspension by solid-liquid separation; the copper oxide powder in the suspension is separated and collected regularly and quantitatively by arranging a switch valve 31 on the fourth pipeline 32.
On the basis of the above-described embodiment, the solid-liquid separation element 4 is a filter press, a centrifuge, or a natural settler.
Based on the technical scheme, the embodiment of the application provides a preparation method of copper oxide powder, which comprises the following specific implementation steps:
s01, pumping the acidic etching waste liquid into the first reaction barrel 1 through the first pipeline 52, starting the first stirring element 12 when the acidic etching waste liquid reaches the designated position of the first reaction barrel 1, adding an oxidant into the first reaction barrel 1 from the oxidant feeding port 6 through the second pipeline 62 under a stirring state, uniformly stirring to obtain a first mixed solution, and standing for later use;
s02, adding the alkaline solution into the second reaction barrel 2 until the alkaline solution reaches 1/3-2/3 of the barrel height, and adjusting the temperature of the second reaction barrel 2 to be more than 50 ℃ by using the temperature control element 21; then, the flow pump 11 is adjusted, the first mixed solution is slowly added into the second reaction barrel 2 from the bottom of the second reaction barrel 2 through the third pipeline 13, and the second stirring element 22 is opened to stir uniformly; when the pH probe 23 senses that the pH of the solution in the second reaction barrel 2 is less than 8, the flow pump 11 is closed, the first mixed solution is stopped from being added, then the alkaline solution is added, so that the pH is more than or equal to 8, and the flow pump 11 is restarted;
due to the addition of the alkaline solution and the volume expansion of the liquid in the barrel caused by the copper oxide synthesis reaction, the reacted copper oxide powder in the second reaction barrel 2 is suspended on the liquid level, and when the liquid level rises to the position of the overflow port 24, the suspension liquid in which the copper oxide powder is suspended overflows from the overflow port 24 and flows into the collection barrel 3;
s03, the on-off valve 31 on the fourth pipe 32 is opened, so that the suspension in the collecting tank 3 flows into the solid-liquid separation element 4 through the fourth pipe 32 to perform the operation of separating the copper oxide powder.
In some embodiments, the acidic waste etching solution is a printed circuit board acidic waste etching solution. The printed circuit board acid etching waste liquid is waste liquid formed after the printed circuit board is etched by the acid etching liquid, and the waste liquid contains a large amount of copper in an ion form, including copper ions and cuprous ions. The copper oxide powder is prepared by using the acidic etching waste liquid of the printed circuit board as a raw material, so that the acidic etching waste liquid is changed into valuable, and the waste of copper resources is reduced.
In some embodiments, the oxidizing agent comprises at least one of hydrogen peroxide, oxygen, ozone, sodium chlorate, and sodium hypochlorite. The oxidizing agent is a substance which has an oxidizing effect and can oxidize cuprous ions into copper ions, and the oxidizing agent is selected to ensure that the cuprous ions in the acidic etching waste liquid can be completely oxidized into the copper ions and promote the dehydration of copper hydroxide formed in the subsequent process to generate copper oxide. In a further embodiment, the oxidizing agent is hydrogen peroxide, the oxidizing agent has good oxidizing activity, and the reaction product is water, so that other substances are not introduced, and the synthesis of the high-purity copper oxide powder is facilitated.
In some embodiments, the weight of the oxidizing agent is 0.5% -20% of the total weight of the acidic spent etching solution and the oxidizing agent. By controlling the dosage of the oxidant within the range, cuprous ions in the acidic etching solution can be completely oxidized into copper ions, the copper ions are promoted to form copper oxide to the maximum extent, the resource waste caused by excessive oxidant is avoided, and the process cost is saved. In one embodiment, the oxidizing agent is hydrogen peroxide, the acidic waste etching solution is a printed circuit board acidic waste etching solution, and the weight of the oxidizing agent is 4% of the total weight of the acidic waste etching solution and the oxidizing agent, so that the efficiency of synthesizing the copper oxide powder is optimized.
In some embodiments, the oxidizing agent is added to the first reaction tank 1 through the second pipe 62 from the oxidizing agent feeding port 6, and stirred at normal temperature for 10 to 180 minutes. Specifically, the normal temperature includes 20 ℃ to 35 ℃. By controlling the temperature and time of the first mixing treatment within the above ranges, the cuprous ions in the acidic etching waste liquid can be promoted to be sufficiently oxidized into copper ions.
In some embodiments, the temperature control element 21 is used to regulate the temperature of the second reaction barrel 2 to be greater than 50 ℃ and less than or equal to 100 ℃. The higher the temperature is, the higher the yield of the copper oxide is, but the increase of the temperature also brings about the increase of energy consumption, and when the reaction temperature is controlled to be 50-100 ℃, the reaction energy consumption can be controlled within a lower range while the yield of the copper oxide is ensured.
In some embodiments, when the pH probe 23 senses that the pH of the solution in the second reaction tank 2 is less than 8, the flow pump 11 is turned off to stop adding the first mixed solution, and then the flow pump 11 is restarted after the alkaline solution is added to make the pH of the solution be 8-12.
In some embodiments, the alkaline solution comprises alkali metal hydroxide, the alkali metal hydroxide is easily ionized in the solution to form alkali metal ions and hydroxide ions, the alkalinity is strong, the pH of the reaction system is ensured to be more than or equal to 8, and the price is low. Among them, alkali metal hydroxides include, but are not limited to, lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, and the like.
In some embodiments, the pH of the alkaline solution is greater than 12. The high-concentration alkaline solution can provide enough hydroxide ions to be combined with copper ions in a mixed system, so that the reaction activity is improved to a certain extent, and the yield of copper oxide is improved.
In some embodiments, the molar ratio of alkali metal ions of the alkali metal hydroxide in the basic solution to copper ions in the first mixed solution is greater than 3: 1. Therefore, the method ensures that copper ions can completely react, is suitable for recovering and treating most of acidic etching waste liquid obtained by the printed circuit board etching process, and can be used for continuously recovering and using the alkaline components which do not participate in the reaction by a subsequent electrolytic method after the reaction is finished, thereby being beneficial to saving the cost.
Further, the preparation method further comprises the following steps: after step S03, the separated copper oxide powder is washed and dried. Removing impurities doped in the copper oxide powder by washing; drying is carried out to obtain dry copper oxide powder, and when the drying temperature is higher, the dehydration of a small amount of copper hydroxide possibly doped in the copper oxide powder to form copper oxide can be promoted to a certain extent, so as to further improve the purity of the copper oxide powder.
The specific operations of washing and drying can be adjusted flexibly according to actual production conditions by referring to the conventional operations in the field. In some embodiments, the filter residue obtained by filtering is washed 3-4 times by using clear water and then washed 2-3 times by using absolute ethyl alcohol. In some embodiments, the washed residue is dried in a vacuum oven or dryer.
Through detection, the purity of the copper oxide powder prepared by combining the preparation device and adopting the preparation method is basically more than 99.0%, the particle size is small, the particle size of the powder is 100-600 nm, the copper oxide powder can be directly put into the market, and the commercial value is high.
The practice of the present invention is illustrated by the following examples.
Example 1
In this embodiment, the apparatus shown in fig. 1 and the printed circuit board acidic etching solution are used to prepare copper oxide powder, which specifically includes the following steps:
(1) pumping the acidic waste etching solution of the printed circuit board into a first reaction barrel 1 through a first pipeline 52, starting a first stirring element 12 when the acidic waste etching solution reaches a specified position of the first reaction barrel 1, adding an oxidant into the first reaction barrel 1 from an oxidant feeding port 6 through a second pipeline 62 under a stirring state, stirring for 60min to obtain a first mixed solution, wherein the dosage of the oxidant is adjusted to enable the mass percentage concentration of the oxidant in the first mixed solution to be 4%, and standing for later use;
(2) adding a sodium hydroxide solution with the pH value of more than 12 into the second reaction barrel 2 until the solution reaches 1/3 of the barrel height, and adjusting the temperature of the second reaction barrel 2 to 65 ℃ by using a temperature control element 21; then, adjusting the flow pump 11, slowly adding the first mixed solution into the second reaction barrel 2 from the bottom of the second reaction barrel 2 through the third pipeline 13, and starting the second stirring element 22 to stir for 4 hours; the pH value of the system is required to be maintained at 9-10 in the stirring process, when the pH probe 23 senses that the pH value of the solution in the second reaction barrel 2 is less than 8, the flow pump 11 is closed, the first mixed solution is stopped to be added, and then the alkaline solution is supplemented to ensure that the flow pump 11 is restarted after the pH value of the system is 9-10;
the volume of the liquid in the second reaction barrel 2 is expanded due to the addition of the alkaline solution and the synthesis reaction of the copper oxide, the reacted copper oxide powder in the second reaction barrel 2 is suspended on the liquid level, and when the liquid level rises to the position of the overflow port 24, the suspension in which the copper oxide powder is suspended overflows from the overflow port 24 and flows into the collection barrel 3;
(3) opening the on-off valve 31 on the fourth pipe 32 so that the suspension in the collecting tank 3 flows into the solid-liquid separation element 4 through the fourth pipe 32 to perform the filtering operation; then, repeatedly washing the filtered copper oxide powder for 4 times by using deionized water according to a solid-liquid ratio of 1:4, washing for 5min each time, repeatedly washing for 2-3 times by using absolute ethyl alcohol according to a solid-liquid ratio of 1:3, washing for 10min each time, and drying a solid phase to obtain pure copper oxide powder;
(4) and (3) concentrating the liquid phase obtained after solid-liquid separation in the step (3) by a permeable membrane, and then carrying out electrolytic treatment by a double-membrane electrolytic method, wherein the concentration of hydrochloric acid collected in a double-membrane electrolytic anode region can reach 20%, and the concentration of sodium hydroxide solution collected in a cathode region can reach more than 30%, wherein the obtained hydrochloric acid is used as a raw material for preparing the acidic etching solution and returns to an etching line, and the sodium hydroxide can be used as a raw material for preparing the sodium hydroxide solution and returns to the step (2).
1. The copper oxide powder prepared in the embodiment 1 is added into dilute sulfuric acid and stirred for 20s to be completely dissolved, and the chlorine content is found to be less than 15ppm through content detection, so that the requirements of direct application of copper oxide in a circuit board electroplating copper plating process on quick dissolution of copper oxide and low chloride ion content are met, and the commercial value is high.
2. The surface morphology of the copper oxide powder prepared in example 1 was observed by a Scanning Electron Microscope (SEM) using the test sample, and the result is shown in fig. 2.
3. The copper oxide powder prepared in example 1 was taken and tested for particle size. The test results are shown in FIG. 3, in which the particle size of the copper oxide powder is 100-600 nm.
4. The copper oxide powder prepared in example 1 was analyzed by an X-ray diffractometer (XRD), and as shown in fig. 4, the purity of the copper oxide powder prepared in this example was more than 99.0% by comparison with the standard picture below the figure.
5. The copper oxide powder prepared in example 1 was subjected to X-ray photoelectron spectroscopy (XPS), and the results are shown in fig. 5.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (8)
1. A production apparatus for copper oxide powder, characterized by comprising:
the first reaction barrel is used for carrying out first mixing treatment on the acidic etching waste liquid containing cuprous ions and an oxidant so as to oxidize the cuprous ions into copper ions and form a first mixed solution;
the second reaction barrel is communicated with the first reaction barrel, is provided with a pH probe and a temperature control element and is used for carrying out second mixing treatment on the first mixed solution and the alkaline solution under the conditions that the pH is more than or equal to 8 and the temperature is more than 50 ℃ so as to form copper oxide;
the collecting barrel is used for collecting the suspension liquid with the copper oxide powder dispersed in the second reaction barrel;
and the solid-liquid separation element is communicated with the collecting barrel and is used for separating the copper oxide powder in the suspension.
2. The apparatus according to claim 1, wherein the second reaction tank is connected to the first reaction tank via a third pipe, and one end of the third pipe is open to the bottom of the second reaction tank.
3. The manufacturing apparatus as set forth in claim 2, wherein a flow pump is provided on said third piping.
4. The manufacturing apparatus as set forth in claim 1, wherein said first reaction barrel is provided with a first stirring member; and/or
The second reaction barrel is provided with a second stirring element.
5. The apparatus of claim 1, wherein the second reaction tank is provided with an overflow port at a tank height of 1/3-2/3, and the tank port of the collecting tank is located directly below the overflow port.
6. The manufacturing apparatus as set forth in claim 1, wherein said collecting vessel communicates with said solid-liquid separation element through a fourth conduit, and said fourth conduit is provided with an on-off valve.
7. The manufacturing apparatus according to any one of claims 1 to 6, wherein the solid-liquid separation element is a filter press, a centrifuge, or a natural settler.
8. The manufacturing apparatus of any one of claims 1 to 6, further comprising: the first reaction barrel is respectively communicated with the acidic etching waste liquid feeding port and the oxidant feeding port through a first pipeline and a second pipeline, and filtering elements for filtering impurities are arranged on the first pipeline and the second pipeline.
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