Copper dissolving system and process for electrolytic copper foil
阅读说明：本技术 一种电解铜箔的溶铜系统及溶铜工艺 (Copper dissolving system and process for electrolytic copper foil ) 是由 廖中良 宋豪杰 熊佑文 冯志建 岳双霞 张建彬 李军 刘新建 方彧 于 2019-10-10 设计创作，主要内容包括：本发明公开了一种电解铜箔的溶铜系统,该系统包括串接的一次溶铜系统以及二次溶铜系统,并设置有压缩空气组件为一次溶铜系统以及二次溶铜系统进行压缩空气供气,其中,一次溶铜系统中包括溶铜罐,溶铜罐下部设置换热装置,并分别在换热装置的上、下部设置有盘管以及隔板以分别通入压缩气体以及防止铜原料；一次溶铜系统通过溢流结构连接二次溶铜系统,并在二次溶铜系统的溶铜罐中进行二次溶铜处理,且在溶铜处理处理过程中进行过滤和溢流操作；系统配合相应的溶铜方法来提供和获得不同浓度的含铜离子的混合物溶液,并通过合理的压缩空气供给来提高反应速率。本发明能够有效提高溶铜质量,减少硫酸铜溶液中亚铜离子和有机物杂质的含量,并降低溶液温度。(The invention discloses a copper dissolving system of electrolytic copper foil, which comprises a primary copper dissolving system and a secondary copper dissolving system which are connected in series, and a compressed air assembly is arranged for compressed air supply of the primary copper dissolving system and the secondary copper dissolving system, wherein the primary copper dissolving system comprises a copper dissolving tank, the lower part of the copper dissolving tank is provided with a heat exchange device, and the upper part and the lower part of the heat exchange device are respectively provided with a coil pipe and a partition plate for respectively introducing compressed gas and preventing copper raw materials; the primary copper dissolving system is connected with the secondary copper dissolving system through an overflow structure, secondary copper dissolving treatment is carried out in a copper dissolving tank of the secondary copper dissolving system, and filtering and overflow operations are carried out in the copper dissolving treatment process; the system is matched with a corresponding copper dissolving method to provide and obtain mixture solutions containing copper ions with different concentrations, and the reaction rate is improved through reasonable compressed air supply. The invention can effectively improve the quality of dissolved copper, reduce the content of cuprous ions and organic impurities in the copper sulfate solution and reduce the temperature of the solution.)
1. A copper dissolving system for electrolytic copper foil, comprising:
a compressed air assembly: the compressed air is used for providing and is connected with the primary copper dissolving system and the secondary copper dissolving system through an air supply pipeline;
a primary copper dissolving system: the device is used for carrying out primary copper dissolving treatment and comprises a primary copper dissolving tank, wherein the upper part of the primary copper dissolving tank is provided with a feed inlet for adding raw material copper and a feed inlet for adding a mixed liquid of dilute copper sulfate and sulfuric acid, the lower part of the primary copper dissolving tank is provided with a heat exchange device, an air supply pipeline extends into the primary copper dissolving tank from two sides of the primary copper dissolving tank, compressed air is introduced into the tank through a coil pipe between the heat exchange device at the lower part of the tank body and the tank bottom, a partition plate for placing the raw material copper is also arranged below the primary copper dissolving tank, the partition plate is arranged above the heat exchange device, small holes are uniformly formed in the partition plate so as to facilitate the compressed air to pass through, and meanwhile, the side of the upper part of the primary copper dissolving tank;
and (3) a secondary copper dissolving system: the secondary copper dissolving tank is connected to the rear part of the primary copper dissolving tank in series and comprises a feed inlet and a discharge outlet, the front end of the feed inlet is connected with an overflow hole beside the primary copper dissolving tank through a feed inlet pipe, the rear end of the feed inlet pipe extends into the secondary copper dissolving tank, meanwhile, a filtering device is arranged between the feed inlet and the discharge outlet, and an overflow structure is arranged between the filtering device and the discharge outlet; the liquid outlet position at the rear end of the liquid inlet pipe is opposite to the filtering device; meanwhile, the air supply pipeline extends into the bottom of the secondary copper dissolving tank and introduces compressed air into the tank.
2. The system for dissolving electrolytic copper foil according to claim 1, wherein the heat exchanger is a heat exchanger.
3. The system for dissolving copper in electrolytic copper foil according to claim 1, wherein the primary copper dissolving tank and the secondary copper dissolving tank are each provided with an induced draft opening as an in-tank gas outlet.
4. The system for dissolving electrolytic copper foil according to claim 3, wherein the induced draft port pipe is connected to an exhaust gas treatment device.
5. The system for dissolving electrolytic copper foil according to claim 1, wherein the volume of the secondary copper dissolving tank is 1/100 to 1/10 times the volume of the primary copper dissolving tank.
6. The system for dissolving copper in electrolytic copper foil according to claim 1, wherein the filtering means comprises a plurality of filter frame structures or filter cage structures, and the filter frame structures or filter cage structures are filled with replaceable activated carbon or filter cloth or filter bag as a filtering material.
7. The system for dissolving electrolytic copper foil according to claim 6, wherein the filter material is activated carbon.
8. The system for dissolving electrolytic copper foil according to claim 1, wherein the overflow structure is a baffle plate disposed between the filtering device and the discharge port, and the height of the baffle plate is lower than the height of the filtering device.
9. A copper dissolving method of electrolytic copper foil utilizes the equipment to carry out copper dissolving operation, and specifically comprises the following steps:
s1, adding raw material copper to a partition plate in the primary copper dissolving tank through a feed inlet, injecting a low-concentration copper sulfate and sulfuric acid mixed solution into the bottom of the primary copper dissolving tank from a liquid inlet at the upper part of the primary copper dissolving tank, controlling the addition amount of the low-concentration copper sulfate and sulfuric acid mixed solution based on the immersion of the raw material copper, and controlling the sulfuric acid concentration of the mixed solution to be 10-150 g/L and the Cu concentration to be Cu2+The concentration is 0-100 g/L;
s2, heating the solution in the primary copper dissolving tank by using a heat exchange device, controlling the heating temperature to be 45-85 ℃, and introducing 0.2-1.0 MPa of compressed air into the solution in the primary copper dissolving tank from two air supply pipelines at two sides of the primary copper dissolving tank, wherein the flow rate is 5-500 m3/h；
S3 adding the mixture of low-concentration copper sulfate and sulfuric acid continuously to make the raw copper generate copper dissolving reaction continuously in the tank to generate copper sulfate, and making the low-concentration copper sulfate solution become high-concentration copper sulfate solution when Cu is present2+When the content reaches 80-160 g/L, the overflow port is opened to make the high-concentration sulfurThe acid copper solution enters a secondary copper dissolving tank from an overflow port of the primary copper dissolving tank;
s4 compressed air is introduced into the secondary copper dissolving tank through the compressed air assembly, and after the compressed air enters the high-concentration copper sulfate solution, oxygen in the air and Cu in the solution+Reaction for producing Cu2+And filtering by a filtering device, overflowing by an overflow structure and then entering a sewage tank from a liquid outlet, thus completing the copper dissolving process.
Technical Field
The invention belongs to the technical field of electrolytic copper foil production, and particularly relates to a copper dissolving system and a copper dissolving process of an electrolytic copper foil.
Background
The copper dissolving is a first procedure of electrolytic copper foil production, provides copper sulfate solution for copper foil production, is a very key procedure, and is a procedure of oxidizing a copper raw material in a container for reaction.
The traditional copper dissolving mode is a soaking mode, raw material copper is soaked in a mixed solution of low-concentration copper sulfate and sulfuric acid in a copper dissolving tank, air is introduced from the tank bottom and heated, copper reacts with oxygen to generate copper oxide, and the copper oxide reacts with the sulfuric acid to generate copper sulfate. However, the immersion type copper dissolving process in the prior art has low efficiency, and the generated Cu is generated due to insufficient oxidation of copper in the copper dissolving reaction process+Can enter the subsequent foil-producing process to cause the defects of burrs, roughness, pinholes, copper nodules and the like of the foil layer, and in addition, the soaking type solutionThe required ambient temperature of copper is higher, and the high concentration copper sulfate solution temperature that leads to producing is far higher than the crude foil temperature, need through the heat exchanger cooling before getting into the crude foil process, and the heat transfer difference in temperature is big, and in addition equipment heat exchange efficiency is low, leads to the energy consumption increase of relevant equipment, is unfavorable for the cost control and the long-term development of enterprise.
Disclosure of Invention
The invention aims to provide a copper dissolving system and a copper dissolving process of an electrolytic copper foil, and aims to solve the problems that the copper dissolving method of the electrolytic copper foil in the prior art is low in copper dissolving efficiency, high in energy consumption, high in solution temperature, low in heat exchange efficiency of a subsequent cooling heat exchanger and high in operation cost, and cuprous ions in the solution cannot be removed.
The technical problem solved by the invention is realized by adopting the following technical scheme:
a copper dissolution system for electrolytic copper foil comprising:
a compressed air assembly: the compressed air is used for providing and is connected with the primary copper dissolving system and the secondary copper dissolving system through an air supply pipeline;
a primary copper dissolving system: the device is used for carrying out primary copper dissolving treatment and comprises a primary copper dissolving tank, wherein the upper part of the primary copper dissolving tank is provided with a feed inlet for adding raw material copper and a feed inlet for adding a mixed liquid of dilute copper sulfate and sulfuric acid, the lower part of the primary copper dissolving tank is provided with a heat exchange device, an air supply pipeline extends into the primary copper dissolving tank from two sides of the primary copper dissolving tank, compressed air is introduced into the tank through a coil pipe between the heat exchange device at the lower part of the tank body and the tank bottom, a partition plate for placing the raw material copper is also arranged below the primary copper dissolving tank, the partition plate is arranged above the heat exchange device, small holes are uniformly formed in the partition plate so as to facilitate the compressed air to pass through, and meanwhile, the side of the upper part of the primary copper dissolving tank;
and (3) a secondary copper dissolving system: the secondary copper dissolving tank is connected to the rear part of the primary copper dissolving tank in series and comprises a feed inlet and a discharge outlet, the front end of the feed inlet is connected with an overflow hole beside the primary copper dissolving tank through a feed inlet pipe, the rear end of the feed inlet pipe extends into the secondary copper dissolving tank, meanwhile, a filtering device is arranged between the feed inlet and the discharge outlet, and an overflow structure is arranged between the filtering device and the discharge outlet; the liquid outlet position at the rear end of the liquid inlet pipe is opposite to the filtering device; meanwhile, the air supply pipeline extends into the bottom of the secondary copper dissolving tank and introduces compressed air into the tank.
By way of further limitation, the heat exchange device is a heat exchanger.
As a further limitation, the primary copper dissolving tank and the secondary copper dissolving tank are both provided with air inducing ports as gas outlets in the tanks for adjusting the air pressure in the tanks and discharging reaction waste gas, and the air inducing ports are connected into a waste gas treatment device through pipelines.
The volume of the secondary copper dissolving tank is smaller than that of the primary copper dissolving tank, and is 1/100-1/10 of the volume of the primary copper dissolving tank.
As a further limitation, the filtering device comprises a plurality of filter frame structures or filter cage structures, and the filter frame structures or filter cage structures are filled with replaceable filtering materials, wherein the filtering materials are activated carbon or filtering cloth or filtering bag, preferably activated carbon.
And as further limitation, the overflow structure is a baffle arranged between the filtering device and the discharge port, the setting height of the baffle is lower than that of the filtering device, the mixture solution in the secondary copper dissolving tank is filtered by the filtering device and then is retained at the inner side of the baffle, and the mixture solution overflows when the liquid level of the mixture solution exceeds the baffle and flows out from the discharge port.
The invention also discloses a copper dissolving method of the electrolytic copper foil, which utilizes the equipment to carry out copper dissolving operation and specifically comprises the following steps:
s1, adding raw material copper to a partition plate in the primary copper dissolving tank through a feed inlet, injecting a low-concentration copper sulfate and sulfuric acid mixed solution into the bottom of the primary copper dissolving tank from a liquid inlet at the upper part of the primary copper dissolving tank, controlling the addition amount of the low-concentration copper sulfate and sulfuric acid mixed solution based on the immersion of the raw material copper, and controlling the sulfuric acid concentration of the mixed solution to be 10-150 g/L and the Cu concentration to be Cu2+The concentration is 0-100 g/L;
s2, heating the solution in the primary copper dissolving tank by using a heat exchange device, controlling the heating temperature to be 45-85 ℃, and introducing 0.2-1.0 MPa of compressed air into the solution in the primary copper dissolving tank from two air supply pipelines at two sides of the primary copper dissolving tank, wherein the flow rate is 5-500 m3/h；
S3 adding the mixture of low-concentration copper sulfate and sulfuric acid continuously to make the raw copper generate copper dissolving reaction continuously in the tank to generate copper sulfate, and making the low-concentration copper sulfate solution become high-concentration copper sulfate solution when Cu is present2+When the content reaches 80-160 g/L, opening the overflow port to enable the high-concentration copper sulfate solution to enter the secondary copper dissolving tank from the overflow port of the primary copper dissolving tank;
s4 compressed air is introduced into the secondary copper dissolving tank through the compressed air assembly, and after the compressed air enters the high-concentration copper sulfate solution, oxygen in the air and Cu in the solution+Reaction for producing Cu2+And filtering by a filtering device, overflowing by an overflow structure and then entering a sewage tank from a liquid outlet, thus completing the copper dissolving process.
The invention has the beneficial effects that:
a secondary copper dissolving system is added in the prior soaking type copper dissolving system to dissolve Cu generated by copper+Oxidized into Cu in secondary copper dissolving system2+Elimination of Cu+Influence on the quality of the copper foil. The volume of the secondary copper dissolving tank in the system is 1/100-1/10 of the volume of the primary copper dissolving tank, the volume is small, the manufacturing cost is low, and in addition, Cu+The oxidation does not need heating, the required air supply amount is small, the energy consumption is very low, but the effect is obvious;
the secondary copper dissolving tank is provided with the filtering device, so that the copper sulfate solution is subjected to coarse filtering, the pressure of a subsequent filtering system is reduced, the service life of a filtering material in the filter is prolonged, and the replacement frequency is reduced. The filter material in the filter is difficult to replace, the filter needs to be stopped, the production is affected very adversely, the filter material in the filter device is easy to replace after reaching saturation, and can be recycled, the filter efficiency is high, the operation cost is low, and the operation cost of the whole filter system can be greatly saved.
The secondary dissolves the copper and need not the heating, and can take away the partial heat in the solution when letting in the compressed air discharge in the jar, and the secondary dissolves the copper jar and also can give off some heat, consequently plays fine cooling effect to the copper sulfate solution, can reduce follow-up cooling heat exchanger burden.
And a liquid baffle is arranged in the secondary copper dissolving tank, so that the filtering area is increased, and the filtering efficiency is improved.
The air inlet mode in the primary copper dissolving tank is changed from one end air inlet mode to two end air inlet mode, the air pressure of the two end air inlets is relatively stable, the air quantity in the tank is consistent, the copper dissolving speed is accelerated, and the Cu of the crude foil system is ensured2+Normal supply of (2).
Drawings
FIG. 1 is a schematic structural diagram of a copper dissolving system according to a preferred embodiment of the present invention.
Wherein: 1. a primary copper dissolving tank; 2. a secondary copper dissolving tank; 11. a feed inlet; 12. a liquid filling port; 131. a first air supply port; 132. a second air supply port; 14. a primary copper dissolving tank air inlet; 15. an overflow port; 16. a partition plate; 17. a coil pipe; 181. a first air supply line; 182. a second gas supply line; 19. a heat exchanger; 191. a steam inlet; 192. a condensed water outlet; 21. a filter material replacement port; 22. a feeding hole of the secondary copper dissolving tank; 23. a third air supply port; 24. a secondary copper dissolving tank air inducing port; 25. a liquid outlet; 26. a U-shaped pipe; 27. a third gas supply line; 28. a filtration device; 29. a baffle plate; 30. a liquid inlet pipe.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further described below by combining the specific drawings and the embodiments.
In the above embodiments, it will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Referring to fig. 1, in the present embodiment, the copper dissolving system includes a primary copper dissolving system and a secondary copper dissolving system, wherein a main container of the primary copper dissolving system is a primary copper dissolving tank 1, a main container of the secondary copper dissolving system is a secondary
A
High-concentration high-temperature copper sulfate solution produced by copper dissolution reaction in the primary copper dissolution tank 1 enters a secondary copper dissolution system from an overflow port 15, the secondary copper dissolution system comprises a secondary copper dissolution tank 2, a filtering device 28 and a baffle 29, the top of the secondary copper dissolution tank 2 is provided with a filtering material replacement port 21, a secondary copper dissolution tank feeding port 22, a compressed air inlet and a secondary copper dissolution tank air induction port 24, wherein the filtering material replacement port 21 is used for replacing a filtering core material in the filtering device 28; the overflow mouth 15 that the secondary dissolves copper jar feed inlet 22 upper portion is connected once and is dissolved copper jar 1 jar body side and be arranged in receiving the high temperature copper sulfate solution of high concentration that once dissolves in copper jar 1, be connected with third air supply line 27 on the compressed air import, the compressed air subassembly is connected to this third air supply line 27 front end, the rear end is connected near the one corner of jar wall with U type pipe 26, even intensive venthole of seting up on the U type pipe 26, the compressed air that gets into secondary through U type pipe 26 and dissolves copper jar 2 except that providing oxygen for the secondary, can also take away some heats in the solution, play the effect that reduces the solution temperature.
The tail end of a high-concentration high-temperature copper sulfate solution inlet 22 is connected with a liquid inlet pipe 30, the liquid inlet pipe 30 extends into the second copper dissolving tank 2, the tail end of the liquid inlet pipe 30 is close to the bottom of a filtering device 28, mixed liquid entering the liquid inlet pipe 30 extends into the tank to ensure that the solution can be completely filtered, the filtering device 28 consists of two filtering material placing baskets, filtering materials are placed in the filtering baskets, one filtering basket is arranged in the middle of a U-shaped pipe 27, the other filtering basket is arranged outside the U-shaped pipe 27, two ends and the bottom of the filtering basket are hermetically fixed with the second copper dissolving tank to prevent partial solution from directly entering the next process from a liquid outlet 25 without being filtered, meanwhile, the solution can be completely filtered, two sides and the bottom of a baffle 29 are respectively connected with the second copper dissolving tank 2, the upper part of the baffle is at a certain distance from the top of the second copper dissolving tank 2, and the, the solution can be completely filtered by the filter device 28, and the baffle 29 also has the purpose of increasing the filtering area and improving the filtering efficiency; the lower part of the side surface of the secondary copper dissolving tank 2 is also provided with a liquid outlet 25, and the high-concentration high-temperature copper sulfate solution entering the secondary copper dissolving tank 2 enters a sewage tank from the liquid outlet after being oxidized, filtered and cooled, so as to supplement Cu for the green foil2+。
The copper dissolving method based on the equipment specifically comprises the following steps:
first, the raw material copper is placed on the
The supply of the mixed solution is maintained, so that the raw material copper reacts with oxygen and sulfuric acid under the heating condition to gradually dissolve to generate copper sulfate which enters the solution when the Cu is dissolved2+When the content is increased to 80-160 g/L, high-concentration high-temperature copper sulfate solution is formed, and then enters a secondary copper dissolving system from the
High-concentration copper sulfate solution enters the secondary
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
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